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  • Articles  (25,720)
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  • 2000-2004
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  • 1
    Electronic Resource
    Electronic Resource
    Fundamental properties of fluoropolyether-based resins and related coatings (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 236 (1996), S. 111-127 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Neuartige Fluoropolyether-Polyol-Harze, die mit konventionellen Härtern wie Polyisocyanaten oder Melaminen aushärtbar sind, wurden hergestellt. Zunächst wurden oligomere NCO-terminierte Prepolymere durch Addition von Fluorpolyether-Makrodiolen unterschiedlicher Molekulargewichte an Isophorondiisocyanate erhalten. Durch die Reaktion dieser Prepolymeren mit Trimethylolpropan wurden endständige Hydroxygruppen eingeführt. Die Viskosität von Lösungen dieser Harze wurde bei unterschiedlichen Konzentrationen (Massenbruch 0,4-0,8) und Temperaturen (25°C-65°C) gemessen. Die erhaltenen Werte wurden auf der Basis der Erickson-Gleichung (Konzentrationsabhängigkeit von η) und unter Berücksichtigung des WLF-und des Arrhenius-Modells (Temperaturabhängigkeit von η) diskutiert. Das thermische Verhalten der Harze und von ausgehärteten Filmen wurde mit DSC bestimmt. Dabei wurden zwei Glasübergange beobachtet, die den separierten fluorhaltigen und nicht-fluorhaltigen Phasen zugeordnet werden können. Die Analyse des Zugverhaltens der Filme zeigte besonders bei den mit Isocyanat gehärteten Proben ein ausgeprägtes hart-plastisches Verhalten. Diese Werkstoffe erscheinen für die Anwendung als hoch-wertige, dauerfeste und klare Beschichtungen geeignet.
    Notes: New fluoropolyether polyolic resins are presented suitable to be cured with conventional hardeners as polyisocyanates or melamines. These resins are prepared by addition of fluoropolyether macrodiols (Fomblin® ZDOLTX) of various molecular weights to isophorone diisocyanate (IPDI) to give oligomeric NCO-terminated prepolymers. The final hydroxy functionality is obtained by the reaction of those prepolymers with trimethylolpropane (TMP). The viscosity of the resins is measured at various concentrations (weight fraction 0.8 - 0.4) and temperatures (T = 25-65°C). The results are discussed in terms of the Erickson equation (η vs. concentration) and using the WLF and Arrhenius models (η vs. T). The thermal behavior is studied by DSC for both the resins and cured films indicating the presence of two Tgs, corresponding to the segregated fluorinated and hydrogenated phases, the former particularly evident with the highest molecular weights of the fluorinated macromer. Tensile curves of selfsupported films are then analyzed showing an evident tough-plastic behavior especially for the isocyanate-cured films. The application of such materials as high-durability clear coats is finally proposed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052360109
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  • 2
    Electronic Resource
    Electronic Resource
    Modification of melamine-formaldehyde moulding compounds with epoxy resins (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 237 (1996), S. 1-44 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Zur Verbesserung der Maßhaltigkeit und der Zähigkeit von gehärteten Melamin-Formaldehyd-Harz-Formmassen (MF) wurden teilverträgliche, methylolgruppenhaltige Epoxidharze (EP) auf Bisphenol A-Basis hergestellt und charakterisiert. Die Vernetzung solcher Epoxyresolharze durch 2-Ethyl-4-methylimidazol in Gegenwart von MF-Harz wurde untersucht. Spritzgepreßte Probekörper zeigen eine Zweiphasenstruktur; die EP-Phase kann als Wirt für carboxy-funktionalisierte, oligomere NBR-Kautschuke (CTBNX) dienen, die für sich allein in MF-Harzen nicht wirksam sind. Unter der Voraussetzung von kovalenten Bindungen in der Phasengrenzfläche kann durch den Zusatz von 0,5 bis 4 Gew.-% CTBNX zur MF-Formmasse bei EP-Anteilen bis 20 Gew.-% eine 50 bis 100proz. Steigerung von Bruchdehnung und Schlagzähigkeit erreicht werden, ohne daß Steifigkeit und Wärmeformbeständigkeit wesentlich abfallen. Bei moderaten EP/CTBNX-Gehalten wird zusätzlich die Nachschwindung von MF-Formteilen vermindert.
    Notes: In order to improve dimension stability and toughness of melamine formaldehyde moulding materials (MF), compatible bisphenol A epoxy resins (EP) with additional methylol groups were synthesized and characterized. Crosslinking of those epoxyresol resins with 2-ethyl-4-methylimidazole in the presence of MF resin was investigated. Transfer-moulded specimens revealed a two-phase morphology in which the EP phase is used as a host for modification with carboxylic functionalized oligomeric NBR rubber (CTBNX), which is not effective in MF moulding materials alone. The addition of 0.5 - 4 wt.-% CTBNX to the MF moulding materials at an epoxy content of maximum 20 wt.-% results in 50-100 % increase of elasticity and toughness without serious decrease in stiffness and heat deflection temperature, provided that covalent interfacial bonds exist. In addition, the post-shrinkage of MF parts decreases if a moderate EP/CTBNX content is introduced.
    Additional Material: 26 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052370101
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  • 3
    Electronic Resource
    Electronic Resource
    New poly(vinyl chloride) blends, IIIPart II cf.5.. Physico-mechanical properties (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 238 (1996), S. 11-30 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Der gleichzeitige Einfluß des Verhältnisses von Fließhilfsmittel (Paraloid K 120N), Rußart und Schlagzähmodifikator (CPE 3615 und Kane Ace B56 A) auf die wichtigsten physiko-mechanischen Eigenschaften unplastifizierter PVC-Mischungen wurde studiert.Die erhaltenen Resultate wurden mathematisch verarbeitet und graphisch als Funktionsflächen dargestellt. Bemerkenswert ist, daß die Einführung von 2,5 und 5 Teilen Ruß eine Verbesserung der physico-mechanischen Eigenschaften ermöglicht. Dieses Resultat ist durch die Anwesenheit der Schlagzäh- und Fließmodifikatoren zu erklären.
    Notes: The concurrent influence of the processing aid (Paraloid K 120N) and the carbon black ratio, as well as the nature and the ratio of the impact modifier (CPE 3615 and Kane Ace B56 A) on the main physico-mechanical characteristics of the poly(vinyl chloride)-based unplasticized mixtures have been studied. The results obtained, processed mathematically and plotted graphically in the form of response surfaces, evidenced that the improvement of certain physico-mechanical properties becomes possible by the introduction of 2.5 parts and 5.0 parts carbon black into these compounds. This is due to the introduction of impact modifiers and processing aids into the mixtures.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052380102
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  • 4
    Electronic Resource
    Electronic Resource
    New polyhydrazides and poly(1,3,4-oxadiazole)s containing pendent phenoxy groups (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 238 (1996), S. 63-71 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Eine Reihe neuartiger Polyhydrazide mit endständigen Phenoxygruppen wurde aus äquimolaren Anteilen von Dicarbonsäuredichloriden und Phenoxyterephthalsäuredihydrazid durch Lösungspolykondensation in N-Methyl-2-pyrrolidinon (NMP) bei niedriger Temperatur hergestellt. Durch thermische Cyclisierung der Polyhydrazide wurden die entsprehchenden Poly(1,3,4-oxadiazol)e mit endständigen Phenoxygruppen erhalten. Die Polymeren wurden durch Viskosimetrie, Löslichkeitsuntersuchungen, IR-Spektroskopie, Differentialkalorimetrie und Thermogravimetrie charakterisiert.
    Notes: A series of new polyhydrazides containing pendent phenoxy groups has been synthesized by low-temperature solution polycondensation of equimolar amounts of diacid dichlorides and 2-phenoxyterephthalic dihydrazide in N-methyl-2-pyrrolidi-none (NMP). The thermal cyclization of the polyhydrazides gave the corresponding poly(1,3,4-oxadiazole)s containing pendent phenoxy groups. The polymers were characterized by viscometry, solubility measurements, IR spectroscopy, differential scanning calorimetry (DSC) and thermogravimetric analysis.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052380106
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  • 5
    Electronic Resource
    Electronic Resource
    Effect of electron beam radiation on mechanical and electrical properties of poly(ethylene-co-vinyl acetate) (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 238 (1996), S. 105-117 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Ein Ethylen-Vinylacetat-Copolymeres (EVA) mit 12% Vinylacetat-Gehalt wurde mit Trimethylolpropantrimethacrylat (TMPTMA) als Sensibilisator mit Elektronen bestrahlt. Die mechanischen und elektrischen Eigenschaften der bestrahlten Copolymerproben wurden untersucht. Die Resultate zeigen, daß sich Zugfestigkeit und Bruchdehnung zunächst mit zunehmender Strahlungsdosis verbessern und bei Überschreiten einer optimalen Strahlungsdosis und Sensibilisatorkonzentration wieder verschlechtern. Durch die Bestrahlung wird eine Vernetzung des Polymeren ausgelöst, die auf den sich mit der Strahlungsdosis erhöhenden Gelanteil zurückgeführt wird. Im Vergleich mit den Originalproben nehmen sowohl die Dielektrizitätskonstante als auch der dielektrische Verlustfaktor durch die Elektronenbestrahlung ab.
    Notes: Ethylene-vinyl acetate (EVA) copolymer (12% vinyl acetate content) is subjected to electron beam irradiation using trimethylolpropane trimethacrylate (TMPTMA) as a radiation sensitizer. Mechanical and electrical studies of these irradiated samples show that the strength properties (tensile strength, elongation at break) are increased with radiation dosage up to an optimum radiation dose and sensitizer level above which the properties begin to deteriorate. Crosslinking of the polymer takes place on irradiation which is attributed to an increased gel content with increasing radiation dose. Compared to the original samples both dielectric constant and dielectric loss factor decrease for samples subjected to irradiation.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052380110
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  • 6
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    Electronic Resource
    Homogeneous synthesis of cellulose p-toluenesulfonates in N,N-dimethylacetamide/LiCl solvent system (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 238 (1996), S. 143-163 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Cellulose-p-toluolsulfonsäureester (Cellulosetosylate) lassen sich durch homogene Umsetzung von Cellulose in einer Lösung aus N,N-Dimethylacetamid und LiCl mit Tosylchlorid (Tos-Cl) und Triethylamin in 24 h bei 8°C in hoher Ausbeute und mit minimalem Einbau von Chlordesoxy-Gruppen herstellen. Die unterschiedlichen Celluloseausgangsmaterialien hatten durchschnittliche Polymerisationsgrade von 280 bis 5100. Die Produkte wurden mit Elementaranalyse, 13C-NMR- und FTIR-Spektroskopie und durch Bestimmung der Grenzviskositäten charakterisiert. Die Erhöhung des Molverhältnisses Tos-Cl/Anhydroglucose-Einheit (AGU) von 0.6 auf 9.0 führte zu einem Anstieg des Substitutionsgrades (DS) von 0.4 bis auf einen Maximalwert von 2.3. Die Cellulosetosylate sind in herkömmlichen organischen Lösungsmitteln wie Dimethylsulfoxid (im gesamten DS Bereich) und in N,N-Dimethylacetamid, N,N-Dimethylformamid, Aceton, Tetrahydrofuran und Trichlormethan (in Abhängigkeit von DS) löslich. Durch 13C-NMR-Spektroskopie wurde nachgewiesen, daß die Tosylierung am O-6 Atom der AGU schneller als an den O-2/3 Atomen erfolgt. Die Analyse der korrespondierenden Ioddesoxycellulosen, die durch Umsetzung mit NaI in Acetylaceton synthetisiert wurden, bestätigte dies zusätzlich. Darüber hinaus wurden wichtige Eigenschaften der Cellulosetosylate wie die Stabilität gegenüber Alkali und thermischer Beanspruchung untersucht.
    Notes: Pure cellulose p-toluenesulfonates (tosylates) with an insignificant formation of chlorodeoxy groups were prepared by reacting cellulose dissolved in a solution of N,N-dimethylacetamide and LiCI with tosylchloride (Tos-CI) in the presence of triethylamine within 24 h at 8°C. Various cellulosic starting materials with a degree of polymerization from 280 to 5 100 were used. The samples obtained were characterized by means of elemental analysis, FTIR and 13C NMR spectroscopy, and their intrinsic viscosities. The rise of the molar ratio of Tos-CI/anhydroglucose unit (AGU) from 0.6 to 9.0 leads to an increase in the degree of substitution (DS) from 0.4 up to a maximum value of 2.3. The cellulose tosylates are readily soluble in common organic solvents like dimethyl sulfoxide (within the whole DS range) and in N,N-dimethylacetamide, N,N-dimethylformamide, acetone, tetrahydrofuran and trichloromethane depending on DS. As revealed by 13C NMR spectroscopy a faster tosylation takes place at the O-6 atom of AGU compared with the O-2/3 atoms. This was additionally confirmed by analysis of the corresponding iododeoxy celluloses synthesized with NaI in acetylacetone. Furthermore, some important properties as stability against alkaline and heat were studied as well.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052380113
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  • 7
    Electronic Resource
    Electronic Resource
    Coating of carbon-fiber surface by silicon carbide via sol-gel mixtures of tetraethyl orthosilicate and phenolic resin (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 27-32 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Herstellung einer SiC-Oberfläche auf Kohlefasern unter Verwendung einer Sol-Gel-Mischung von Tetraethylorthosilikat (TEOS) und Phenolharz wurde untersucht. FTIR- und SEM-Untersuchungen zeigten, daß die SiC-Oberfläche durch carbothermische Reduktion der Sol-Gel-Mischung bei 1 420°C innerhalb von 15-20 min in einer Argon-Atmosphäre gebildet werden kann. Mittels TGA konnte gezeigt werden, daß die SiC-Beschichtung die thermo-oxidative Stabilität der Kohlefasern erhöht. Bei der erreichten SiC-Schichtdicke von 0,47 μm, bei einem C/Si-Verhältnis von 4, zeigt sich keine Beeinflussung der mechanischen Stabilität der Kohlefasern.
    Notes: The preparation of a SiC coating on a carbon fiber surface using a sol-gel mixture of tetraethyl orthosilicat (TEOS) and phenolic resin was studied. FTIR and SEM investigations indicated that the SiC coating can be formed by carbothermal reduction of the sol-gel mixture at 1420°C for 15-20 min in an argon atmosphere. TGA of the coated fiber was also performed, showing that the SiC coating improves the thermooxidative stability of the carbon fiber. With the thickness of the obtained coating of 0.47 μm using a C/Si ratio of 4, this treatment does not affect the carbon fiber strength.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052390103
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  • 8
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    Adhesive properties of some pressure-sensitive adhesive agents containing oligomer additives (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 55-62 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Diese Mitteilung behandelt den Einfluß von oligomeren Polypropylen- und Polybutylenölen mit unterschiedlichem Molekulargewicht auf die adhäsiven Eigenschaften von ataktischem Polypropylen (aPP) und dessen Mischungen mit einem Styrol-Ethylhexylacrylat-Copolymeren. Die mechanische Adhäsionsarbeit Am von Mischungen, die ataktisches Polypropylen und das Oligomere enthalten, steigt mit dem Molekulargewicht des Oligomeren, was im Fall des Propylenöls signifikanter ist. Im Fall der ternären Mischungen des ataktischen Polypropylens mit dem Styrol-Ethylhexylacrylat-Copolymeren und Oligomeren wird ein Adhäsions-Maximum beobachtet, wenn der Gehalt an Styrol-Ethylhexylacrylat-Copolymeren in der Mischung ungefähr 30 Gew.-% erreicht. Wenn kein Oligomeres in der Mischung vorhanden ist, kann man bei dieser Zusammensetzung ein Adhäsions-Minimum beobachten, was auf die Unverträglichkeit der übrigen Komponenten zurückzuführen ist.
    Notes: This paper deals with the influence of oligomers, namely propylene oil and butylene oil, of different molecular weight on the adhesive properties of atactic polypropylene (aPP) and its mixtures with styrene-2-ethylhexyl acrylate (S-EHA) copolymer. The mechanical work of adhesion Am of the mixture containing atactic polypropylene and oligomer increases with the molecular weight of the oligomer, which was more significant in the case of propylene oil. For ternary mixtures aPP-S-EHA copolymer/oligomer a maximum of adhesion can be observed if the content of the S-EHA copolymer in the mixture reaches about 30 mass-%. In the absence of oligomers in the mixture a minimum of adhesion can be observed for this composition, which can be attributed to the incompatibility of the remaining components.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052390106
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  • 9
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    Untersuchungen zur synthese von poly(butadien-co-propylenoxid) mit einem ziegler-natta-titankatalysatorsystem (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 107-119 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: After comparison of three catalyst systems, i.e. [Nd(Oct)3/Al2Cl3ET3/Al(i-But)3, Ni(Oct)2/BF3OEt2/AlEt3 and Al(i-But)3/I2/TiCl4] the titanium catalyst system was used for the copolymerization of 1,3-butadiene with propylene oxide. The effects of monomer ratio on copolymer composition, conversion, microstructure, molar mass and molar mass distribution as well as of time of polymerization and of the aluminium/titanium ratio were evaluted. The copolymerization parameters were determined according to Kelen-Tüdős as rbutadiene = 0,9 and rpropylene oxide = 3,9. Copolymerization was confirmed by 13C NMR spectroscopy and extract evaluation combined with 1H NMR spectroscopy.
    Notes: Für die Copolymerisation von 1,3-Butadien mit Propylenoxid wurde nach dem Vergleich der drei Katalysatorsysteme Nd(Oct)3/Al2Cl3ET3/Al(i-But)3, Ni(Oct)2/ BF3OEt2/AlEt3 und Al(i-But)3/I2/TiCl4 das Titankatalysatorsystem eingesetzt. Neben dem Einfluß der Monomerzusammensetzung auf den Umsatz, die Microstruktur, die Copolymerzusammensetzung, die Molmassen sowie die Molmassenverteilungen wurden auch die Polymerisationszeit und das Aluminium/Titan-Verhältnis untersucht. Die Copolymerisationsparameter wurden nach Kelen-Tüdős zu rButadien = 0,9 und rPropylenoxid = 3,9 bestimmt. Der Copolymernachweis erfolgte über 13C-NMR-Spektroskopie und Extraktionsuntersuchungen in Verbindung mit 1H-NMR-Spektroskopie.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052390110
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  • 10
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    Phosphorus-containing polyurethanes based on bisphenol A via N-alkylation (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 191-199 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Phosphorhaltige Polyurethane (PU-P) auf der Basis von Bisphenol A wurden durch N-Alkylierung hergestellt und mittels IR- und 1H NMR-Spektroskopie charakterisiert. Physikalische und thermische Eigenschaften dieser Polyurethane wurden mittels Differentialkalorimetrie, Thermogravimetrie, Röntgenbeugung und Untersuchungen der Löslichkeit, der Feuerbeständigkeit (Sauerstoffindex, LOI) und der reduzierten Viskosität bestimmt. Die Glastemperaturen der N-alkylierten Polymeren sanken von 120°C für das Ausgangspolymere bis auf 29°C für das N-alkylierte Polyurethan mit 2 Gew.-% Phosphor. Die Viskosität der N-alkylierten Polyurethane nahm von 0,36 dL g-1 auf 0,24 dL g-1 ab. Die phosphorhaltigen Polyurethane besitzen eine geringere thermische Stabilität und bessere Löslichkeit sowie höhere Feuerbeständlgkeit als das Ausgangspolymere. Die Röntgenstreuexperimente ergaben, daß ein erhöhter Phosphorgehalt der Polyurethane die Kristallinität herabsetzt.
    Notes: Phosporus-containing polyurethanes (PU-P) based on bisphenol A were prepared by N-alkylation. The structures of N-alkylated polyurethanes were characterized by IR and 1H NMR spectra. Physical and thermal properties of the phosphorus-containing polyurethanes were investigated with differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray diffraction, tests of solubility, limiting oxygen index (LOI) and reduced viscosity. Tg of the N-alkylated polymers decreased from 120°C for the starting polymer to 29°C of the 2.0 wt.-% phosphorus-containing polyurethanes. The viscosity of N-alkylated polyurethanes also decreased from 0.36 dL g-1 to 0.24 dL g-1. The thermal stability of polyurethanes decreased on the introduction of phosphorus groups. The LOI values of polyurethanes showed that fire resistance of phosphorus-containing polyurethanes was enhanced. X-ray diffraction measurements showed that the increased phosphorus content was accompanied by decreased crystallinity of the polyurethanes. The solubility of PU-P was improved.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052390116
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  • 11
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    Are cured thermoset resins inhomogeneous?Lecture presented at International Symposium on Advanced Network-Polymers, Kansai University (ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1995 (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 1-15 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: This question was addressed using various methods to monitor the process of curing and state of the final network. Attention was particularly focused on the possible inhomogeneous network formation as a consequence of the crosslinking process. An analysis of experimental data has revealed that some cured resins can be considered as homogeneous as the corresponding uncrosslinked materials. Resins cured by simple stepwise alternating chemistries, with good compatibility of components, usually fulfill the criterion of homogeneity. A family of epoxy resins cured with polyamines belongs to this category. Nodular structures seen by electron microscopy are a result of interaction of the electron beam or etching. Such structures are also observed for uncrosslinked polymers investigated under the same conditions. Formation of inhomogeneities in a number of thermoset systems is due to (a) chainwise mechanism of network formation with fast propagation inducing cyclization and steric volume exclusion and (b) poor compatibility of components of the system made stronger by increasing molecular weights and crosslinking during curing. Networks formed by freeradical polymerization and copolymerization of polyvinyl monomers can serve as an example of crosslinking-driven formation of inhomogeneities.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052400101
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  • 12
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    Design of network polymers by photopolymerizationLecture presented at the “International Symposium on Advanced Network Polymers, Kansai University” (ISANKU), at Kansai Univeristy, Suita, Osaka, Japan, on December 5-6, 1995. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 83-90 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The base and transition metal catalyzed isomerization of allyl and crotyl ethers affords a facile, high yield route to the preparation of a variety of mono-, di-, and multifunctional 1-propenyl and 1-butenyl ethers. Employing this novel method, monomers containing epoxide, ester, ether carbonate and urethane groups can be prepared from their readily available allyl and crotyl precursors. In general, these monomers display very high reactivity in cationic polymerizations. In our work, we have focused on photoinduced cationic polymerizations of these monomers using diaryliodonium and triarylsulfonium salt photoinitiators. To study these very fast photopolymerizations, extensive use of real-time infrared spectroscopy was made. Employing this technique, the effects of monomer and photoinitiator structure on the rates of polymerization were studied.
    Additional Material: 1 Ill.
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    Designing elastomer network for desired tire performance characteristics (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 137-149 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Rubber elasticity is associated with changes in configurational entropy of a long chain. Because the chain cannot change its configuration instantaneously, there is a time delay in deformation to an applied force. This delayed response is the source of viscoelasticity and hysteresis energy loss of elastomer networks. Many tire performance properties are related to the viscoelasticity of tire components. Wet and dry traction of tire is related to the energy loss of the tread material at very high frequencies. On the other hand, rolling resistance of tire is characterized by the energy loss of tread material at relatively low frequencies. The dynamic viscoelastic properties of elastomer network shows characteristic zones on a frequency scale. At very high frequencies the energy loss is controlled by the segmental motions of the polymer chain. At lower frequencies the energy loss is related to the longer range motions of the chain. A series of polymers was synthesized to study the effect of micro- and macro-structure of the polymer on the viscoelastic properties of tread compounds and their tire performance properties. As expected from the theory, the wet traction of the tire was highly correlated to the segmental motions of the chains; namely, the glass transition temperature of the polymer. The energy loss of the compounds at a higher temperature, however, was related to the macrostructure of the polymer chain. Those examples illustrate that the fundamental understanding of the theory of elastomer network allows a tire engineer to obtain the best balance of tire performance characteristics.
    Additional Material: 7 Ill.
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    Molecular design of novel network polymers (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 171-180 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Cationic, anionic, and radical ring-opening polymerization of spiro and bicyclic monomers, and their application to network polymers have been developed. Bicyclo orthoesters (BOEs), spiro orthoesters (SOEs), and spiro orthocarbonates (SOCs) were polymerized by cationic double ring-opening. Bicyclobis(γ-butyrolactone)s and spirobis(γ-butyrolactone)s were copolymerized with epoxides by anionic alternating ring-opening. Polymers from SOCs bearing exomethylene groups consisted of ring-opened and vinyl polymerized units. The degree of ring-opening of SOCs depended upon the number of rings and steric hindrance. The radical polymerization of vinylcyclopropanone cyclic acetals depended on the ring-size. With the monomers bearing 5- and 6-membered acetal rings, single ring-opened polymers were obtained. With the monomer bearing 7-membered acetal ring, the polymer mainly consisted of double ring-opened unit. These monomers could be crosslinked by bifunctionalization. Poly(cyclic orthoester)s linked by covalent bonds with dithiols to bifunctional SOEs were crosslinked by acid catalysts, and the reversible crosslinking-depolymerization system could be controlled by temperature.
    Additional Material: 1 Ill.
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    Characterization of polyurethane network elastomers (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 205-211 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyester urethane network elastomers with incorporated hard segment oligomers have been prepared by poly(ethylene adipate)glycol (PEA), 2,4-tolylene diisocyanate (TDI), and 1,4-butanediol (BD). These hard segment oligomers were hydroxy-terminated oligomers ([BD-TDI]n-BD; n=1,3), obtained by reacting BD with TDI. Concentrations of allophanate as a cross-linking site were determined by the amine degradation method. Hard segment moieties were obtained by a novel selective hydrolysis of soft segments in the elastomers. Molecular weight distributions of hard segment were measured by means of GPC. Mechanical and thermal properties were measured. Dependence of rubber elasticity on physical cross-linking between normal elastomers and the elastomers with incorporated hard segment oligomers were discussed.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052400119
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  • 16
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    Network formation and swelling behavior of photosensitive poly(vinyl alcohol) gels prepared by photogenerated crosslinkingPoster presented at the “International Symposium on Advanced Network-Polymers, Kansai University” (ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1995. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 231-239 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Poly (vinyl alcohol) with pendent styrylpyridinium groups (SbQ) is insolubilized by photoirradiation. An association takes place in SbQ groups. The association of polymer chains becomes marked with increasing the number of SbQ groups. Mainly intermolecular crosslinks were formed. Transparent and homogeneous macrogels consisting of several intermolecular crosslinks are obtained.The proportion of the free water to the bound water in PVA-SbQ gels was 3.3-2.9 despite of the large change in conversion of photodimerization of SbQ groups, x=0.27-0.58. The water uptake after swelling of the gels in water increased 6-27 times compared to the original weight at pH=7. The higher the degree of photocrosslinking, the lower was the degree of swelling. The water diffusion coefficients, D, were (2.2-5.8) × 10-5 cm2 S-1 for a 88% saponified PVA with 1 . 3 mol% SbQ groups. The volume of the gel increased discontinuously about 10-fold for the 99% saponified PVA with 0 . 096 mol% SbQ and 51% water (49% acetone). The acetone concentration at the transition decreased with increasing the degree of saponification of the PVA.
    Additional Material: 10 Ill.
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    Hydrogels for biomedical use based on 1-vinyl-2-pyrrolidone crosslinked with macromonomers (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 151-160 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Durch anionische Copolymerisation von Allylmethacrylat und Methylmethacrylat wurden Makromonomere unterschiedlicher Kettenlänge mit durchschnittlich drei Allyl-Doppelbindungen pro Kette hergestellt́ und mit NMR-Spektroskopie und Gelpermeationschromatographie charakterisiert. Durch Copolymerisation der Makromonomeren mit 1-Vinyl-2-pyrrolidon wurden dreidimensionale Strukturen erhalten. Die optischen und mechanischen Eigenschaften der Produkte wurden untersucht, und die Quellungseigenschaften und Vernetzungsgrade wurden bestimmt. Die Copolymereigenschaften wurden durch Makromonomere mit Kettenlängen bis 40 Einheiten nur wenig beeinflußt. Bei Kettenlängen über 50 Einheiten wurde eine leichte Abnahme der Wasseraufnahmefähigkeit und eine deutliche Erhähung des Elastizitätsmoduls beobachtet. Die Vernetzungsgrade hängen von der Makromonomer-Kettenlange ab; eine merkliche Erhöhung aufgrund der groößeren Zahl an Methyl-Methyl-Wechselwirkungen wurde bei Kettenlangen über 50 Einheiten festgestellt. Die Copolymeren zeigen günstige Festigkeits-Dehnungs-Eigenschaften und einen geringen Gehalt an wasserlöslichen Extrakten, in denen durch IR-Spektroskopie 1-Vinyl-2-pyrrolidon-Homopolymere identifiziert wurden. Obwohl mit allen untersuchten Makromonomeren gute Resultate erzielt wurden, scheint für die Copolymerisation mit 1-Vinyl-2-pyrrolidon das Makromonomere mit 50 Einheiten am besten geeignet.
    Notes: Macromonomers of various chain lengths with an average of three allyl double bonds per chain were prepared by anionic copolymerization of allyl methacrylate with methyl methacrylate. The macromonomers were characterized by gel permeation chromatography and nuclear magnetic resonance. The macromonomers were then copolymerized with 1-vinyl-2-pyrrolidone to form three-dimensional structures. Their optical, swelling and mechanical properties were studied and the crosslinking efficiency was determined. The copolymer properties are not greatly affected by macromonomer chain lengths up to 40-mers; above 50-mers there is a slight decrease in the equilibrium water content and a significant increase in the modulus of elasticity. The crosslinking efficiency depends on the macromonomer chain length; a marked increase was observed for the 50-mer because of a greater number of methyl-methyl interactions. Copolymers have favourable strength-strain properties and a low content of water-soluble extracts, in which the IR analysis demonstrated the presence of 1-vinyl-2-pyrrolidone homopolymers. In spite of the good results obtained for all the macromonomers described in this work, the 50-mer seems to be optimal for copolymerization with 1-vinyl-2-pyrrolidone.
    Additional Material: 6 Ill.
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    Zur härtung von diandiglycidylether mit anhydridmodifizierten phenolischen härtern und zu vergleichbaren in situ-reaktionen (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 201-213 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: The curing of diglycidyl ether of bisphenol A (DGEBA) with 2,6-dimethylol-p-cresol modified by hexahydrophthalic acid anhydride was investigated and compared with the analogous in situ curing of DGEBA, hexahydrophthalic acid anhydride and 2,6-dimethylol-p-cresol. The chemical reactions were investigated by means of titration and different spectroscopic and chromatographic methods. It was examined whether the less complicated and therefore cheaper in situ reaction delivers postcured products with equal or better properties. Furthermore, it was investigated whether the results are similar using technical phenolic hardeners.
    Notes: Die Härtung von Diandiglycidylether (DDGE) mit hexahydrophthalsäureanhydridmodifiziertem 2,6-Dimethylol-p-kresol (HHPSA-DMPK) wurde untersucht und mit der in situ durchgeführten Vernetzung von DDGE mit Hexahydrophthalsäureanhydrid (HHPSA) und 2,6-Dimethylol-p-kresol (DMPK) verglichen. Die chemischen Reaktionen wurden durch Titration der Epoxidgruppen und mit verschiedenen spektroskopischen und chromatographischen Methoden untersucht. Es wurde geprüft, ob die weniger aufwendige und daher preiswertere in situ-Härtung zu Produkten mit gleichen oder besseren Endeigenschaften führt. Weiterhin wurde die Übertragbarkeit der Ergebnisse auf den Einsatz technischer Phenolharzhärter getestet.
    Additional Material: 9 Ill.
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    Characterization and application of poly(vinyl alcohol)/starch composite as a sizing agentResults published in this paper were extracted from the Ph. D. Thesis to be submitted by M. M. Hashem to Cairo University, Egypt. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 241 (1996), S. 149-163 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Zur Entwicklung neuartiger ökologisch verträglicher makromolekularer Schlichtemittel wurden in früheren Arbeiten Copolymerisationsreaktionen zwischen Polyvinylalkohol (PVA) und Stärke unter Verwendung von chemisch reaktiven bifunktionellen Verbindungen wie N-Methylolacrylamid beschrieben. Im Rahmen dieser Arbeit werden die physikochemischen Eigenschaften des resultierenden Copolymeren untersucht. Von Bedeutung sind hierbei insbesondere Merkmale wie Molekulargewichtsverteilung, Klebekraft, Stabilität, Löslichkeit sowie rheologische Eigenschaften. Derartige Kenntnisse über die physikochemische Beschaffenheit der PVA-Ausgangsverbindung sowie des makromolekularen Endproduktes sind eine wesentliche Voraussetzung für die Entwicklung von neuen Produkten, die als wasserlösliche, recycelbare Schlichtemittel zur Anwendung in der Textilindustrie kommen können.
    Notes: A macromolecular sizing agent based on the copolymerization of poly(vinyl alcohol) (PVA) with hydrolysed starch was prepared using the chemically reactive bifunctional compound N-methylolacrylamide. Detailed characteristics of the resultant PVA/N-methylolcarbamoylethylated starch copolymer were studied where emphasis has been placed on solubility, rheological properties, molecular weight distribution, adhesive power and stability. Elucidation of the nature of the macromolecular segments of both N-methylolcarbamoylethylated PVA as well as PVA/N-methylolcarbamoylethylated starch copolymer fulfilled the prerequisite to tailor PVA/starch copolymer which is appropriate for application as a water-soluble recyclable sizing agent by ultrafiltration.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052410112
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    Peripherally restraining type rubber bearingLecture presented at the “International Symposium on Advanced Network-Polymers, Kansai University” (ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1995. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 151-162 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Seismic isolation was reconfirmed to be extremely efficient for the protection of buildings, and hence human life, on the occasion of the Great Hanshin Earthquake. Rubber bearings are placed under the buildings for isolation, and thus the type of rubber bearings is a dominant factor for efficient isolation. In this report, the performance of peripherally restraining type rubber bearing (PRB) was examined where its contracted model was found to simulate the performance of full scale PRB precisely. Damping ratio and vertical spring constant of PRB are as good as the existing ones. PRB showed lower critical shear strain, but it was concluded that no problems were found for the actual use of PRB.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052400113
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    Computational study of network formation of phenolic resinsPoster presented at the “International Symposium on Advanced Network-Polymers, Kansai University” (ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1995. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 181-186 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The network formation of phenol-formaldehyde resin was investigated by the Monte Carlo (MC) simulation technique. The observed value of the gel point, pc, was exactly determined as a critical extent of reaction, where the Mw/Mn in soluble parts is maximum. The MC simulation with the cubic percolation theory was applied to the gelation of phenolic resins and gave an exact gel point, which was in excellent agreement with the observed value of pc. The simulation showed that the intramolecular reaction occurred frequently with increasing the gel fraction beyond the gel point. The structural analysis of the maximum cluster with the computer strongly supported the contribution of the intramolecular reaction to the network formation of the gel.
    Additional Material: 5 Ill.
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    PH-induced structure change of poly(vinyl alcohol) hydrogel crosslinked with poly(acrylic acid)Poster presented at the “International Symposium on Advaned Network-Polymers, Kansai University”(ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1955. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 213-219 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The structure of the hydrogel of poly(vinyl alcohol) (PVA) and poly(acrylic acid) (PAA) was investigated by small angle X-ray scattering (SAXS) of synchrotron radiation. A physically crosslinked blend gel, which was prepared by repetitive freezing and thawing of an aqueous solution of PVA and PAA, could be chemically crosslinked by esterfication of PVA with PAA even in the hydrogel state. The chemical crosslinking induced the destruction of physical crosslinks into a folded structure, indicating that the chemical crosslinking proceeds at the sites around the physical crosslinks that contain PVA and PAA in much higher concentration than other portion of the gel. The pH-induced structure changes of the PVA hydrogels, chemically crosslinked with poly(acrylic acid) (PAA) were investigated by SAXS on the samples of various chemical crosslinking time. The gels were shrunk at pH4, and swollen at pH8. The results of SAXS showed, that the Porod slope changed with chemical crosslinking time from -3.5 to -2.9 at pH4, and from -2.9 to -2.4 at pH8. The results suggest that a folded structure as a structural domain, which is characterized by fractally rough interface, tends to change into the structure that corresponds to percolation cluster, particularly at pH8. The gels immersed in pH8 showed a remarkable structure change accompanying swelling. The results revealed that a conformational change of PAA chains, induced by the pH change, can be explained by the presence of a structural domain in the gel network, where both PVA chains and PAA chains get entangled and partially form a interpenetrating polymer network(IPN).
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052400120
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    Polyurethane-elastomer-actuatorPoster presented at the “International Symposium on Advanced Network-Polymers, Kansai University” (ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1995. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 221-229 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyurethane elastomers were investigated as electrically active materials for actuators. Components in hard segment and soft segment in the elastomers were varied. The elastomers with excellent electrostrictive properties were limited to those which had soft segments of polyesters and polylactones. It turned out, that the elastomers, whose soft segments are polyethers are electrically inert under the experimental conditions. The chemical structure of the hard segment seems not to influence to the electrostrictive property. The charging and discharging process was investigated. The charging process was found to proceed simultaneously with the contracting process caused by the electric field, suggesting that the orientation of the soft segment in the elastomer plays critical rolls in the electrostrictive action. In the elastomer, which has a soft polyether segment and was inactive to the electric field, could be actuated very efficiently when the elastomer was swollen with dimethyl sulfoxide. We conclude that the polyurethane elastomer, whose soft segment has chemical bonds with a relatively large dipole moment, can be actuated by the electric field application, and that even the elastomer, whose soft segment is inactive, could be actuated in the presence of a solvent with a large dipole moment. Thus, the concept found with the gel, could be applied to an elastomer, the soft segment of which plays partly the roll of the solvent in the gel.
    Additional Material: 5 Ill.
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    Preparation of oxidized 6-O-glycolchitosan, pH sensitivity of its aqueous solution and of its cross-linked hydrogel (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 263-273 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Chitosan and 6-O-glycolchitosan, a water-soluble chitosan derivative, were oxidized by periodate. In the case of chitosan, only degradation products were obtained. With 6-O-glycolchitosan, however, water-soluble amphoteric polyelectrolyte derivatives of chitosan having higher molecular weight were obtained. The oxidized 6-O-glycolchitosan (OX-GC) showed a pH sensitive change of viscosity in aqueous solution. Moreover, the OX-GC hydrogel, cross-linked with glutaraldehyde, showed a pH sensitive swelling behavior. The OX-GC showed biodegradation behavior by lysozyme after acetylation.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052400125
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    A polymer network of unsaturated polyester and bismaleimide resins: Yielding and fracture behaviour (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 241 (1996), S. 11-29 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Das Fließ- und Bruchverhalten eines durch das gleichzeitige Härten eines ungesättigten Polyesters (UP) und eines wärmehärtbaren Bismaleimidharzes (BMI) erhaltenen quervernetzten Polymernetzwerkes wurde über einen weiten Temperatur- und Beanspruchungsbereich untersucht. Die Fließspannung σy und der Youngsche Elastizitätsmodul E steigen bei Zunahme der Spannungsbeanspruchung bzw. bei Absinken der Temperatur. Zudem steigen bei ansonsten gleichen Testbedingungen σy und E mit zunehmendem BMI-Gehalt im Blend. Andererseits wurde eine Beeinflussung des Bruch-Parameters Kc durch die Gegenwart des BMI nicht beobachtet. Der Fließprozess wurde sowohl mit Hilfe der Theorie von Argon als auch mit der von Bowden untersucht; die daraus abgeleiteten Molekül-Parameter wurden mit der bei der Härtung gebildeten Molekularstruktur in Beziehung gesetzt.
    Notes: The yielding and the fracture behaviour of an intercrosslinked polymer network obtained by the simultaneous curing of an unsaturated polyester (UP) and a thermosetting bismaleimide resin (BMI) was investigated in a wide range of temperatures and testing rates. The yield stress σy and the Young's modulus E increase by increasing the testing rate and decreasing temperature. Moreover, under the same testing conditions, σy and E increased as the BMI content in the blend was enhanced. On the other hand, it was found that the fracture parameter Kc was not affected by the presence of BMI. The yielding process was analyzed using the theories both of Argon and Bowden and the molecular parameters derived there were related to the molecular structure of the network developed upon curing.
    Additional Material: 13 Ill.
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    Fluorinated poly(1,3,4-oxadiazole-imide-amide)s (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 242 (1996), S. 159-169 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Dicarbonsäuredichloride mit sowohl Hexafluorisopropyliden-Brücken und Imidringen im Molekül wurden mit p-Aminobenzhydrazid oder Mischungen aus aromatischen Diaminen und p-Aminobenzhydrazid oder Terephthaldihydrazid zu Poly(hydrazidimid-amid)en umgesetzt, die anschließend zu neuen fluorhaltigen Poly(1,3,4-oxadiazol-imid-amid)en mit verschiedenem Amid/Oxadiazol-Verhältnis cyclodehydriert wurden. Diese sind in polaren amidischen Lösungsmitteln löslich; aus solchen Lösungen lassen sich flexible Filme herstellen. Die Glasübergangstemperaturen liegen zwischen 254°C und 325°C. Sie sind bis zu 415-450°C thermisch stabil.
    Notes: A series of new fluorinated poly(1,3,4-oxadiazole-imide-amide)s containing various ratios of amide/oxadiazole groups in the repeating unit have been prepared by cyclodehydration of the corresponding poly(hydrazide-imide-amide)s resulting from the reaction of diacid dichlorides incorporating both hexafluoroisopropylidene bridges and imide rings with p-aminobenzhydrazide or with mixtures of certain aromatic diamines and p-aminobenzhydrazide or terephthalic dihydrazide. The new polymers are soluble in polar amidic solvents and can be processed into flexible films by casting from solution. Their glass transition temperatures are in the range 254-325°C and they are thermally stable up to 415-450°C.
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    Electric resistivity of hydroscopic copoly(ester-ether)s containing zwitterionic units and their utilization for antistatic modification of polyester fiber (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 242 (1996), S. 171-181 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Blockcopoly(ester-ether) mit verschiedenen ionischen Einheiten wie Sulfobetain (S-Betain), Carbobetain (C-Betain) und Ammoniumtosylat wurden hergestellt und hinsichtlich ihrer Eignung als antistatische Modifikatoren für Polyethylenterephthalat (PET)-Fasern untersucht. Die ionischen Segmente wurden aus N,N-Bis(2-hydroxyethyl)methylamin generiert und statistisch mit den Polyester- und Polyoxyethylen(PEO)-Einheiten cokondensiert. Aus den Copolymeren mit S-Betain-Einheiten wurden im Schmelzspinnverfahren dicke Filamente hergestellt und deren elektrischer Widerstand bestimmt. Abhängig von der Zusammensetzung (25-75 Gew.-% PEO, 1-2 mol-% S-Betain) wurden Widerstände zwischen 108 und 1010 Ω cm-1 gemessen. Die drei copolymerartigen Modifikatoren wurden mit PET durch Blendspinnen gemischt. Die so erhaltenen PET-Fasem zeigen nicht nur gute mechanische sondern auch verbesserte antistatische Eigenschaften. Die Fasern aus dem S-Betain enthaltenden Copolymeren weisen dabei die kürzeste Halbwertszeit des Abbaus der elektrostatischen Ladung auf, obwohl der Oberflächenwiderstand dieses Materials in der Größenordnung 1013 Ω cm-2 dem Wert der mit C-Betain und Ammoniumtosylat hergestellten Fasem ähnlich ist. Die PET-Fasern bewahren ihre guten antistatischen Eigenschften auch nach dem Fäben und wiederholtem Waschen, da sowohl die hydrophilen als auch die ionischen Gruppen an den Polyesterketten fixiert sind.
    Notes: Block copoly(ester-ether)s containing different ionic units, i.e., sulfobetaine (S-betaine), carbobetaine (C-betaine), and ammonium tosylate, were prepared and evaluated as antistatic modifiers of PET fiber. The ionic units were readily derived from N,N-bis(2-hydroxyethyl)methylamine and co-condensed randomly with the polyester and poly(oxyethylene) (PEO) units. For the copolymers containing S-betaine units, a thick filament was melt-spun to evaluate their apparent electric resistivity. Depending on the unit compositions (25-75 wt.-% of PEO and 1-2 mol-% of S-betaine), resistivities ranging from 108 to 1010 Ω cm-1 were obtained. Then, the three copolymer-type modifiers were blended with poly(ethylene terephthalate) (PET) by the ordinary blend-spinning technique. The blend PET fibers obtained showed not only good mechanical properties, but also improved antistatic properties. Particularly, the fiber blended with the copolymer containing S-betaine units had the shortest half-life time of leakage of static charge, although the surface area resistivity, being in the order of 1013 Ω cm-2, was similar to that of the fibers blended with the copolymers containing C-betaine and ammonium tosylate units. These blend PET fibers were found to retain good antistatic properties even after dyeing and repeated washings, because both the hydrophilic and ionic groups are immobilized with the polyester chains.
    Additional Material: 3 Tab.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052420112
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    Untersuchungen zum reaktionsverhalten beim vorliegen von depolymerisationsreaktionen. Untersuchung von copolymerisationen des α-methylstyrols (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 243 (1996), S. 11-37 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: For radical copolymerizations of α-methylstyrene (MS) with methacrylonitrile (MAN) and of MS with acrylonitrile (AN) studies were carried out to examine postulations of kinetic models known from literature, in particular the terminal model with chain-length-independent and chain-length-dependent depolymerization steps. The results of investigations were based on measurements of the sequence length distributions from 13C-NMR spectra. Analyses of MS/MAN copolymers with various compositions were carried out. Reaction parameters and depolymerization constants depending on temperature were calculated. The values of enthalpy and entropy of polymerization and the ceiling temperature were computed for MS to ΔH = 26,5 ± 0,5 kJ mol-1, ΔS = 95 ± 5 J mol-1 K-1, Tceiling = 65 ± 1°C. The terminal model with depolymerization steps turned out to be wrong for the accurate description of the polymerization behaviour in case of the tested systems. Results clearly show important penultimate effects. At the point of knowledge, the description of the polymerization behaviour in terms of a penultimate model with depolymerization steps are suggested.
    Notes: Für die radikalischen Copolymerisationen von α-Methylstyrol (MS) mit Methacrylnitril (MAN) sowie MS mit Acrylnitril (AN) wurden Untersuchungen zur Prüfung der in der Literatur postulierten kinetischen Modelle des „sequenzlängenunabhängigen“ bzw. „sequenzlängenabhängigen“ Terminalmodells mit Depolymerisationsschritten durchgeführt. Sie basieren auf Analysen der Sequenzverteilungen aus 13C-NMR-Spektren. Resultate von 13C-NMR-Untersuchungen an MS/MAN-Polymeren variabler Zusammensetzung werden vorgestellt. Reaktionsparameter und Gleichgewichtskonstanten wurden direkt aus den Informationen der 13C-NMR-Spektren für das Terminalmodell mit Depolymerisationsschritten in Abhängigkeit von der Reaktionstemperatur der Polymeren bestimmt. Hieraus konnten die Polymerisationsenthalpie ΔH = 26,5 ± 0,5 kJ mol-1, die Polymerisationsentropie ΔS = 95 ± 5 J mol-1 K-1 sowie die Ceilingtemperatur Tceiling = 65 ± 1°C für MS bestimmt werden. Es wurde nachgewiesen, daß im Rahmen der Terminalnäherung auch mit Berücksichtigung von Depolymerisationseinflüssen keine adäquate Beschreibung des Copolymerisationsverhaltens im Falle der untersuchten Systeme möglich ist. Vielmehr konnten als Ergebnis der Untersuchungen sowohl in Copolymeren von MS mit AN als auch mit MAN signifikante Penultimate-Effekte nachgewiesen werden. Aufbauend auf diesen Ergebnissen wird die Anwendung eines auf einer Penultimate-Näherung basierenden Modells, welches auch das Gleichgewicht in den Wachstumsreaktionen von MS berücksichtigt, zur theoretischen Vorhersage des Copolymerisationsverhaltens vorgeschlagen.
    Additional Material: 14 Ill.
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    Epoxidation of cis-cyclooctene with molecular oxygen catalyzed by magnesium oxide supported polytitazane cobalt (III) complexes (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 243 (1996), S. 69-75 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Ein auf Magnesiumoxid aufgebrachter Polytitazan-Cobalt (III)-Komplex diente als effektiver Katalysator für die Epoxidierung von cis-Cycloocten mit molekularem Sauerstoff bei Normaldruck in Gegenwart von Isobutyraldehyd als Reduktionsmittel. Nach XPS-Untersuchungen wird Cobalt (III) durch den mehrzähnigen Stickstoffliganden des Polytitazans stabilisiert. Bei 25°C beträgt der cis-Cycloocten-Umsatz nach fünf Stunden 95,2%, mit einer Selektivität von 100% für das cis-Cyclohexylenoxid. Der Katalysator Kann mindestens neun Mal ohne Aktivitätsverlust verwendet werden.
    Notes: Magnesium oxide supported polytitazane cobalt (III) complex is demonstrated as an effective catalyst for the epoxidation of cis-cyclooctene with molecular oxygen at atmospheric pressure in the presence of isobutyraldehyde as the sacrificial reductant. XPS data show that the high-valent cobalt (III) is stabilized by the multidentate nitrogen ligand of polytitazane. The conversion of cis-cyclooctene is as high as 95.2% with 100% selectivity to the cis-cyclooctene oxide at 25°C within 5 h. The catalyst can be used at least nine times without loss of its activity.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052430106
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    Phase diagram and crystallization of polycarbonate/poly-∊-caprolactone blends (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 243 (1996), S. 177-187 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Es wird über die Gleichgewichts-Schmelzpunktsdepression von Polycarbonat aus Bisphenol A (PC) in Mischungen mit Poly-∊-caprolacton (PCL) berichtet. Hierzu wird ein Modell entwickelt, das den gekrümmten Verlauf der gemessenen Hoffman-Weeks-Plots zu erklären vermag. Es berücksichtigt die Konzentrationsinhomogenitäten, die mit fortschreitender Kristallisation an der Kristallwachstumsfront entstehen. Die gelegentlich beobachtete Schmelzpunktsdepression der PCL-Komponente wird diskutiert. Der Flory-Hugginssche Wechselwirkungsparameter wird zu -0,09 berechnet; aus diesem kleinen Wert muß geschlossen werden, daß die Mischungspartner enthalpisch nur schwach wechselwirken. Der merkliche Abfall der Glastemperatur des PC nach Einmischen von PCL bewirkt eine beträchtliche Kristallisation aus der Schmelze; es können PC-Kristallinitätsgrade bis zu 25% erreicht werden.
    Notes: It is reported on the equilibrium melting point depression of polycarbonate from bisphenol A (PC) in its blend with poly-∊-caprolactone (PCL). To this end, a model which explains the bended course of the measured Hoffman-Weeks plots is developed which takes into account the composition changes at the crystal growth front upon progressive crystallization. The occasional melting point depression of the PCL component is discussed. The calculated Flory-Huggins parameter of χ12 ≍ -0.09 indicates only weak enthalpic interactions. The remarkable drop in the glass transition temperature of PC with blending allows PC degrees of crystallinity up to 25% upon crystallization from the melt.
    Additional Material: 6 Ill.
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    Synthesis and properties of powdery hydrogels based on acrylamide, methacrylamide, and their N-substituted derivatives (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 243 (1996), S. 151-159 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Leicht vernetzte Hydrogele auf der Basis von Acrylamid, N-(1,1-Dimethyl-3-oxobutyl)acrylamid, N,N-Dimethylacrylamid, Methacrylamid, N-(2-Hydroxypropyl)-methacrylamid und N-[Tris(hydroxymethyl)methyl]methacrylamid wurden in Form von pulverigen Substanzen synthetisiert, die aus Aggregaten sehr kleiner Partikel (∼10-1 μm) bestehen. Die pulverartigen Hydrogele wurden durch Fällungspolymerisation in Aceton und Diethylether unter Verwendung von N,N′-Methylenbisacrylamid und Ethylendimethacrylat als Vernetzungsmittel synthetisiert. Es wurden die Abhängigkeiten des Quellungsgrades in Wasser, der Größe, des Aggregationsgrades und der spezifischen Oberfläche von Partikeln, und des Inhalts von wasserlöslichen Substanzen in den Hydrogelen von den Bedingungen ihrer Synthese verfolgt. Die Eignung einzelner der synthetisierten Hydrogele für die Herstellung von Silikon-kautschuk-Hydrogel-Kompositen wird diskutiert.
    Notes: Lightly crosslinked hydrogels based on acrylamide, N-(1,1-dimethyl-3-oxobutyl)-acrylamide, N,N-dimethylacrylamide, methacrylamide, N-(2-hydroxypropyl)methacrylamide and N-[tris(hydroxymethyl)methyl]methacrylamide were synthesized in form of fine powders, consisting of aggregates of very small (∼10-1 μm) particles. The powdery hydrogels were obtained by precipitation polymerization in acetone and diethyl ether, using N,N′-methylenebisacrylamide and ethylene dimethacrylate as crosslinking agents. Dependences of water-swellability, particle size, aggregation, specific surface and content of the uncrosslinked water-soluble polymers and low-molecular-weight substances in the hydrogels on the conditions of their synthesis were studied. Suitability of particular powdery hydrogels synthesized for the preparation of silicone rubber-hydrogel composites is discussed.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052430113
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    Polycarbonat-ein vielseitiger werkstoff mit zukunft (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 244 (1997), S. 43-66 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The market development of bisphenol-A-polycarbonate has shown higher growth than any other engineering thermoplastic. The reasons can be found in the permanent improvement of the cost/performance-relationship and in the technical use of the variability of the basic structure. Incorporation of specific monomer units leads to tailor-made properties for a wide range of applications, as for example medical devices, electronic parts and glazing.This process has not yet slowed down, rather it is accelerated by new results from research and development. The improvement of flaw behavior and pit replication for new grades of materials for the next generation of compact discs, new grades that can be sterilized by γ-radiation without degradation and the microstructuring by low-energy laser systems are examples for the ongoing expansion of polycarbonate applications. Surface modification by hardcoatings with nanosized particles will allow to enter the fast growing market of glazing.
    Additional Material: 27 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052440103
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    Polyamide, polyester und polyoxymethylen. Die klassischen technischen kunststoffe und ihre perspektiven (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 244 (1997), S. 67-92 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Polyamide, Polyester und Polyoxymethylen sind mit einem weltweiten Verbrauch von derzeit 2,4 Mio t pro Jahr wichtige technische Kunststoffe. Sie werden aufgrund ihrer besonderen Eigenschaftsprofile überwiegend im Fahrzeugbau und in der Elektroindustrie für hochbelastete Funktionsbauteile eingesetzt. Der vorliegende Beitrag behandelt Polymerisationswege, Eigenschaften und ausgewählte neue Entwicklungen dieser Polymerklassen.Teilaromatische Polyamide stoßen durch ihre Dimensionsstabilität und thermische Belastbarkeit in Anwendungen vor, die bisher Duromeren oder Metallen vorbehalten waren. Glasfaserverstärkte Polyamide mit besonders hoher Dauerwärmebeständigkeit übemehmen wichtige Funktionen im Motorbereich von Fahrzeugen. Polyamid-Blends sind als Karosseriewerkstoffe ein Schlüssel zu leichten Autos mit niedrigem Treibstoffverbrauch. Halogenfrei flammgeschützte Polyamide erhöhen Sicherheit und Umweltverträglichkeit in brandgefährdeten Anwendungsbereichen.Polybutylenterephthalat als technisch wichtigster Polyester eröffnet in Mischung mit amorphen Polymeren neue Perspektiven durch geringerenVerzug und bessere Oberfläche bei glasfaserverstärkten Teilen. Polybutylennaphthalat erweitert den Anwendungsbereich zu höheren Temperaturen. Von Polybutylenterephthalat abgeleitete Copolyester sind biologisch abbaubar und daher vielversprechend für kompostierbare Folien.Polyoxymethylen-Copolymere haben ihre Stärke in der günstigen Kombination aus Steifigkeit, Dimensionsstabilität, Gleit/Reibe-Verhalten und Beständigkeit gegen heißes Wasser und Kraftstoff.Aufgrund ihres hohen und noch weiter steigerungsfähigen Leistungsvermögens werden Polyamide, Polyester und Polyoxymethylen das in den letzten Jahren gezeigte Wachstum in Zukunft weiter ausbauen können.
    Notes: Polyamide, polyester and polyoxymethylene having presently a worldwide sales volume of 2,4 million tons a year are important engineering thermoplastics. Based on their special property profiles they are mainly used in the automotive and electronic industry for high performance functional parts. This contribution presents polymerisation processes, properties, and selected new developments for these polymer classes.Semiaromatic polyamides due to their dimensional stability and thermal resistance lend themselves to applications which were so far reserved for thermosets or metals. Glass fiber reinforce polyamides designed to have the highest possible heat ageing resistance can take important functions under the hood. A polyamide blend used as a material for exterior body parts is key to light weight cars with strongly reduced fuel consumption. Halogene free flame retardant polyamide increases fire safety and environmental safety in flame sensitive applications.Polybutyleneterephthalate as the technically most important polyester offers new perspectives in blends with amorphous polymers leading to lower distortion and better surface quality in glass fiber reinforced parts. Polybutylenenaphthalate is widening the range of application of polyesters towards higher temperatures. Copolyesters derived from polybutyleneterephthalate are biologically degradable and are therefore promising materials for fermentable foils.Polyoxymethylene copolymers show an outstanding combination of stiffness, dimensional stability, friction and wear as well as resistance against hot water and fuel.As a result of their excellent properties and the existing potential for further improvements polyamide, polyester and polyoxymethylene will continue to grow above average in the future.
    Additional Material: 18 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052440104
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    Sind polyurethanwerkstoffe ein reifes gebiet? (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 244 (1997), S. 121-133 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The world-wide production of polyurethanes has exceeded 6 mio. metric tons in 1994. Compared with the produced amounts of large-scale thermoplastics such as PE, PVC, PP and PS, polyurethanes keep the 5th place.Polyurethanes (PUR) are segmented polymers, which can be synthesized from preformed building blocks in a modular unit construction system. The chemical modules and the various possibilities of combination will be discussed here.Tailor-made polyurethane materials can be divided into two main-fields of application: foams and compact PUR.The main constituents of polyurethane materials are diisocyanates and polyols. These key- chemicals are well characterised with respect to their technological, economical and ecological properties. Taking into account the availability, the masses of production and the experiences that have been collected with the PUR main constituents, these PUR precursors seem to be very mature already.In contrast to this, the PUR-materials made from these building blocks still offer numerous novel problem-solutions, resulting from the variability of the diisocyanate-poly-addition reaction: PUR materials are most commonly segmented into several phases. The formation of hard- and softsegments can be easily demonstrated by looking at thermoplastic polyurethanes (TPU). A deeper understanding of this phase separation and the molecular organisation within these materials promises to realize prospectic polymeric architectures with new and improved properties. PUR materials will still be able to offer new answers to future requirements in balancing economical and ecological needs. By looking at the life-cycles of soft and hard-foams, polyurethane-coatings and thermoplastic PUR-elastomers, this contribution will adress the question: “Is PUR-chemsitry still a challenging field?”
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    Fire-retardant action of potassium nitrate in polyamide 6 (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 245 (1997), S. 23-35 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Zugabe von 10-20 Gew.-% Kaliumnitrat (KN03) zu Polyamid 6 (PA 6) vermindert die Brennbarkeit des Polymeren. Das thermische Verhalten der KN03/PA 6-Mischung wurde mittels Thermogravimetrie, Differentialkalorimetrie und Analyse der fluchtigen Anteile untersucht. Feste Zersetzungsprodukte der Mischung wurden mittels Infrarotspektroskopie, Rontgendiffraktometrie und Elektronenresonanzspek-'troskopie analysiert. Es wurde gefunden, daß KNO3 dem Flielßen und Tropfen der Schmelze vorbeugt und die Karbonisierung auf der Oberflache des Polymeren fordert. Das verringert die Brandgefahr und verbessert die Feuerbestandigkeit. Andererseits geht KNO3 mit PA 6 in der kondensierten Phase eine exotherme Reaktion ein und setzt Sauerstoff frei, der wiederum die Brennbarkeit von PA 6 begiinstigt. Der Mechanismus der chemischen Wechselwirkung van KNO3 mit PA 6 wird diskutiert.
    Notes: The addition of 10-20 wt.-% of potassium nitrate (KNO3) to polyamide 6 (PA 6) improves the fire retardance of the polymer. The thermal decomposition behaviour of the PA 6/KN03-mixture was studied using thermogravimetry, differential scanning calorimetry and thermal volatilisation analysis. Solid products of the thermal decomposition of the mixture were analysed by infrared spectroscopy, X-ray diffraction and electron paramagnetic resonance. It was found that KNO, prevents flowing and dripping of the melt and promotes charring on the surface of the polymer which decreases its fire hazard and improves its fire retardance. On the other hand, KNO3 exothermally reacts with PA 6 in the condensed phase and supplies oxygen to the gas phase which increases the combustibility of PA 6. The mechanism of the chemical interaction of KN03 with PA 6 is discussed.
    Additional Material: 8 Ill.
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    Effect of tricalcium phosphate, hydroxyethyl methacrylate, and ethylene glycol dimethacrylate on the mechanical properties of acrylic bone cement (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 245 (1997), S. 49-62 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Der Einfluß einer Beimischung von Tricalciumphosphat (TCP), Hydroxyethylmethacrylat (HEMA) und Ethylenglycoldimethacrylat (EGDMA) auf die Eigenschaften eines chirurgischen Knochenzements wurde untersucht. Die in Zugversuchen entstandenen Bruchflächen wurden mittels Rasterelektronenmikroskopie charakterisiert. Der Einfluß der Additive auf den Temperaturanstieg während der Polymerisation wurde geprüft. Zug-, Biege- und Druckfestigkeit des ausgehärteten Zements nahmen mit zunehmendem TCP-Gehalt ab, der Elastizitätsmodul stieg dagegen an. Die Zugfestigkeit nahm mit steigendem HEMA-Gehalt geringfügig zu und blieb oberhalb 15 Gew.-% HEMA konstant. Zug-, Biege- und Druckfestigkeit zeigten bei einem EGDMA-Gehalt von 2 Gew.-% (in HEMA) ein Maximum. HEMA und EGDMA beschleunigten die Polymerisation, wogegen TCP retardierend wirkte.
    Notes: The effects of the addition of tricalcium phosphate (TCP), hydroxyethyl methacrylate (HEMA), and ethylene glycol dimethacrylate (EGDMA) on the properties of standard surgical Simplex-P radiopaque bone cement have been investigated. The fracture surface after tensile test was studied by scanning electron microscopy. The influence of these components on the temperature rise during polymerization was investigated. It was found that the tensile strength, the bending strength, and the compressive strength decreased with increasing TCP content, whereas the inverse was observed for the Young's modulus. The tensile strength slightly increased with increasing HEMA content and then it levelled off when the HEMA content was higher than 15 wt.-%. It seemed that there were maximum tensile, bending and compressive strengths when 2 wt.-% EGDMA (in HEMA) was added. Polymerization occurred more rapidly when HEMA and EGDMA were added, whereas the inverse result was found with TCP.
    Additional Material: 7 Ill.
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    The relative physical and thermal properties of polyurethane elastomers. Effect of chain extenders derived from dihydroxynaphthalene (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 245 (1997), S. 89-104 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Polyurethanelastomere wurden in Gegenwart von zwei Dihydroxynaphthalin(DHN)-Verbindungen und deren bromierter Derivate als Kettenverlängerer hergestellt. Als Polyole wurden Polycaprolactondiol und Polytetramethylenglykol und als Diisocyanat-Komponenten Diphenylmethandiisocyanat (MDI) und Dicyclohexylmethan-4,4′-diisocyanat (HMDI) eingesetzt. Der Einfluß der Struktur der Kettenverlängerer auf die physikalischen und thermischen Eigenschaften der Polyurethane wurde untersucht. Wegen der besseren Phasenmischungswirkung der 1,5-DHN-Segmente haben die damit hergestellten Polyurethane höhere Glasübergangstemperaturen und bessere dynamische Eigenschaften als die Polyurethane auf 2,7-DHN-Basis. Der Einbau von bromierten DHN-Einheiten erschwert die Entflammbarkeit. Durch das große freie Volumen der Bromatome wird jedoch die Rotation der DHN-Einheiten eingeschränkt, was zu Polyurethanen mit verringerten Phasenmischungs- und Kristallisationsgraden führt. Die bromhaltigen Polyurethane zeigen zudem eine Verschlechterung der mechanischen und physikalischen Eigenschaften und eine erhöhte Löslichkeit.
    Notes: Polyurethane elastomers were synthesized based on polyols such as poly(caprolactonediol) and poly(tetramethylene glycol), diisocyanates such as diphenylmethane-4,4′-diisocyanate (MDI) and dicyclohexylmethane-4,4′-diisocyanate (HMDI), and two dihydroxynaphthalenes (DHNs) and their brominated derivatives used as chain extenders. The effects of the chemical structures of the chain extenders on the physical and thermal properties of the polyurethanes were investigated. Because of the higher degree of phase mixing of the 1,5-DHN unit, the 1,5-DHN-based polyurethanes have higher Tg values and higher dynamic properties than 2,7-DHN-based polyurethanes. Introduction of bromine atoms increased the flame retardance. However, the large free volume of bromine atoms restricted the rotation of DHNs, thus, directly decreasing the degree of phase-mixing and crystallinity of the polyurethanes. Introducing bromine atoms also decreased the mechanical and dynamic properties and increased the solubility of the polyurethanes.
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    Synthesis and characterization of polypyrrolepolyurethane cationomer composites (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 245 (1997), S. 139-147 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Aus Poly(oxytetramethylen), 4,4′-Bibenzyldiisocyanat, N-Methyldiethanolamin als Kettenverlängerer und Acrylsäure/Polyacrylsäure als Quaternisierungsagens wurden Poly(etherurethan)-Kationomere hergestellt. In aus diesen Kationomeren hergestellten Filmen wurde Pyrrol (15 Gew.-%) in Gegenwart von CuCl2 polymerisiert. Die Filme wurden mittels dynamisch-mechanischer Analyse, Thermogravimetrie und Differentialthermoanalyse charakterisiert. Die elektrische Leitfähigkeit beträgt für den Film ohne Polypyrrol 7.5 · 10-12 Ω-1 cm-1 und mit Polypyrrol 4.5 · 10-6 Ω-1 cm-1.
    Notes: Poly(ether urethane) cationomers based on poly(oxytetramethylene), 4,4′-bibenzyldiisocyanate, N-methyldiethanolamine as chain extender, and acrylic acid/poly(acrylic acid) as quaternization agent were synthesized. Pyrrole (15 wt.%%) was polymerized in films of the ionomer containing CuCl2. The films were characterized by dynamic mechanical analysis, thermogravimetry and differential scanning calorimetry. The electric conductivity of the film without polypyrrole is 7.5 · 10-12 Ω-1 cm-1, while incorporation of polypyrrole increases the conductivity to 4.5 · 10-6 Ω-1 cm-1.
    Additional Material: 2 Ill.
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    Synthesis, characterization and polymerization of waxy monomers (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 245 (1997), S. 155-164 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Wachsartige Monomere und Vernetzer wurden aus kommerziellen Wachsen durch Veresterung mit 2-Hydroxyethylmethacrylat, Glycerindimethacrylat oder Glycidylmethacrylat oder durch Funktionalisierung mit 2-Isocyanatoethylmethacrylat synthetisiert. Die erhaltenen opaken Methacrylate mit Schmelzpunkten zwischen 45 und 80°C wurden in Substanz bzw. Toluollösung in Gegenwart von Radikalinitiatoren polymerisiert. Die Polymeren zeichnen sich durch eine breite Molmassenverteilung aus. Im Gegensatz zur Substanzpolymerisation ist der Doppelbindungsumsatz nach der Lösungspolymerisation nahezu vollständig. Aufgrund der hohen Molmasse der Monomeren ist der beobachtete Polymerisationsschrumpf sehr gering. Polymerisate mit Vernetzermonomeren zeigen eine verbesserte mechanische Stabilität.
    Notes: Waxy monomers and crosslinkers, respectively, were synthesized from commercially available waxes by esterification with 2-hydroxyethyl methacrylate, glycerol dimethacrylate, or glycidyl methacrylate or by functionalization with 2-isocyanatoethyl methacrylate. The resulting opaque methacrylates with melting points between 45 and 80°C were polymerized in bulk and in toluene solution in presence of free radical initiators. The obtained polymers were characterized by a broad molecular weight distribution. Opposite to the bulk polymerization, the double bond conversion in solution polymerization is nearly quantitative. The observed volume shrinkage during polymerization is very low due to the high molecular weight of the monomers. Polymerizates containing crosslinking comonomers exhibit improved mechanical stability.
    Additional Material: 5 Tab.
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    Zur Kinetik der stabilisierten Fällungs-polymerisation eines Kationischen Monomeren in wäßrigen Natriumchlorid-Lösungen (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 245 (1997), S. 165-181 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: The stabilized free-radical precipitation polymerization of the cationic monomer N-(2-methacryloyloxyethyl)-N,N-dimethylbenzylammonium chloride (MADAMBQ) in aqueous solutions of sodium chloride was studied by reaction calorimetry. Poly(ethylene oxide) was used as stabilizer. The rate of polymerization reaches its maximum immediately after initiation and remains nearly constant up to 50 % conversion followed by a decrease that could be described by a first order kinetics. The particles formed are approximately 1 to 30 μm in diameter and are stable over a period of several months.A model based on the theory of homogeneous particle nucleation is suggested to describe the kinetic course of polymerization, taking into account the rate of polymerization in both phases. With the assumption that the concentration of monomer in the phases is determined by a Nernst distribution law, the kinetics of the early stage of polymerization can be modelled reasonably well.The solution polymerization and the unstabilized precipitation polymerization of MADAMBQ was also studied.
    Notes: Die Kinetik der stabilisierten Fällungspolymerisation des kationischen Monomeren N-(2-Methacryloyloxyethyl)-N,N-dimethylbenzylammoniumchlorid (MADAMBQ) in wäßrigen Natriumchlorid-Lösungen wurde mittels Reaktionskalorimetrie untersucht. Polyethylenoxid höherer Molmasse wurde als Stabilisator eingesetzt. Die Reaktionsgeschwindigkeit ist über einen größeren Umsatzbereich nahezu konstant und fällt anschließend mit dem Umsatz annähernd linear ab. Die Teilchengrößenverteilung der gebildeten Dispersion ist bimodal mit Teilchen von etwa 1 bis 30 μm Durchmesser.Zur Beschreibung des Geschwindigkeitsverlaufs der Fällungspolymerisation wird ein Modell vorgeschlagen, das die Polymerisation in der Wasser- sowie in der Polymerphase berücksichtigt. Die Teilchenbildung soll durch homogene Nukleierung erfolgen. Es wird angenommen, daß die Konzentration des Monomeren in den Phasen durch ein Nernstsches Verteilungsgleichgewicht bestimmt wird. Zu Vergleichszwecken wurde auch die Polymerisation von MADAMBQ in Lösung und als nicht stabilisierte Fällungspolymerisation durchgeführt.
    Additional Material: 8 Ill.
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    An investigation of the grafting of cellulose powder with acrylamide under a magnetic field (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 246 (1997), S. 1-9 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Cellulosepulver, hergestellt durch Nitrierung von Eichen-Furfural-Lignocellulose, wurde mit Acrylamid radikalisch gepfropft. Die Pfropfreaktion wurde sowohl in Gegenwart eines äußeren Magnetfeldes (0,15-0,35 T) als auch ohne Magnetfeld durchgeführt. Der Einfluß von Monomerkonzentration, Initiatorkonzentration, Polymerisationszeit und temperatur sowie der magnetischen Feldstärke auf den Polymerisationsverlauf wurde untersucht. Es wurde festgestellt, daß der Pfropfumsatz mit zunehmender Feldstärke signifikant ansteigt.
    Notes: Cellulose powder obtained from oak furfural lignocellulose by nitration reaction was grafted with acrylamide using a radical initiation. The grafting reactions were carried out and compared both in presence and in absence of a continuous external magnetic field with the intensity extended between 0.15-0.35 T. The effect of monomer and initiator concentration, time and temperature of reaction and magnetic field intensity onto the grafting process were examined. It was observed that the presence of a magnetic field leads to a significant increase of the graft conversion.
    Additional Material: 4 Ill.
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    Radical polymerization of poly(butyl acrylate) in the presence of poly(L-lactic acid), 1. Synthesis, characterization and properties of blends (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 246 (1997), S. 49-63 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Poly(L-milchsäure) ist ein biokompatibler, semikristalliner, thermoplastischer Polyester mit ungünstigen mechanischen Eigenschaften. Daher wurde in einem “reactive blending”-Prozeß ein Acrylkautschuk, n-Butylacrylat, mittels einer Suspensionspolymerisation in Wasser auf in einem organischen Lösungsmittel gelöste Poly(L-milchsäure) gepfropft. Die gebildeten Copolymeren konnten isoliert und durch NMR-Spektroskopie und DSC-Messungen charakterisiert werden. Die Untersuchung der mechanischen Eigenschaften ergab keine befriedigenden Ergebnisse, weil die Kautschukphase wahrscheinlich aus viskosen linearen Makromolekülen besteht und daher keine elastischen Eigenschaften besitzt. In weiteren Arbeiten soll der Syntheseweg so modifiziert werden, daß durch den Einbau von Diacrylaten eine zumindest partielle Vernetzung der Kautschukphase erreicht wird.
    Notes: Poly(L-lactic acid) is a biocompatible polyester, semicrystalline, thermoplastic, with low versatility in mechanical properties. To overcome this problem, a reactive blending procedure was performed by grafting an acrylic rubber, n-butyl acrylate, via water suspension polymerization onto poly(L-lactic acid) dissolved in an organic solvent. It was possible to isolate the copolymeric phase formed from the two polymers and characterize it by using NMR and DSC techniques. Mechanical tests on blends gave no satisfactory response, probably because the rubbery phase is composed essentially of viscous linear macromolecules, not able to perform elastic properties. Work is in progress to modify the synthetic pathway to incorporate diacrylates in order to realize a rubbery phase at least partially cross-linked.
    Additional Material: 7 Ill.
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    Tin-coupled styrene-butadiene rubbers (SBRs). Relationship between coupling type and propertiesBased on a paper presented at the 148th Meeting of the Rubber Division, American Chemical Society, Cleveland, Ohio, 17-20 October 1995. (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 246 (1997), S. 85-96 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Zur Entwicklung von neuen Styrol-Butadien-Kautschuken (SBRs) für Reifenanwendungen sind mehrere Arten von Zinn-Polymer-Bindungen (Styryl-, Butadienyl-, Isoprenyl- and α-Methylstyryl-Zinn) sowohl in linearen als auch in verzweigten Ketten untersucht worden. Die dynamisch-mechanischen Eigenschaften von Vulkanisaten mit Ruß wurden analysiert, um eine Beziehung zwischen den Strukturparametern der Polymeren und den Materialeigenschaften herzustellen. Der Polymer-Füll-stoff-Wechselwirkungsparameter, der durch das Verhältnis von mechanischen und dynamischen Termen definiert ist, wurde zur Charakterisierung der Verbindungen herangezogen. Der Einbau von verschiedenen Zinn-Polymer-Bindungen in lineare und in verzweigte SBR-Ketten bewirkte eine Verbesserung der Hystereseeigenschaf-ten der Vulkanisate und eine Veranderung des Wechselwirkungsparameters.
    Notes: Following the development of new SBRs for tyre applications, several kinds of tin-polymer bonds (styryl-, butadienyl-, isoprenyl- and α-methylstyryltin) have been studied, in both branched and linear chains.Dynamic-mechanical properties of the carbon black vulcanizates have been analyzed to establish a relationship between structural parameters of polymers and compound properties. The filler-polymer interaction parameter, defined by a ratio of mechanical and dynamic terms, has been used for the evaluation of the compounds. The introduction of different types of tin-polymer bonds, in branched and linear chains of the SBRs, implies an improvement in the hysteresis properties of the vulcanizates as well as a modification of the interaction parameter.
    Additional Material: 1 Ill.
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    A novel spin-finishing method for antistatic modification of polyester fiber. Surface reaction onto amine-containing copoly(amide-ethers) blended with polyester fiber (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 246 (1997), S. 109-123 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Copoly (amid-ether) rnit zwei unteschiedlichen Aminfunktionalitäten wurden als antistatische Modifikatoren für Polyethylenterephthalatfasern (PET) eingesetzt. Die tertiären Aminogruppen schmelzegesponnener Copolymerfilamente wurden rnit drei Alkylierungsmitteln umgesetzt, wobei ein Sulfobetain, ein Carbobetain bzw. Ammoniumionen gebildet wurden. Dadurch wurde der scheinbare spezifische Widerstand der Filamente auf größfienordnungsmäßfiig 106 bis 108 Ω/cm verringert. Da sich die quaternisierten Copolymeren beim Blend-Spinnen rnit PET zersetzen, wurden Blendfasern von PET mit einem Copolymeren nach dem Schmelzespinnen einer Quaternisierung oder Vernetzung rnit Alkylierungsmitteln bzw. Epoxyvernetzern unterzogen, was die antistatischen Eigenschaften der Fasern im Vergleich rnit der unbehandelten Faser verbesserte. Insbesondere die mit Epoxiden vernetzten Fasern wiesen antistatische Eigenschaften auf, wie sie mit dieser Modifizierungsmethode bislang nicht erreicht wurden. Die antistatischen Eigenschaften blieben nach dem Fkben erhalten, da sowohl die hydrophilen als auch die ionischen Gruppen auf der Faseroberflache immobilisiert waren. Da Quaternisierung bzw. Vernetzung in einem Arbeitsgang rnit dem Verspinnen und Verstrecken der Fasern innerhalb einer kurzen Reaktionszeit erfolgen, sollte diese “spin-finishing„ genannte Methode konventio- nellen Verfahren bezuglich Kosten und Produktivitat uberlegen sein.
    Notes: Copoly(amide-ethers) containing two types of tertiary amine units were made as antistatic modifiers for poly(ethylene terephthalate) (PET) fibers. The filaments of the copolymers were melt-spun and reacted with three alkylating agents in order to quaternize the tertiary amine into a sulfo-betaine, a carbobetaine, and an ammonium ion. The apparent electric resistivity of the filaments was greatly reduced by this reaction, being in the range of 106 to 108 Ω/cm. However, because these quaternized copolymers incurred decomposition during blend spinning with PET, a blend PET fiber containing one type of copoly(amide-ether) was melt-spun and subjected to quaternization of the amino groups as well as to surface crosslinking with various alkylating and epoxy agents. The quaternized blend fibers obtained showed improved antistatic properties compared with the original blend fiber. Particularly, the fibers crosslinked with epoxy compounds were found to have the best antistatic properties that had ever been attained with this type of modification. The antistatic properties were retained even after dyeing, because both hydrophilic and ionic groups had been effectively immobilized on the surface. Since this quaternization and crosslinking could be conducted on-line with spinning and drawing within a short reaction time, this modification technique is called “spin-finishing method”, which should be superior to the conventional methods in terms of cost performance and productivity.
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    Etching of a low-density polyethylene film by fuming nitric acid (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 249 (1997), S. 33-46 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Filme aus Polyethylen niedriger Dichte (LDPE) wurden mit rauchender Salpetersäure behandelt. Die Oberflächeneigenschaften sowie die Bildung polarer Gruppen wie auf der geätzten Filmoberfläche wurden mit SEM-, IR- und XPS-Methoden analysiert. Die mechanische Festigkeit eines aus dem geätzten LDPE-Film und einem Epoxidharz hergestellten Laminats sowie die Bedruckbarkeit der geätzten Oberflächen wurden untersucht und mit einer unbehandelten Probe verglichen. Die Oberflächenrauhigkeit und die Gegenwart polarer Gruppen erhöhen die mechanische Festigkeit des Laminats aus dem geätzten Film durch mechanische Verankerung und chemischer Wechselwirkungen. Die Oberfläche des behandelten LDPE-Films ist besser bedruckbar als die des unbehandelten Films.
    Notes: Low-density polyethylene (LDPE) films were treated with fuming nitric acid (FNA). The surface characteristics and also the insertion of polar groups like on the etched LDPE film surface were measured by SEM, IR and XPS analyses, respectively. The mechanical performance of a laminate of the etched film with epoxy resin and also the printability of the etched film surface were tested and compared with the unetched sample. The surface roughening and the presence of polar groups enhance the mechanical strength of the laminate of FNA-treated film due to mechanical interlocking and chemical interaction. The printability of the treated film surface is also superior to that of the untreated LDPE film surface.
    Additional Material: 10 Ill.
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    Polymerization of lactams, 87Part 86 cf.21.. Block copolymers of poly(∊-caprolactam) and polybutadiene prepared by anionic polymerization. Part I: Preparation and properties (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 237 (1996), S. 123-141 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Es wurde der Einfluß der Polymerisationsbedingungen auf die Eigenschaften von Poly(∊-Caprolactam)-Polybutadien-Blockcopolymeren untersucht, die durch Reaktionsformgießen bei der anionischen ∊-Caprolactam-Polymerisation, initiiert durch das ∊-Caprolactam-Kaliumsalz, in Anwesenheit von α,ω-Dihydroxypolybutadien und Isocyanaten oder deren blockierter Derivate als Funktionalisierungsmittel hergestellt wurden.Es wurde der Einfluß des Polybutadiengehalts, dessen Molekulargewichts, des Isocyanat-Typs und der Polymerisationstemperatur auf die mechanischen Grundeigenschaften und auf die Polymerisationsgeschwindigkeit bestimmt.
    Notes: The effect of the polymerization conditions on the properties of poly(∊-caprolactam)-polybutadiene block copolymers prepared by polymerization casting through anionic polymerization of ∊-caprolactam initiated with potassium salt of ∊-caprolactam in the presence of α,ω-dihydroxy-polybutadiene and isocyanates or their blocked derivatives as functionalizing agents was investigated.The influence of the content of telechelic polybutadiene, its molecular weight, type of diisocyanate, and polymerization temperature on the fundamental mechanical properties of the prepared materials and on the polymerization rate was evaluated.
    Additional Material: 10 Ill.
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    Celluloseether als Trennschichten hydrophiler Polymermembranen (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 249 (1997), S. 11-32 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: This paper reports on polymer membranes characterized by a surface layer of hydroxyalkyl derivatives of cellulose. Water compatible polymers like hydroxyalkyl derivatives of cellulose are preferably those exhibiting good chemical stability and desired membrane characteristics. Normally, water-compatible polymers used in the coating solutions must be rendered water-insoluble after coating. By adapting crosslinking conditions on separation problems, the membranes are useful for many processes in the fields of biotechnology, food and chemical industry.The membranes presented here possess the advantage of being highly resistant to chemical and biological degradation and, hence, have long lifetimes under many process conditions.
    Notes: Es wird die Entwicklung hydrophiler Polymermembranen diskutiert, die nach Beschichtung mit Celluloseethern und anschließender Vernetzung auf den asymmetrischen Trägermembranen interessante Permeations- und Trenneigenschaften bei hervorragenden chemischen Stabilitäten, vor allem beim Membrantrennverfahren der Nanofiltration, aufzeigen. Weiterhin werden Aussagen zu den Gastrenneigenschaften der Celluloseetherkompositmembranen getroffen.Erläutert werden die Permeations- und Trenndaten der Kompositmembranen in Korrelation zur Vernetzung der Celluloseether anhand verschiedener Einflußgrößen, was qualitative und gegebenenfalls quantitative Aussagen zum Vernetzungsmechanismus der Celluloseetherderivate erlaubt. Dabei stehen die Vernetzungstemperatur, der Einfluß der katalysierenden Wasserstoffionen und bedingt die Vernetzungszeit im Vordergrund. Abgerundet werden die Arbeiten durch Ermittlungen rheologischer Daten, die in Zusammenhang zu den Vernetzungsreaktionen und damit zu membranspezifischen Größen stehen.Infolge der hervorragenden chemischen Stabilität der Celluloseether werden Einsatzmöglichkeiten der Kompositmembranen zur Nanofiltration niedermolekularer Verbindungen aus organisch hochbelasteten Systemen beschrieben.
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    Synthesis of tetrahydrofuran-styrene and tetrahydrofuran-methyl methacrylate block copolymers via poly(tetrahydrofuran) with azo groups (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 238 (1996), S. 55-62 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Tetrahydrofuran (THF) wurde mit dem Initiatorsystem 4,4′-Azobis(4-cyanopentanoylchlorid)/SnCI4 kationisch polymerisiert. Das gebildete Poly(THF) mit je einer Azogruppe in der Hauptkette wurde als Initiator für die Polymerisation von Styrol (S) und Methylmethacrylat (MMA) bei 70°C eingesetzt. Die dabei entstandenen PTHF-PS-PTHF- bzw. PTHF-PMMA-Blockcopolymeren wurden mittels Fällungsfraktionierung, spektroskopischen Methoden und Viskositätsmessungen charakterisiert.
    Notes: The cationic polymerization of tetrahydrofuran (THF) initiated by 4,4′-azobis(4-cyanopentanoyl chloride) (ACPC) and SnCI4 is described. Poly(THF) samples possessing azo gorups in the main chain thus obtained were used as initiator in the polymerization of styrene (S) and methyl methacrylate (MMA) at 70°C to yield PTHF-PS-PTHF and PTHF-PMMA block copolymers. Characterization of the block copolymers was carried out by fractional precipitation, spectroscopic methods and viscosity measurements.
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    The effects of a slushing oil on the curing and degradation behavior of an oil-accommodating epoxy adhesive (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 238 (1996), S. 129-141 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Wirkung von aliphatischem Korrosionsschutzöl auf das Aushärte- und Abbauverhalten eines ölkompatiblen Epoxidharzklebers wurde mittels Differentialkalorimetrie (DSC), Fourier-Transformations-Infrarot-Spektroskopie (FTIR) und Thermogravimetrie (TGA) untersucht. Die Ergebnisse der DSC- und FTIR-Messungen deuten darauf hin, daß die Härtungsgeschwindigkeit des untersuchten Epoxid-Systems durch das Vorhandensein des Öls nur wenig beeinflußt wird. Dennoch bestätigt das Absinken der exothermen Härtungskurve, begleitet von einer Verbreiterung des Glasübergangstemperaturbereichs, daß das Öl den Aushärtemechanismus beeinflussen kann und in der Lage ist, die Struktur des gehärteten Harzes zu verändern. Außerdem geht aus den TGA-Messungen hervor, daß die Temperaturbeständigkeit des Harzes sich in Gegenwart des Öls verschlechtert; dies wird auf Veränderungen in der Struktur und im Abbaumechanismus des Epoxid-Systems zurückgeführt.
    Notes: The effect of aliphatic slushing oil on the curing and degradation behavior of an oil-accommodating epoxy adhesive is studied by using differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), and thermogravimetric analysis (TGA). The results of FTIR and DSC indicate that the curing rate of the tested epoxy system is little affected in the presence of the oil. However, the decrease of the curing exotherm accompanied with a broadening of the glass transition confirms that the oil can affect the curing mechanisms and may change the structure of the cured resin. Additionally, it is evident from the TGA results that the thermal resistance of the resin deteriorates in the presence of the oil, which is attributed to the changes in the structure and the degradation mechanism of the epoxy system.
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    Electrochemical polymerization of some monomers with schiff's base structure. A voltammetric study (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 1-12 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die elektrochemische Polymerisation von Pyrrol-2-aldehyd-azin, 2,2′-[1,4-Phenylenbis(nitrilomethylidyn)]dipyrrol und 2,2′-[1,4-Biphenylylenbis(nitrilomethylidyn)]dipyrrol läuft als anodische Fällungspolymerisation ab. Monomere und Polymere wurden voltammetrisch unter Verwendung von Platin- und “Paste-carbon”-Elektroden untersucht. Die Ergebnisse stimmen mit MO-Berechnungen überein, wobei die Reaktivität der Monomeren nach Hückel abgeschätzt wurde.
    Notes: The electrochemical polymerization of some Schiff's base-type monomers like pyrrole-2-aldehyde azine, N,N′-di(2-pyrrolylmethylene)-1,4-diaminobenzeneSystematic name: 2,2′-[1,4-phenylenebis(nitrilomethylidyne)]dipyrrole., and N,N′-di(2-pyrrolylmethylene)-4,4′-diaminobiphenylSystematic name: 2,2′-[4,4′-biphenylylenebis(nitrilomethylidyne)]dipyrrole. proceeds as a precipitating polymerization to the anodic compartment. The voltammetric study of monomers and polymers using Pt electrodes and paste-carbon electrodes were carried out. The results are in agreement with the MO calculations using the Hückel approximation for evaluating of the reactivity of the monomers.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052390101
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    Stereoselective polymerization of butadiene by a new dicationic nickel complex (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 33-41 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Der neuartige dikationische Komplex [dppfNi(MeCN)4][BF4]2 (dppf = 1,1′-Bis(diphenylphosphin)ferrocen) zeigte in Anwesenheit von Diethylaluminiumchlorid (AIEt2CI) hohe Aktivität für die Polymerisation von 1,3-Butadien. Reaktionsdauer, Temperatur und das Aluminium/Nickel-Verhältnis wurden auf maximale Aktivität und Selektivität optimiert. Umsätze über 90% konnten erreicht werden. Im Vergleich zu Polybutadienen, die mit anderen Nickel-Phosphin-Systemen hergestellt wurden, zeigten die synthetisierten Polybutadiene höhere cis-1,4-Anteile (〈80%) und eine geringe Bildung von 1,2-Einheiten (2%). Alle Polymeren hatten niedrige mittlere Molekulargewichte (Mw 〉 11 800).
    Notes: The new dicationic nickel complex [dppfNi(MeCN)4][BF4]2 (dppf = 1,1′-bis(diphenylphosphino)ferrocene) in the presence of diethylaluminium chloride (AIEt2CI) exhibited high activity on the 1,3-butadiene polymerization. Reaction time, temperature and aluminium/nickel molar ratio were optimized in order to achieve maximum activity and selectivity. Conversions higher than 90% were obtained in contrast to other nickel-based systems using phosphine ligands, the resulting polybutadiene showed high cis-1,4 (〈80%) content and only small amount of 1,2-units (2%). All polymers presented low molecular weights (Mw 〉 11 800).
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052390104
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    Structural changes in poly(methyl methacrylate) during deep-etch X-ray synchrotron radiation lithography. Part II: Radiation effects on PMMAPart I cf.1. Dedicated to Prof. Dr. Werner Borchard on the occasion of his 60th birthday (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 79-91 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Bei der Bestrahlung von Polymethylmethacrylat (PMMA) mit Röntgensynchrotronstrahlung ändert sich die chemische Struktur des Polymeren. Die Ergebnisse der analytischen Untersuchungen dieser Arbeit weisen darauf hin, daß neben einem Abbau der Polymerketten auch einzelne Esterseitengruppen abgespalten werden. Durch die Bestrahlung entstehende Langkettenverzweigungen wurden bei PMMA nicht gefunden. Dadurch unterscheiden sich die physikalischen und chemischen Eigenschaften des bestrahlten Polymeren von denen des unbestrahlten.
    Notes: The irradiation of poly(methyl methacrylate) changes the chemical constitution of the polymer. In addition to a decrease in molar mass further radiation-induced radical reactions cause changes in the chemical constitution of the polymer. Analysis of the reaction products shows that formation of long-chain branching can be excluded. Along with degradation of the chain lengths, ester groups in the side chains are attacked. The result is a modified polymer with a physical and chemical behaviour different from that of the starting polymer.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052390108
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    Synthesis of flexible polyarylates by interfacial polycondensation. Part II: Incorporation of 4,4′-thiodiphenol (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 133-149 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Zähigkeit von Polyarylaten wurde durch den Einbau von 4,4′-Thiodiphenol und Bisphenol A, die in der wäßrigen Phase einer Grenzflächenpolykondensation vorgelegt wurden, erhöht. Die modifizierten Polyarylate besitzen leicht erniedrigte Zugfestigkeiten und Zugmoduli, aber aufgrund der Flexibilität der eingebauten Segmente stark erhöhte Izod-Schlagzähigkeiten. Darüber hinaus bleiben die guten thermischen Eigenschaften der Polyarylate nach der Modifizierung erhalten, so daß die hergestellten Materialien auch für Anwendungen mit sehr hohen Anforderungen an die thermische Belastbarkeit geeignet sind.
    Notes: The toughness of polyarylates was improved by incorporation of 4,4′-thiodiphenol and bisphenol A, being introduced in the aqueous phase of an interfacial polycondensation reaction. The modified polyarylates possessed slightly lower tensile strength and modulus but much higher Izod impact strength due to the flexibility of the incorporated segments. In addition, the superb thermal properties typical for polyarylates were reserved in the modified polyarylate, thus assuring its broad applicability for those applications where extremely stringent criteria of thermal characteristics are required.
    Additional Material: 16 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052390112
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    Le rôle des systèmes photoamorceurs dans l'efficacité de photoréticulation de l'homopolymère dicyclopentadiène acrylateNom systématique: Tricyclo[5.2.1.02.6]déc-4-en-8-yl acrylate. (DCPA) et acrylate d'éthyle (AE) et des dérivés copolymères DCPA/AE (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 239 (1996), S. 169-190 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: The photocrosslinking efficiency of a series of commercial photoinitiators and multicomponent photosensitive systems on uncrosslinked acrylic matrices has been estimated. Copolymers used for this study are tricyclo[5.2.1.02,6]dec-4-en-8-yl acrylate/ethyl acrylate copolymers of variable composition (100/0, 40/60, 20/80, 0/100) synthesized in solution by a free-radical process. The irradiations were carried out at large wavelengths (λ ≥ 310 nm). Systems of benzophenone/benzoyl peroxide led to really fast crosslinking kinetics for 10 min of irradiation.
    Notes: L'efficacité de photoréticulation de toute une série de photoamorceurs commerciaux et de systèmes photosensibles multicomposants a été évaluée sur des matrices acryliques non réticulées. Les polymères utilisés pour cette étude sont des homopolymères et des copolymères d'acrylate de dicyclopentadiène/acrylate d'éthyle de composition variable (100/0, 40/60, 20/80, 0/100) synthétisés en solution par voie radicalaire. Les irradiations ont été effectuées à des grandes longueurs d'ondes (λ ≥ 310 nm). Les systèmes benzophénone/peroxyde de benzoyle ont permis d'obtenir des cinétiques de réticulation très rapides pour des temps d'irradation de 10 min.
    Additional Material: 12 Tab.
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    Products of polycondensation of 4,4′-biphenyldithiol with some hydrocarbon dihalides (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 13-21 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Polysulfide wurden mit hoher Ausbeute durch Hochtemperatur-Lösungspolykondensation von 4,4′-Dimercaptobiphenyl mit ausgewählten aliphatischen und aromatisch-aliphatischen Dihalogenkohlenwasserstoffen hergestellt. Um die optimalen Polykondensationsbedingungen zu bestimmen, wurde der Einfluß folgender Faktoren auf die reduzierte Viskosität und die Ausbeute der Polysulfide ermittelt: Art des organischen Lösungsmittels, Art des Halogenwasserstoff-Akzeptors, Konzentration der organischen Reagenzien, Reaktionstemperatur und -zeit. Die Polykondensation des Dithiols mit Bis(4-chlormethylphenyl)methan wurde als Modellsystem eingehender untersucht. Die Polysulfidstrukturen wurden mittels Elementaranalyse, IR-Spektroskopie und Röntgenstrukturanalyse bestätigt. Aus der thermogravimetrischen Analyse wurden die Zersetzungstemperatur, der Gewichtsverlust bei dieser Temperatur und das Maximum der Zersetzungsgeschwindigkeit erhalten. Weiterhin wurden einige physikalisch-chemische, mechanische und dielektrische Eigenschaften ermittelt. Die beste thermische und chemische Bestandigkeit zeigt das aus dem Dithiol und 4,4′-Bis(chlormethyl)biphenyl hergestellte Polysulfid, was auf dessen vorwiegend aromatische Struktur zuriickgefuhrt werden kann.
    Notes: Polysulfides were synthesized with high yield by high-temperature solution polycondensation of 4,4′-biphenyldithiol with selected aliphatic and aromatic-aliphatic hydrocarbon dihalides. To determine the optimum polycondensation conditions, the influence of the following factors on reduced viscosity and yield was studied: type of organic solvent, type of hydrogen halide acceptor, concentration of reagents, reaction temperature, and reaction time. A thorough examination was carried out only for the polycondensation of dithiol with bis(4-chloromethylphenyl)methane chosen as model system. The structures of the polysulfides were confirmed by elemental analysis, X-ray analysis, and infrared spectroscopy. The temperature of initial decomposition, the percentage of mass loss, and the temperature of the fastest decomposition, process were determined from curves of differential thermal and thermogravimetric analysis. Some physicochemical, mechanical and electrical properties were determined. The highest thermal and chemical resistance has been found for the polysulfide obtained from 4,4′-biphenyldithiol and 4,4′-bis(chloromethyl)biphenyl, probably because of the predominantly aromatic structure.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052510102
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    Organic-inorganic hybrid sol-gel materials, 2. Application for dental composites (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 61-72 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Drie organisch-anorganische Hybridmaterialien wurden nach dem Sol-Gel-Verfahren durch kovalenten Einbau von Poly(styrol-co-methylmethacrylat)(Poly(St-co-MMA))-, Polymethylmethacrylat(PMMA)- und Polystyrol(PS)-Struktureinheiten in ein SiO2-Netzwerk hergestellt und als Füllstoffe (bis zu 60 Gew.-%) in Dentalharzen verwendet. Der Einfluß der Füllstoffe auf einige mechanische Eigenschaften der Harze wurde untersucht. Die Härte der gefüllten Dentalharze nahm mit steigendem Füllstoffgehalt zu, wogegen die Biegefestigkeit abnahm. Die Druckfestigkeit der gefüllten Harze war besser als die des ungefüllten Harzes, nahm jedoch mit steigendem Füllstoffgehalt ab.
    Notes: By incorporating poly(methyl methacrylate) (PMMA), polystyrene (PS), and poly(styrene-co-methyl methacrylate) (poly(St-co-MMA)) structure units covalently into the SiO2 glass network via a sol-gel approach, three organic-inorganic hybrid materials (PMMA-SiO2, PS - SiO2, and poly(St-co-MMA) - SiO2) have been prepared. The three hybrid sol-gel materials were used as filler (up to 60 wt.-%) for dental composite resins. The effect of the three filler materials on several mechanical properties of the dental composite resins was investigated. The hardness of the filled dental composites increased with increasing filler content, whereas the bending strength decreased. The compressive strength of the composites was improved, compared with the unfilled resin, but decreased with inreasing filler content.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052510106
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    Adsorption of BTX compounds from aqueous solutions by water-insoluble starch (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 107-116 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Adsorption von Benzol, Toluol und p-Xylol (BTX) aus wäßrigen Lösungen mittels hochvernetzter kationischer Stärke mit tertiären Amingruppen wurde untersucht. Der endotherme Adsorptionsvorgang ist vom Anfangs-pH-Wert und der Anfangskonzentration abhängig und kann mit einer Langmuir-Isotherme beschrieben werden.Die Adsorptionswärme (Δ) bei pH 4 beträgt für Benzol, Toluol und Xylol 29,45 kJ mol-1, 34,41 kJ mol-1 bzw. 35,58 kJ mol-1, bei pH 10 30,17 kJ mol-1, 35.56 kJ mol-1 bzw. 39,39 kJ mol-1. Die adsorbierte Menge nimmt in der Reihenfolge Benzol 〉 Toluol 〉 Xylol ab.
    Notes: The removal of benzene, toluene and p-xylene (BTX) compounds from aqueous solutions with highly crosslinked cationic starch containing tertiary amine groups was investigated. The adsorption process has found to be initial pH- and initial concentration-dependent, endothermic, and follows the Langmuir isothermal adsorption.The heats of adsorption (ΔH) at initial pH = 4 of benzene, toluene and p-xylene compounds are 29.45 kJ mol-1, 34.41 kJ mol-1, and 35.58 kJ mol-1, respectively, those at initial pH = 10 are 30.17 kJ mol-1, 35.56 kJ mol-1, and 39.39 kJ mol-1, respectively. The order of the amount of adsorbed BTX compounds on the adsorbent is benzene 〉 toluene 〉 p-xylene.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052510110
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    Thermogravimetric and ESR studies of polymer/metal precursors for high-temperature superconductors (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 157-170 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Bi-Sr-Ca-Cu-Komplexverbindungen von Polymethacrylsäure (PMAA) und Kresolnovolaken, die als Precursoren für Hochtemperatursupraleiter (HTSL) eingesetzt werden, sowie deren Cu-Komplexsalze wurden ESR-spektroskopisch und thermogravimetrisch untersucht. In den PMAA-Proben wurden drei verschiedene Cu2+-Spezies nachgewiesen: i) Cu2+-Paare, ii) isolierte Cu2+-Ionen und iii) Cu2+-Cluster. Bei niedrigem Cu-Gehalt der Proben bilden die Cu2+-Paar-Bindungen den Hauptanteil, bei hohem Cu-Gehalt überwiegen die Clusterbindungen. In den Novolakproben wurden nur isolierte Cu2+-Ionen und Cu2+-Cluster nachgewiesen. Die Einführung der Cu-Ionen erniedrigt die thermische Stabilität der Polymeren, der thermische Abbau erfolgt stufenweise. In den PMAA-Proben wird die erste Abbaustufe bei ≈ 220°C durch die Cu2+-Paar-Komplexe verursacht.
    Notes: Bi-Sr-Ca-Cu complexes of poly(methacrylic acid) (PMAA) and cresol novolac, which are precursors for high-temperature superconductors (HTSC) and Cu complexes of those polymers were investigated by ESR spectroscopy and thermogravimetry. In the PMAA samples three different kinds of Cu2+ species were detected: i) Cu2+ pairs, ii) isolated Cu2+ ions and iii) Cu2+ clusters. While Cu2+ pairs are the main species at low Cu concentrations, clusters become dominant at high Cu contents. In the novolac samples Cu2+ was only detected in isolated sites and clusters. The introduction of Cu ions lowered the thermal stability of the polymers and led to a stepwise decomposition. In the PMAA samples the first decomposition step at ≈ 220°C is caused by the Cu2+ pair complexes.
    Additional Material: 6 Ill.
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    Polymerization of 1,3-butadiene with neodymium chloride/2-ethylhexanolate/triethylaluminium catalyst systemIPCL communication No. 325. (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 193-205 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Neodymchlorid-2-ethylhexanolate mit der allgemeinen Formel NdCl3 · nL wurden durch eine Liganden-Austauschreaktion zwischen Neodymchloridisopropanolat (I) und 2-Ethylhexanol (EH) hergestellt. Die Hexanolate NdCl3 · 1,5 EH (II) und NdCl3 · 2,5 EH (III) wurden durch Elementaranalyse und Gravimetrie charakterisiert. Die katalytische Aktivität der Hexanolate bei der Homopolymerisation von 1,3-Butadien in Gegenwart von Triethylaluminium wurde untersucht. Die Verbindung III zeigte eine höhere Aktivität als die Verbindung II. Höhere Katalysator- und Cokatalysatorkonzentrationen sowie eine höhere Temperatur steigerten den Umsatz, wogegen die Viskosität der Produkte abnahm. Mit zunehmender Reaktionszeit erhöhten sich sowohl der Umsatz als auch die Viskosität. Die cis-1,4-Konformation wurde durch die Variation von Temperatur und Cokatalysatorkonzentration beeinflußt. Der gesamte Anteil der cis-1,4-Stuktur lag jedoch in allen Fällen über 99%, während die Produkte nur einen sehr geringen Vinyl-Anteil von 〈1% enthielten. Die Zugabe einer elektronenspendenden Verbindung verringerte den cis- 1,4-Gehalt aber auf 87%.
    Notes: Neodymium chloride 2-ethylhexanolates of the general formula NdCl3 · nL were prepared by ligand exchange reaction between neodymium chloride ispropanolate (I) and 2-ethylhexanol (EH). These hexanolates, NdCl3 · 1.5 EH (II) and NdCl3 · 2.5 EH (III), were characterized by elemental analysis and gravimetry. The catalytic activity of these hexanolates in combination with triethyl aluminium in the homopolymerization of 1,3-butadiene was studied, and the activity was found to be higher with III than II. The conversions increased with increasing the catalyst and co-catalyst concentrations and the temperature, whereas the intrinsic viscosity decreased. The conversions and the intrinsic viscosity decreased. The conversions and the intrinsic viscosity increased with reaction time. The cis-1,4 structure was influenced by variation in temperature and co-catalyst concentration, however, the total cis-1,4 structure was always more than 99% with very low vinyl content (〉1%). Addition of an external electron donor decreased the cis-1,4 content to 87%.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052510117
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    Ideal crosslinked-polymers and their characterization in free-radical monovinyl-divinyl copolymerizationsPoster presented at the “International Symposium on Advanced Network-Polymers, Kansai University” (ISANKU), at Kansai University, Suita, Osaka, Japan, on December 5-6, 1995. (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 240 (1996), S. 275-284 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The critical conditions in which the classical Flory-Stockmayer gelation theory (F-S theory) is applicable to monovinyl-divinyl copolymerizations were pursued in detail. The resulting prepolymers or precursors of ideal crosslinked-polymers were characterized as standard polymers for the discussion of network formation in free-radical monovinyl-divinyl copolymerizations. Methyl methacrylate was copolymerized with a small amount of ethylene dimethacrylate, butylene dimethacrylate or nonapropyleneglycol dimethacrylate in the presence of lauryl mercaptan, a chain transfer agent to reduce the occurrence of a thermodynamic excluded volume effect and intramolecular crosslinking as the primary and secondary factors, respectively, for the greatly delayed gelation in the free-radical monovinyl-divinyl copolymerizations and, moreover, to keep the primary chain length constant by inhibiting a gel effect. The ratio of the actual gel point to the theoretical one reached 1.1, supporting the validity of F-S theory. The resulting prepolymers were subjected to SEC-MALLS analysis to determine the molecular weights, the molecular-weight distributions and the radii of gyration; the correlations of molecular weight vs. elution volume and radius of gyration vs. molecular weight were useful for the characterization of the precursors of ideal network-polymers.
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1996.052400126
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    Chemical reactions on polysaccharides, 5Part 4: Chloroacetylated derivatives of dextran, Cellul. Chem. Technol. 26 (1992) 675. Reaction of mesyl chloride with pullulan (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 241 (1996), S. 1-10 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Reaktion von Mesylchlorid mit vernetzten Pullulan-Mikropartikeln wurde untersucht, insbesondere der Einfluß der Reaktionsbedingungen auf das Produktverhältnis Chlordeoxy-/O-Mesylpullulan. In N,N-Dimethylformamid wird vorwiegend Chlordeoxypullulan gebildet, während in Pyridin bei niedrigen Temperaturen der Mesylester das Hauptprodukt ist. In N,N-Dimethylacetamide entstehen Chlordeoxy und Mesylgruppen im Verhältnis 2:1. Durch die Einführung der Chlordeoxy- bzw. Mesylgruppen werden die Mikropartikel hydrophob.
    Notes: The reaction of mesyl chloride with crosslinked pullulan microparticles was investigated, in particular the influence of the reaction conditions on the ratio between the two possible products chlorodeoxy or O-mesyl pullulan. It was found that in N,N-dimethylformamide the preponderent reaction product is chlorodeoxy pullulan, while in pyridine at low temperatures the main product is the mesyl ester of pullulan. In N,N-dimethylacetamide, the substituent groups are both chlorodeoxy and mesyl ones, in about 2:1 ratio. By the introduction of either chlorodeoxy or mesyl groups, the pullulan-crosslinked microparticles become hydrophobic.
    Additional Material: 8 Ill.
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    Structural analysis of poly(4-hydroxybutyl acrylate)-grafted silk fibres (1996)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 241 (1996), S. 41-56 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Poly(4-hydroxybutylacrylat) poly(4-HBA) wurde aus wäßrigem Medium mit Ammoniumpersulfat als Initiator auf Seide (bombyx mori) aufgepfropft. Die Gewichtszunahme stieg proportional mit der Monomerkonzentration im Pfropfsystem. Der Pfropfgrad lag im Bereich von 45 bis 65%. Die Feuchtigkeitsaufnahme nahm bei einer Gewichtszunahme von 〉10% stark ab. Die mechanischen Eigenschaften der Seidenfasern zeigten mit steigender Gewichtszunahme keine wesentliche Änderung. Doppelbrechung und isotroper Brechungsindex nahmen bis zu einer Gewichtszunahme von 35% ab und blieben dann unverändert. Röntgenbeugungsdiagramme zeigten, daß die kristalline Struktur durch die Pfropfbehandlung nicht modifiziert wird. Kalorimetrische (DSC), thermomechanische (TMA) und thermogravimetrische (TG) Analysen ergaben, daß das thermische Verhalten der poly(4-HBA)-gepfropften Seidenfasern nur leicht verändert wird. Die zur Bestimmung des dynamisch-mechanischen Verhaltens der Seidenfasern durchgeführten DMA-Messungen zeigten eine Verschiebung der E′- und E″-Modulspitzen zu niedrigeren Temperaturen mit steigender Gewichtszunahme. Ablagerungen auf der Faseroberfläche der bei einem hohen Monomer/Seide-Verhältnis (〉50%) gepfropften Seide wurden mit Rasterelektronenmikroskopie nachgewiesen.
    Notes: Poly(4-hydroxybutyl acrylate) poly(4-HBA) was graft-copolymerized onto silk fibres (bombyx mori) in aqueous medium with ammonium persulfate as initiator. The weight gain increased with increasing concentration of monomer in the grafting system. The grafting efficiency ranged from 45 to 65%. Equilibrium moisture regain decreased sharply beyond 10% weight gain. The tensile properties of the silk fibres did not change significantly as a function of the increasing weight gain. Birefringence and isotropic refractive index decreased until 35% weight gain and then remained unchanged. The X-ray diffraction patterns showed that the crystalline structure was not affected by grafting. Differential scanning calorimetry (DSC), thermomechanical (TMA), and thermogravimetric (TG) measurements showed that poly(4-HBA)-grafted silk fibres underwent only slight changes in the thermal behaviour. The dynamic mechanical measurements (DMA) exhibited a downward shift of both the storage (E′) and loss modulus peak (E″) with increasing weight gain. Scanning electron microscopy (SEM) observations showed the presence of some deposits adhering to the surface of silk fibres grafted at high monomer/silk ratio (〉50%).
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1996.052410104
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    The effects of desolvation methods of the recrystallized MgCl2-alcohol adduct on catalyst characteristics and the bulk density of polyethylene (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 17-25 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: MgCl2-Träger für einen Ethylenpolymerisationskatalysator wurden mit Hilfe der Rekristallationsmethode hergestellt, wobei Methanol als Lösungsmittel diente. Der Einfluß verschiedener Lösungsmethoden des rekristallisierten MgCl2-Alkohol-Adduktes auf die morphologischen Charakteristika der Katalysatoren wurde untersucht. Die Lösungsmethode beeinflußt die Eigenschaften der Katalysatoren beträchtlich. Die dargestellten Katalysatoren wiesen unterschiedliche Ti/Mg-Verhältnisse auf, sowohl was die Oberfläche als auch die gesamten Katalysator-Partikel betrifft. Betrachtet man die Ti-Verteilung und Aktivitätsprofile, dann erweisen sich nicht nur die Polymerisationsbedingungen, sondern auch die Ti-Verteilung auf dem Katalysator als wichtige Faktoren, welche die Dichte der Polymeren beeinflussen.
    Notes: The MgCl2 supports for an ethylene polymerization catalyst were prepared by the recrystallization method using methanol as a solvent. The effects of different desolvation methods of the recrystallized MgCl2-alcohol adduct on the morphological characteristics of the catalysts were examined. The desolvation method greatly affects the characteristics of the catalyst. The prepared catalysts had different Ti/Mg ratios with respect to both surface content and entire catalyst particles. Considering Ti distribution and activity profiles, not only the polymerization conditions but also the Ti distribution on the catalyst appear to be an important factor which affects the bulk density of the polymers.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052530102
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    Synthesis of aromatic poly(ether ketone)s with ferrocene units in the main chain (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 89-97 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Aromatische Poly(etherketon)e mit Ferrocen-Einheiten in der Hauptkette wurden durch direkte Polykondensation von 1,1′-Ferrocendicarbonsäure mit Diphenylether oder 1,4-Diphenoxybenzol hergestellt. Als Katalysatoren wurden Trifluormethansulfonsäure, Methansulfonsäure/P2O5 (Eatons Reagens) oder Trifluormethansulfonsäure/P2O5 verwendet. Polykondensationen bei Raumtemperatur für 24 h ergaben Poly(arylenetherketon)e mit Grenzviskositäten bis zu 40 mL g-1. Die Monoacylierung von Diphenylether mit Ferrocencarbonsäure wurde im Hinblick auf die Effektivität von Eatons Reagens als Katalysator und Lösungsmittel eingehender untersucht.
    Notes: Aromatic poly(ether ketone)s with ferrocene units in the main chain were prepared by direct polycondensation of 1,1′-ferrocenedicarboxylic acid with diphenyl ether or 1,4-diphenoxybenzene using various catalysts such as trifluoromethanesulfonic acid (triflic acid), a combination of methanesulfonic acid/P2O5 (Eaton's reagent) or a combination of triflic acid/P2O5. Polycondensations at room temperature for 24 h gave poly(arylene ether ketone)s with inherent viscosities up to 40 mL g-1. Monoacylation of diphenyl ether with ferrocenecarboxylic acid was studied in detail in order to show the efficiency of polymer formation employing Eaton's reagent as catalyst and solvent.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052530107
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    Mechanical and structural characteristics of phenolphthalein poly(ether sulfone)/ultra-high molecular weight polyethylene blends (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 73-80 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die mechanischen und strukturellen Eigenschaften von Blends aus Phenolphthalein-Polyethersulfon und ultrahochmolekularem Polyethylen (UHMWPE) wurden anhand von Zug- und Biegeversuchen, Raster- und Transmissionselektronenmikroskopie untersucht. Die Zugabe einer geringen Menge UHMWPE (2 Gew.-%) führt zu einer Verstärkung der PES-C-Matrix. Höhere UHMWPE-Konzentrationen verschlechtern die mechanischen Eigenschaften. Die Strukturuntersuchungen zeigen, daß die Blends im gesamten Zusammensetzungsbereich mehrphasig sind. Bei geringen UHMWPE-Konzentrationen ist die UHMWPE-Phase gleichmäßig verteilt und entlang der Fließrichtung orientiert, was mit der starken Grenzflächenadhäsion zur Verbesserung des mechanischen Verhaltens beiträgt. Mit steigender UHMWPE-Konzentration nimmt die Domänengröß der UHMWPE-Phase zu.
    Notes: Mechanical and structural properties of blends of phenolphthalein poly(ether sulfone) (PES-C) with ultra-high molecular weight polyethylene (UHMWPE) were investigated using tensile and bending testing, scanning electron microscopy and transition electron microscopy. The incorporation of minor amounts of UHMWPE (2 wt.-%) into PES-C has a reinforcement effect. With higher concentrations of UHMWPE, the mechanical properties decrease gradually. Structural studies demonstrated that the blends are multiphasic in the whole composition range. The minor UHMWPE, dispersed uniformly and oriented along the flow direction, as well as the strong interfacial adhesion contribute to the increase of the mechanical performance of the blends. The domain size of the UHMWPE phase was found to increase with the increase of its concentration.
    Additional Material: 6 Ill.
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    Redox copolymer with N-bromosulfonamide groups for the decomposition of cyanide ions in dilute aqueous solutions (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 117-130 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Ein Redoxcopolymeres, ein makroporöses Poly(Styrol-co-Divinylbenzol) (S/DVB)-Harz mit N-Bromsulfonamidgruppen, wurde angewandt, um Cyanide aus wäßrigen Lösungen zu entfernen. Dieses Harz enthält aktives Brom in den funktionellen Gruppen (1.86 mmol g-1, 3.72 meq g-1) und weist Oxidationseigenschaften auf. Es wurde sowohl in statischen als auch in dynamischen Systemen für die Oxidation von Cyanidionen zu nichttoxischen Verbindungen angewandt. Die Reaktionen wurden in wäßrigen Lösungen mit 26-2600 mg L-1 CN- bei unterschiedlichen pH-Werten durchgeführt. Die Ergebnisse zeigten, daß dieses Harz die Cyanide leicht zu Cyanaten oxidiert, die ca. 1000 mal weniger toxisch sind. Bei Kontakt mit dem Harz fiel die Cyanidkonzentration in den Lösungen unter 0.05 mg L-1 CN-. Die —SO2NBrNa-Gruppen gingen dabei in —SO2NH2-Gruppen über. Diese konnten wiederum mit Natriumhypochlorit- und Natriumbromid-Lösungen reaktiviert werden. Es wurde auch eine Alternative zu der Cyanidionenoxidation mit N-Bromsulfonamid-Harz untersucht, indem ein analoges N-Chlorsulfonamid-Harz in Gengenwart von katalytischen Mengen von Bromiden angewandt wurde.
    Notes: A redox copolymer, macroporous poly(styrene-co-divinylbenzene) (S/DVB) resin having N-bromosulfonamide groups, was used for removal of cyanide ions from aqueous solutions. This resin contains active bromine in functional groups (1.86 mmol g-1, i. e. 3.72 meq g-1) and shows oxidative properties. It was employed in static and flow system for oxidation of cyanide ions to non-toxic compounds. The reactions were carried out in aqueous media containing 26-2600 mg L-1 CN- at different pH values. The data showed that the resin having active bromine easily oxidized cyanides, forming cyanates being 1000-times less toxic than cyanides. In contact with the resin the concentration of cyanides in tested solutions dropped below 0.05 mg L-1 CN-. During the oxidation processes the —SO2NBrNa groups transform to —SO2NH2 groups. They can be reactivated by use of sodium hypochlorite and bromide solutions. As an alternative to oxidation of cyanides by N-bromosulfonamide resin, the oxidation of these ions by N-chlorosulfonamide resin with addition of a small amount of bromides was examined.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052510111
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    Mitteilungen/Announcements (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 251 (1997), S. 207-208 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: No Abstract
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/apmc.1997.052510118
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    Hydrolytic and thermal stability of novel polyurethane elastomers (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 33-43 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Novel Polyester glycols with alkyl side groups were used for the improvement of thermal stability and hydrolytic stability of polyester urethane elastomers. The novel polyester glycols used are poly( β -methyl- δ -valerolactone)glycol (PMVL), poly(3-methyl pentamethylene adipate) glycol (PMPA), poly(nonamethylene-co-2-methyl octamcthylene carbonate) gycol (PNCO). A mixture of PNCO and poly(dimethyl siloxane)gycol (PNCO/PDMS) was also used. Polyurethane network elastomers were prepared from 4,4′-diphenylmethane diisocyanate (or 2,4-tolylene diisocyanate), and a mixture of 1,4-butane diol and trimethylol propane by a prepolymer method. Mechanical properties, Tg, thermal stability, and hydrolytic stability were measured. Morphology were also measured by means of polarizing microscopy, dynamic viscoelastometer, and ESR. The properties of novel polyurethane elastomers have good mechanical properties comparable to those of the general purpose polyester urethanes, and better thermal and hydrolytic stability than PTMG-based polyurethane. These polyurethane elastomers were exposed in out door during 2 year in Nagasaki, JAPAN. The novel polyurethane clastomers held alomost constant values for gel fraction, swelling ratio, relative modulus during 12 months, while poly(oxytetramethylene oxide)-based polyurethane as a control decreased the these values. Relationship of degradation behaviors with chemical structure and morphology were discussed.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052520103
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    Oxidizability of lactams and lactam-based polyamidesDedicated to Dr Jan Šebenda on the occasion of his 70th birthday (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 139-151 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: In the chain oxidation of N-alkylamides with molecular oxygen, propagation is the ratedetermining step under conditions when the oxidation rate is independent of oxygen pressure. The oxidizability of lactams and lactam-based polyamides correlates with the energy of the formation of N-alkylamide radical by abstraction of hydrogen from the methylene group adjacent to nitrogen. While for lactams this energy depends on the number of carbons in the lactam ring, for N-alkylamides and polylactams such dependence is not observed.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052520110
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    Use of EPR to image nitroxyl radicals in hals stabilized polymers (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 179-193 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: An X-band EPR-Imaging apparatus which allowed us to determine the distribution of nitroxyl radicals within solid samples of polymeric materials containing hindered amine stabilizers, is described. It is shown that EPR Imaging represents a powerful tool for investigating the growth and decay of nitroxyls formed in polymers irradiated under air for long periods. Since the variations of the radical concentration can be monitored both in time and in the space, this technique provides valuable information not easily attainable by means of other methods.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052520113
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    Photo-oxidation mechanisms of poly(2,6-dimethyl-1,4-phenylene oxide). (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 237-256 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A re-examination of the photo-oxidation mechanism of poly(2,6-dimethyl-1,4-phenylene oxide) (PPO) at both long and short irradiation wavelengths under accelerated conditions is reported. The formation rate of poly-2,6-dimethylphenoxy (PDMP) radicals, have been observed by esr spectroscopy, while benzylic-type radicals have been detected by spin trapping experiments using nitrosodurene under UV irradiation conditions. The changes of FTIR spectra obtained under accelerated photo-oxidative conditions show the formation of primary oxidation products such as aromatic aldehydes and quinones. The direct formation of radical cations and superoxide anions by a photo-induced electron-transfer reaction is suggested under our conditions. In addition, some results on the of photo-oxidation PPO/PS blends as a function of polystyrene tacticity are also reported. In the case of syndiotactic polystyrene the blend photostability shows some differences in comparison with the blend containing atactic polystyrene. This effect has been ascribed to the absence of excimers in syndiotactic polystyrene which are not revealed by fluorescence measurements. Finally, the chemical modification of PPO with bromine gave a bromomethylated PPO with different amounts of CH2 Br groups, which has been used for further substitution reactions with alkoxy sodium salts of 4-hydroxy-2,2,6,6-tetramethyl-1-piperidinyloxy (TEMPO) and 4-hydroxy-1,2,2,6,6-pentamethylpiperidine (PMPP). The accelerated photo-oxidation of a modified copolymer PPO-PMPP containing a 60% PMPP moieties as side groups and its blends with pure PPO has been followed by FTIR and esr spectroscopies. Some comparisons with a commercially available hindered amine light stabilizers (HALS) and a modified copolymer PPO-PMPP are also reported under the same photo-oxidative conditions.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/apmc.1997.052520116
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    Zähigkeit und Relaxationsverhalten von Polymethylmethacrylat, Polystyrol und Polycarbonat (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 27-49 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: For innovative applications of plastics, which take advantage of special properties of polymeric materials, comprehensive understanding on strengthening and toughening mechanisms is required. The temperature-dependent mechanical behaviour of PMMA, PS and PC under dynamic loading conditions were investigated by means of an instrumented Charpy impact tester. The elastic-plastic fracture mechanics parameters, the energy-determined J-integral, and the deformation-determined crack opening displacement, δ, enable to do structure-related quantification of micromechanical processes. The J-integral values showed a maximum, resulting from an energy-dissipative process. The maximum values for PMMA occurred at 50°C and for PC at 40°C , which is related to the secondary(β) relaxation as evaluated from the frequency dependence of the mechanical loss factor. The 0-relaxation initiated shear deformation mechanisms, which led to a local increase of toughness. In polycarbonate, toughness is strongly increased due to a stress-induced shear flow process at temperatures higher than -25°C. Correlations between morphology and toughness can be derived with the help of optical investigations of stable crack propagation on fracture surfaces.
    Notes: Innovative Kunststoffanwendungen, die die speziellen Eigenschaften polymerer Werkstoffe gezielt ausnutzen, erfordern vertiefte Kenntnisse über festigkeits- und zähigkeitsbestimmende Mechanismen. Das sich in Abhängigkeit von der Temperatur ändernde Werkstoffverhalten von PMMA, PS und PC wurde bei dynamischer Beanspruchung mittels instrumentierter Kerbschlagbiegeprüfung bestimmt. Mit der verformungsbestimmten Rißöffnungsverschiebung δ und dem energiebestimmten J-Integral stehen Kenngrößen der Fließbruchmechanik zur Verfügung, die eine strukturbezogene Quantifizierung der temperaturabhängigen mikromechanischen Prozesse erlauben. Die J-Integralwerte zeigen für PMMA bei 50°C und für PC bei -60°C ein durch einen energiedissipativen Prozeß verursachtes Maximum. Dieses Maximum steht, wie sich aus der Interpretation der Frequenzabhängigkeit des mechanischen Verlustfaktors ergibt, mit der Neben(β)-Relaxation in Beziehung. Dabei initiiert die β-Relaxation Scherdeformationsmechanismen, die ihrerseits die lokale Zähigkeitserhöhung bewirken. Ab -25°C führt für PC ein spannungsinduzierter Scherfließprozeß zu einer erheblichen Zähigkeitssteigerung. Durch die Einbeziehung lichtmikroskopischer Untersuchungen des stabilen Rißfortschritts auf der Bruchfläche können Morphologie-Zähigkeits-Korrelationen abgeleitet werden.
    Additional Material: 16 Ill.
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    Thermostable block copolymers, 2Part 1 cf. 16.. Preparation and characterization of soluble blockcopolyimides (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 71-88 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Eine Reihe von Polyamidimid-Polyimid-Blockcopolymeren (PAI-PI-BCPs) wurde durch Polykondensation von PAI-Blöcken mit Amino-Endgruppen und PI-Blöcken mit Anhydrid-Endgruppen hergestellt. Zur Synthese der Blöcke mit Molekulargewichten im Bereich von ca. 2000 bis 15000 wurden nur technisch leicht zugängliche Monomere, wie Trimellitsäureanhydridchlorid, Benzophenontetracarbonsäuredianhydrid, 4,4′-Diaminodiphenylmethan, 2,4-Toluylendiamin und 4,4′-Diaminodiphenylsulfon eingesetzt. Dabei zeigte sich, daß durch den blockartigen Aufbau die Löslichkeit-und damit die Verarbeitbarkeit-im Vergleich zu den reinen, unlöslichen Polyimiden wesentlich verbessert werden konnte, bei nahezu gleichbleibender Thermostabilität. So wurden BCPs mit guten mechanischen Eigenschaften, Thermostabilitäten bis ca. 480°C (Thermogravimetrie, 5% Gewichtsverlust) und guten Löslichkeiten in Dimethylacetamid und anderen polaren aprotischen Lösungsmitteln erhalten.
    Notes: New poly(amide-imide)-poly(imide) block copolymers (PAI-PI-BCPs) were prepared by polycondensation of amino-terminated PAI-blocks with anhydride-terminated PI-blocks. For the syntheses of the blocks with molecular weights from 2000 to 15000 only commercially available monomers were used, e.g. trimellitic acid anhydride chloride, benzophenone tetracarboxylic acid dianhydride, 4,4′-diaminodiphenylmethane, 2,4-toluenediamine and 4,4′-diaminodiphenylsulfone. The BCPs were shown to have better solubility compared to the pure, insoluble PIs with only minor decrease of the thermostability. Thus, BCPs with good mechanical properties, thermostabilities up to 480°C (thermogravimetric analysis, 5% weight loss) and good solubility in dimethylacetamide and other polar aprotic solvents were obtained.
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    Block and graft copolymers with polysiloxane and poly(N-acyliminoethylene) sequences (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 139-149 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Eine Reihe von Polysiloxan/Poly(N-acetyliminoethylen)-(PSiO/PNAI)-Block- und -Pfropfcopolymeren wurde durch Polymerisation von 2-Methyl-2-oxazolin (MeOZO) mit funktionellen Polysiloxan-Prepolymeren als Initiatoren synthetisiert. Die Copolymeren wurden mit IR- und 1H NMR-Spektroskopie sowie Elementaranalyse, Differentialkalorimetrie und Thermogravimetrie charakterisiert. Der Einbau sowohl von hydrophoben als auch von hydrophilen Sequenzen verleiht den Polymeren amphiphile Eigenschaften. Ihre Eigenschaften in Lösung und als Feststoffe lassen die Produkte für Anwendungen als nichtionische Emulgatoren, Oberflächenmodifikatoren, Gele, usw. geeignet erscheinen.
    Notes: A series of polysiloxane/poly(N-acetyliminoethylene) (PSiO/PNAI) block and graft copolymers were synthesized by the initiation of 2-methyl-2-oxazoline (Me-OZO) polymerization with functional polysiloxane prepolymers. The copolymerization products were characterized by IR- and 1H NMR spectroscopy, elemental analysis, DSC and thermogravimetry. The insertion of both hydrophobic and hydrophilic sequences in the macromolecular structure induces a behavior characteristic of amphiphilic compounds. Their solution and solid state behavior evidenced peculiarities which make them able to act as nonionic emulsifiers, surface modifiers, gels, etc.
    Additional Material: 4 Ill.
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    The state of water in styrene-grafted and sulfonated poly(vinylidene fluoride) membranes (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 151-167 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Der Zustand von Wasser in Protonenaustausch-Membranen, hergestellt durch Pfropfen von Styrol auf Polyvinylidenfluorid-Filme (PVDF-g-PS) mittels Elektronenstrahlen und anschließendes Sulfonieren (PVDF-g-PSSA), wurde mittels Differentialkalorimetrie (DSC), Raman-Spektroskopie und Rontgen-Diffraktion (SAXS) ermittelt. Die Raman-Untersuchungen zeigten, daß einzelne Wassermolekule durch hydrophobe Wechselwirkungen an die Polymerketten gebunden sind. Die DSC-Untersuchungen zeigten, daß Wasser in den Membranen in drei verschiedenen Umgebungen vorliegt: nicht gefrierendes ionisch gebundenes Wasser, gefrierendes freies Wasser und gefrierendes gebundenes Wasser. Die Menge an nicht gefrierendem Wasser betragt unabhangig vom Pfropfungsgrad etwa 10 H2O/SO3H (mol/mol). Die Menge an gefrierendem Wasser ist stark vom Pfropfungsgrad abhangig. Oberhalb eines Pfropfungsgrades von 50% werden Werte von 40 H20/S03H (mol/mol) erreicht. Die Leitfahigkeit von nur nicht gefrierendes Wasser enthaltenden Membranen ist gering, d. h., das ionisch gebundene Wasser kann nicht allein die fur den Transport von Protonen und Wasser notwendigen Kanale bilden. Die SAXS Untersuchungen zeigten, daß Wasser/Sulfonsaure-Cluster in Membranen aus hydratisiertem PVDF-g-PSSA mit einem Bragg-Abstand von 25 Å gebildet werden. Diese Cluster formen die Kanale fur den Ionentransport und die Leitfähigkeit.
    Notes: The state of water in proton exchange membranes prepared by pre-irradiation (electron beam, 100 kGy) grafting of styrene onto poly(vinylidene fluoride) films (PVDF-g-PS), followed by sulfonation (PVDF-g-PSSA), has been studied with thermal analysis, Raman spectroscopy and small angle X-ray diffraction (SAXS). Raman spectra show that, in addition to free liquid water in the membranes, single water molecules are weakly bound to the polymer backbone. Thermal analysis shows that there are three types of water molecules in the membrane; non-freezable water associated with the ionic sites, freezable free water, and freezable bound water. The amount of non-freezable water is around 10 H2O/SO3H (mol/mol), and is independent of the degree of grafting (d.o.g.). The amount of freezable water is strongly dependent on the d.o.g. as long as the grafting has not penetrated the whole of the film, and reaches a value of around 40 H2O/SO3H (mol/mol) above a d.o.g. of 50%. The conductivity of membranes containing only the non-freezable water is low, i. e. the ionically bound water alone does not form the domains necessary for proton and water transport. SAXS measurements show that water/sulfonic acid clusters in hydrated PVDF-g-PSSA membranes with a Bragg distance of 25 Å are formed; these form the ion conducting channels in the membrane.
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    MITTEILUNGEN/ANNOUNCEMENTS (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 211-211 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
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    URL: http://dx.doi.org/10.1002/apmc.1997.052530117
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    Tensile and flexural behavior of polypropene sheets with different crystallinities of surface layer (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 253 (1997), S. 201-210 
    Details
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Zug- und Biegemoduli von preßgeformten Polypropen-Probekörpern mit unterschiedlichen Oberflächenkristallinitäten wurden basierend auf der Annahme eines Schicht-Verbund-Modells untersucht. Es zeigte sich, daß die Spannungs-Dehnungs-Kurven der Zugversuche und die Werte der Biegeablenkung im wesentlichen von der Oberfächenkristallinität abhängen, jedoch erwiesen sich die Bruchspannungen als von der Oberflächenkristallinität unabhängig. Es wird angenommen, daß das beobachtete Zug- und Biegeverhalten der Proben auf der Grundlage eines Schicht-Verbund-Modells, bei dem eine massive, starre Platte zwischen zwei weichen Schichten eingebettet ist, charakterisiert werden kann.
    Notes: The tensile and flexural moduli of the compression-molded sheets of polypropene with different surface layer crystallinity were investigated based on a layered composite model. It was found that the tensile stress-strain curve and flexural deflection depended largely on the surface layer crystallinity, but the ultimate strain-at-break values were independent of the surface layer crystallinity. It is suggested that the tensile and flexural behavior can be characterized using a layered composite model in which a bulk plate was sandwiched between two surface layers.
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    The role of charge transfer complexes in the photodegradation of polyolefins (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 45-54 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Addition of HALS-stabilisers, the cut-off wavelength of the light source, the temperature and the oxygen pressure have an influence on the UV-degradation mechanism of polyolefins. All these parameters influences the conversion of oxygen into polymeric carbonyls. The results are explained assuming that the initiation of the UV-degradation of pololefins is due to substrate-oxygen charge transfer complexes (CTCs).
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    Fracture behavior of exposed HDPE specimens with an embrittled layer due to UV-exposure (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 69-88 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The applicability of fracture mechanics was studied on UV-exposed HDPE Charpy specimens. The failure distribution of the stress at failure measured in three-points bending tests showed a bifurcation in failure processes. At high stresses yielding occurs, resulting in large strain at failures. At lower stresses crack propagation causes low strain at failures. Due to the bifurcation in failure processes the ductile-brittle transition temperature of exposed specimens is hard to determine.Specimens notched after exposure showed a decrease in the critical stress intensity values. The effective notch depth of exposed specimens was found to be larger than the thickness of the oxidized layer measured by FT-IR and density measurements.
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    Deactivation processes of 2-hydroxyphenyl-1,3,5-triazines  -  polymeric and monomeric UV absorbers of the benzotriazole and triazine class (1997)
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 252 (1997), S. 119-138 
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    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: In the 2-hydroxyphenyl-1,3,5-triazines, the intramolecular hydrogen bond is stronger than in the corresponding 2-hydroxyphenylbenzotriazoles. Compounds with only one aryl group in the 2-hydroxyphenyl-1,3,5-triazine series show proton-transferred fluorescence with large Stokes shift and high quantum yield. No such fluorescence is observed, in contrast, for compunds with three aryi groups bearing no electrondonating groups on the aryl moieties. When the hydrogen atom of the intramolecular hydrogen bond is replaced by CH3, the respective derivative shows fluorescence with a normal Stokes shift.Various copolymers of MA-TIN 1 (2-[2-hydroxy-3-tert.-butyl-5-(O-[2-hydroxy-3-(2-methylpropenoyloxy)propyl]-2-carbonyloxyethyl)phenyl]benzotriazole), and MA-TZ 1 (2,4-Bis(2,4-dimethyl-phenyl)-6-[2-hydroxy-4-(2-hydroxy-3-[2-methylpropenoyloxy])propoxyphenyl]-1,3,5-triazine) with styrene, methyl methacrylate, and methacrylic acid have been synthesized by radical polymerization. The absorption spectra in the longwavelength UV region appear unchanged compared to those of the monomeric UV absorbers indicating that the stabilizer chromophores are conserved intact in the polymer. Both the monomeric and the polymeric stabilizers exhibit a strongly Stokesshifted, temperature-dependent, low-quantum-yield, proton-transferred fluorescence. This may be taken as evidence that the intramolecular hydrogen bond, which is essential for the photostability of this type of UV absorber, remains intact also in the copolymers. Activation energies of the radiationless deactivation process can be evaluated from the temperature dependence of this fluorescence. These energies lie between 4 and 5 kJ/mol for most of the benzotriazole and triazine stabilizers investigated.Fluorescence-decay measurements with crystalline MA-TIN 1 at different temperatures reveal a close correspondence of the temperature dependence between decay times and relative quantum yields. The radiationless process is thence concluded to originate from the proton-transferred level S1'. The decay time at room temperature is estimated at 70 ps, close to the value for crystalline TIN P (2-(2-hydroxy-5-methylphenyl)benzotriazole). The proton-transferred fluorescence of MA-TIN 1 exhibits a biexponential decay profile whereas solid TIN P, in contrast, displays only one single lifetime.
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    The stability of transmembrane helices: A molecular dynamics study on the isolated helices of bacteriorhodopsin (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 401-422 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bacteriorhodopsin (bR) continues to be a proven testing ground for the study of integral membrane proteins (IMPs). It is important to study the stability of the individual helices of bR, as they are postulated to exist as independently stable transmembrane helices (TMHs) and also for their utility as templates for modeling other IMPs with the postulated seven-helix bundle topology. Toward this purpose, the seven helices of bR have been studied by molecular dynamics simulation in this study. The suitability of using the backbone-dependent rotamer library of side-chain conformations arrived at from the data base of globular protein structures in the case TMHs has been tested by another set of 7 helix simulations with the side-chain orientations taken from this library. The influence of the residue's net charge on the helix stability was examined by simulating the helices III, IV, and VI (from both of the above sets of helices) with zero net charge on the side chains. The results of these 20 simulations demonstrate in general the stability of the isolated helices of bR in conformity with the two-stage hypothesis of IMP folding. However, the helices I, II, V, and VII are more stable than the other three helices. The helical nature of certain regions of III, IV, and VI are influenced by factors such as the net charge and orientation of several residues. It is seen that the residues Arg, Lys, Asp, and Glu (charged residues), and Ser, Thr, Gly, and Pro, play a crucial role in the stability of the helices of bR. The backbone-dependent rotamer library for the side chains is found to be suitable for the study of TMHs in IMP. © 1996 John Wiley & Sons, Inc.
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    Solid state and solution conformations of a helical peptide with a central gly-gly segment (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 515-526 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of amino acids with contrasting conformational tendencies on the stereochemistry of oligopeptides has been investigated using an octapeptide Boc-Leu-Aib-Val-Gly-Gly-Leu-Aib-Val-OMe, which contains two helix-promoting Aib residues and a central helix-destabilizing Gly-Gly segment. Single crystal x-ray diffraction studies reveal that a 3 10-helix is formed up to the penultimate Aib residue, at which point there is a helix reversal in the backbone, reminiscent of a C-terminal 6 → I hydrogen bond. The curious feature in the crystal is the solvation of the possible 6 → 1 bond by a CH3OH molecule, where the OH is inserted between O(3) and N(8) and participates in hydrogen bonds with both. The cell parameters are as follows: space group P212121, a = 10.649(4) Å, b = 15.694(5) Å, c = 30.181(8) Å, R = 6.7% for 3427 data (| F0| 〉 3σF) observed to 0.9 Å. Nuclear magnetic resonance studies in CDCl3 using NH group solvent accessibility and nuclear Overhauser effects as probes are consistent with a 3 10-helical conformation. In contrast, in (CD3)2SO, unfolding of the central segment results in a multiple β-turn structure, with β-turn conformations populated at residues 1-2, 3-4, and 6-7. CD studies in methanol-2,2,2-trifluoroethanol (TFE) mixtures also provide evidence for a solvent-dependent structural transition. Helical conformations are populated in TFE, while type II β-turn structures are favored in methanol. © 1996 John Wiley & Sons, Inc.
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    Single helical structure of curdlan triacetate (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 557-566 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The molecular and crystal structure of curdlan triacetate, acetylated (1 → 3)β-D-glucan, was analyzed by means of an x-ray diffraction technique with the help of the linked-atom least-squares method. Unit cell dimensions are a = b = 11.00(1), c(fiber axis) = 22.91 (9) Å, and γ = 120°. The space group is P61. The unit cell contains six chemical repeating units related by 6/I-helical symmetry, which is essentially the same as the backbone conformation of one of the modifications (form I) of curdlan. During the refinement calculation, the terminal methyl in every acetyl moiety was elastically restrained to the trans conformation commonly observed in related oligosaccharide structures. The difference Fourier map, the observed and calculated densities, and the thermogravimetric measurement indicated one water molecule per glucose residue. The water oxygen is linked to two carbonyl oxygens in adjacent molecules by hydrogen bonds. The conformation of the primary acetyl moiety is a (skew, -gauche, trans). So far, no skew conformation was observed for the primary acetyl and hydroxyl moieties except in α, β-panose. In both cases, the unusual eclipsed orientation of the primary group is attributed to the hydrogen bond and this conformation is quite different from that of pachyman triacetate. © 1996 John Wiley & Sons, Inc.
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    Quantum mechanical calculations and experimental measurement of N-terminal charge effects on 1HN and 1HCα chemical shifts in peptides (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 573-581 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Nuclear magnetic resonance spectroscopists are increasingly utilizing chemical shifts to characterize the secondary structure of proteins. The present study addresses the effects that the positively charged amino group at the N-terminus of a peptide has on 1HN and 1HCα chemical shifts along the chain. This information is necessary for interpreting chemical shift data for proteins and/or for peptides that are used as models for protein structure. The chemical shifts for the 1H resonances of four peptides that differ only in the location of their N-terminii are assigned using two-dimensional nmr spectroscopy. The peptides have sequences derived from the β subunit of the glycoprotein hormone human chorionic gonadotropin (hCG-β). Comparison of the 1HN and the 1HCα chemical shifts for residues common to all four peptides reveals downfield shifts for 1HN and the 1HCα resonances within three residues of the N-terminus compared with chemical shifts in the interior of the peptide. The magnitude of the downfield shift is larger for resonances nearer the N-terminus. Quantum mechanical calculations of the 1HN and 1HCα chemical shifts in peptides constructed with six alanine units also predict a significant terminus effect. The calculations agree both qualitatively and quantitatively with the experimental data. The inductive nature of the end effect is confirmed in the calculations by Mulliken population analysis. End effects should be taken into account in determining protein secondary structures from chemical shifts. © 1996 John Wiley & Sons, Inc.
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    A fluorescence and CD study on the interaction of synthetic lipophilic hepatitis B virus preS(120-145) peptide analogues with phospholipid vesicles (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 607-618 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The interaction of the immunogenic peptide of human hepatitis B virus (HBV) preS(120-145), including B and T epitopes, with phospholipid vesicles has been studied by fluorescence techniques and CD. In addition, interaction of three lipopeptides derived from preS(120-145) containing stearoyl, cholanoyl, and tripalmitoyl-S-glyceryl-cysteine (Pam3C) SS moieties with dipalmitoylphosphatidylcholine (DPPC) has been investigated by polarization fluorescence spectroscopy. Fluorescence experiments showed an increase in fluorescence intensity and a blue shift of the maximum emission wavelength upon interaction of preS(120-145) with DPPC vesicles below the transition temperature (Tc), indicating that the tryptophan moiety enters a more hydrophobic environment. Moreover, fluorescence polarization experiments showed that the peptide decreased the membrane fluidity at the hydrophobic core, increasing the Tc of the lipid and decreasing the amplitude of the change of fluorescence polarization associated with the cooperative melting of 1,6-diphenyl-1,3,5-hexatriene labeled vesicles. The absence of leakage of vesicle-entrapped carboxyfluorescein indicates that the peptide did not promote vesicle lysis. Besides, the three lipopeptides derived from preS(120-145) showed a more pronounced rigidifying effect at the hydrophobic core of the bilayer, with a significative increase in the Tc. Stearoyl- and cholanoyl-preS(120-145) restricted the motion of lipids also at the polar surface, whereas Pam3CSS-preS(120-145) did not alter the polar head group order. Finally, CD studies in 2,2,2-triflouroethanol or in presence of vesicles suggested that the bound peptide adopted amphiphilic α-helical and β-sheet structures, with an important contribution of the β-turn. It is concluded that preS(120-145) can interact with the lipid membrane through the formation of an amphipathic structure combination of β-sheet and α-helix aligned parallel to the membrane surface, involving the N-terminal residues, and penetrating only a short distance into the hydrophobic core. The C-terminal part, with a combination of β-turn and β-sheet structure, remains at the outer part of the bilayer, being potentially accessible to immunocompetent cells. Furthermore, coupling of an hydrophobic moiety to the N-terminal part of the peptide favors anchoring to the membrane, probably facilitating interaction of the peptide with the immunoglobulin receptor. These results are in agreement with the induction of immune response by preS(120-145) and with the enhanced immunogenicity found in general for lipid-conjugated immunopeptides. © 1996 John Wiley & Sons, Inc.
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    Masthead (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996) 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/bip.360380501
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    Isomerization of the Xaa-Pro peptide bond induced by ionic interactions of arginine (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 673-682 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Inclusion of Arg or Pro residues in proteins and peptides has been proved to play an essential role in biochemical functions through ionic interactions, conformational transitions, and formation of turns as well. In this study we present the conformational properties of the Ac-Arg-Ala-Pro (1), Ac-Arg-Ala-Pro-NH2 (2), Ac-Arg-Pro-Asp-NH2 (3), and Ac-Arg-Pro-Asp (4) tripeptides, using 1H-nmr spectroscopy and molecular dynamics. These peptides were modeled with the aim of studying the role of the Arg-guanidinium to carboxylate ionic interactions on the Xaa-Pro peptide bond isomerization. It was found with 1 and 4 that arginine preferentially interacts with the C-terminal carboxylate group, even though the β-carboxylate is also accessible. This tendency of the Arg moiety was found to induce the cis disposition of the Ala-Pro peptide bond in 1. It was also confirmed that the Arg…Asp side chain-side chain ionic interaction in 3 plays a key role in backbone folding and structural stabilization through a type I β-turn. The nmr pattern for 3 showed a remarkable similarity with that for various Arg-Tyr-Asp containing peptides, a sequence that is crucial for the adhesion properties of the Leishmania gp63 glycoprotein. © 1996 John Wiley & Sons, Inc.
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    A search for the ideal type I β-turn (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 723-732 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In 1968 C. Venkatachalam (Biopolymers, Vol. 6, pp. 1425-1436) predicted the ideal forms of β-turns (type I, type II, etc.) based entirely on theoretical calculations. Subsequently, over a thousand x-ray structures of different globular proteins have been analyzed, with results suggesting that the most important form among the hairpin conformers is the type I β-turn. For the latter type of hairpin conformation, the original computations had predicted φi+1 = -60°, ψi+1 = -30°, φi+2 = -90°, and ψi+2 = 0° as backbone torsion angle values, and these have been used from that time as reference values for the identification of the type I β-turn. However, it has never been clarified whether these “ideal” backbone torsion angle values exist in real structures, or whether these torsion angles are only “theoretical values.” Using the most recent release of the Protein Data Bank (1994), a survey has been made to assign amino acid pairs that approach the ideal form of the type I β-turn. The analysis resulted in four sequences where the deviation from ideal values for any main-chain torsion angles was less than 2°. In order to determine whether such a backbone fold is possible only in proteins owing to fortuitous cooperation of different folding effects, or whether it occurs even in short peptides, various attempts have been made to design the optimal amino acid sequence. Such a peptide model compound adopting precisely the predicted torsion angle values [φi+1 = -60°, ψi+1 = -30°, φi+2 = -90°, and ψi+2 = 0°] could provide valuable information. The solid state conformation of cyclo[(δ) Ava-Gly-Pro-Thr (O1Bu)-Gly] reported herein, incorporating the -Pro-Thr- subunit, yields values suggesting that the “ideal” type I β-turn is even possible for a peptide where there are no major environmental effects present. © 1996 John Wiley & Sons, Inc.
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    Characterization of the bioactive form of linear peptide antagonists at the δ-opioid receptor (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996), S. 759-768 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The stereochemical requirements for δ-opioid receptor binding of a series of linear peptide antagonists with a novel conformationally restricted Phe analogue (Tic) as a second residue were examined by using a variety of computational chemistry methods. The δ-opioid receptor analogues with significant affinity, Tyr-Tic-NH2 (TI-NH2), Tyr-Tic-Phe-OH (TIP), Tyr-Tic-Phe-NH2(TIP-NH2), Tyr-Tic-Phe-Phe-OH (TIPP), Tyr-Tic-Phe-Phe-NH2) (TIPP-NH2), and the low affinity δ-opioid peptides Tyr-Pro-Phe-Pro-NH2 (morphiceptin) and Tyr-Phe-Phe-Phe-NH2 (TPPP-NH2), were included in this study. The conformational profiles of these peptides were obtained by consecutive cycles of high and low temperature molecular dynamic simulations, coupled to molecular mechanical energy minimization carried out until no new conformational minima were obtained. Comparing the results for TPPP-NH2 and TIPP-NH2, the presence of the conformationally restricted Tic residue did not greatly reduce the number of unique low energy conformations, but did allow low energy conformers involving cis bonds between the first two residues. The conformational libraries of these peptides were examined for their ability to satisfy the three key ligand components for receptor recognition already identified by previous studies of high affinity cyclic (Tyr1-D-Pen2-Gly3-Phe4-D -Pen5) enkephalin (DPDPE) type agonists: a protonated amine group, an aromatic ring, and a lipophilic moiety in a specific geometric arrangement. Two types of conformations common to the five high δ-opioid affinity L-Tic analogues were found that satisfied these requirements, one with a cis and the other with a trans peptide bond between the Tyr1 and Tic2 residues. Moreover, both the Tic2 and Phe3 residues could mimic the hydrophobic interactions with the receptor of the Phe4 moiety in the cyclic DPDPE type agonists, consistent with the appreciable affinity of both di-and tripeptides. The low δ-opioid receptor affinity of morphiceptin can be understood as the result of conformational preferences that prevent the fulfillment of this pharmacophore for recognition. © 1996 John Wiley & Sons, Inc.
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    Masthead (1996)
    New York : Wiley-Blackwell
    Biopolymers 38 (1996) 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/bip.360380601
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    Nonmonotonic temperature dependence of the flexibility of bacteriophage fd (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 13-22 
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    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: We present two experiments that probe the temperature dependence of the flexibility of the filamentous virus fd by examining aspects of the liquid crystalline nature of fd suspensions. The first measurement is of the temperature variation of the coexisting fd concentrations at the isotropic-cholesteric phase transition. The second measurement is of the magnetic field induced birefringence or Cotton-Mouton constant in the isotropic phase as a function of temperature. We compare these measurements with the theoretical treatment of Onsager, Khokhlov-Semenov, and Chen and conclude that the flexibility of fd varies nonmonotonically with temperature and has a minimum in persistence length at 35°C. © 1996 John Wiley & Sons, Inc.
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    Hydrophobic solvation in aqueous trifluoroethanol solution (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 43-50 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The titration of an aqueous solution of a de novo designed peptide with trifluoroethanol (TFE) shows complete helix formation with the addition of only 30% TFE. A molecular simulation of the peptide, in which a single shell of TFE molecules initially surrounds the peptide, reveals preferred sites of solvent interaction. The TFE molecules show greater preference for the hydrophobic compared with hydrophilic side chains. The helix-enhancing ability of TFE in aqueous solution may be rationalized in terms of stabilizing the hydrophobic collapse of apolar side chains of the formed helix. © 1996 John Wiley & Sons, Inc.
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    Mobility-resolved 13C-NMR spectroscopy of primary plant cell walls (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 51-66 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Primary plant cell walls contain highly hydrated biopolymer networks, whose major chemistry is known but whose relationship to architectural and mechanical properties is poorly understood. Nuclear magnetic resonance spectroscopy has been used to characterize segmental mobilities via relaxation and anisotropy effects in order to add a dynamic element to emerging models for cell wall architecture.For hydrated onion cell wall material, single pulse excitation revealed galactan (pectin side chains), provided that dipolar decoupling was used, and some of the pectin backbone in the additional presence of magic angle spinning. Cross-polarization excitation revealed the remaining pectin backbones, which exhibited greater mobility (contact time dependence, dipolar dephasing) than the cellulose component, whose noncrystalline and crystalline fractions showed no mobility discrimination. 1HT2 behavior could be quantitatively interpreted in terms of high resolution observabilities. Mobility-resolved spectroscopy of cell walls from tomato fruit, pea stem, and tobacco leaf showed similar general effects.Nuclear magnetic resonance study of the sequential chemical extraction of onion cell wall material suggests that galactans fill many of the network pores, that extractability of pectins is not dependent on segmental mobility, and that some pectic backbone (and not side chain) is strongly associated with cellulose.Analysis of the state of cellulose in four hydrated cell walls suggests a noncrystalline content of 60-80% and comparable amounts of Iα and Iβ polymorphs in the crystalline fraction. Comparison with micrographs for onion cell walls shows that noncrystalline cellulose does not equate to chains on fibril surfaces, and chemical shifts show that fully solvated cellulose is not a significant component in cell walls. © 1996 John Wiley & Sons, Inc.
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    Optimization methods for conformational sampling using a Boltzmann-weighted mean field approach (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 103-114 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An optimization protocol is proposed that combines a mean field simulation approach with Boltzmann-weighted sampling. This is done by including Boltzmann probabilities of multiple conformations in the optimization procedure. The method is demonstrated on a simple model system and on the side-chain conformations of phenylalanines in a small hexapeptide. For comparison, calculations were performed using classical stochastic dynamics simulations [M. Saunders, K. N. Houk, Y. Wu, C. Still, M. Lipton, G. Chang, and W. C. Guida (1990), Journal of the American Chemical Society, Vol. 12, pp. 1419], iterative optimization of probabilities on a fixed set of basis conformations [P. Koehl and M. Delaure (1994), Journal of Molecular Biology, Vol. 239, pp. 249-275], and simulations with locally enhanced sampling [A. Roitberg and R. Elber (1991), Journal of Chemical Physics, Vol. 95, pp. 9277-9287]. Although approximations are used in our method, the results may be more physically meaningful than those of the other procedures discussed. Furthermore, the approximate Boltzmann distribution allows generalization of the results. © 1996 John Wiley & Sons, Inc.
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    Treating sequence dependence of protein stability in a mean-field model (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 115-127 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several statistical mechanical theories of protein stability have recently been developed, based on mean-field approximations, random energy models, or related assumptions. None of these models treats how protein stability depends on the monomer sequence: they only treat sequences as being random. Here, as a first approximation to sequence effects, we develop theory for how the compact conformations of copolymer chains of two monomer types A and B depend on 4 composition quantities: the numbers of AA, AB, BA, and BB segments. We apply this to improving the “reconfiguration term” of a mean-field treatment of protein stability [K. A. Dill (1985), Biochemistry, Vol. 24, pp. 1501-1509]. Reconfiguration refers to the change of a compact chain from a random conformation to one with an optimal hydrophobic core. By comparison with exhaustive enumeration studies, we find that the theory gives improved estimates for reconfiguration properties in compact copolymers. One interesting result is that for a chain of a given length and hydrophobic (H)/polar (P) composition, some hydrophobic clustering in the sequence (PHHHHP .) is more stabilizing than if hydrophobic and polar residues are perfectly alternating (HPHP .). © 1996 John Wiley & Sons, Inc.
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    Topographic analysis of the S7 binding subsite of the tachykinin neurokinin-1 receptor (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 133-147 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Conformationally and configurationally restricted rotameric probes of phenylalanine have been incorporated in the sequence of substance P (SP) - Arg-Pro-Lys-Pro-Gln-Gln-Phe-Phe-Gly-Leu-Met-NH2 - for analyzing the binding pockets of Phe7 (S7) and Phe8 (S8), in the neurokinin-1 receptor. These analogues of phenylalanine are (2S, 3R)- and (2S, 3S)-indanylglycines, E- and Z-α, β-dehydrophenylalanines, and 2(S)-α, β-cyclopropylphenylalanines [ΔE Phe, ΔZPhe, ▿E2(S)Phe, and ▿Z2(S)Phe]. Binding data obtained with either conformationally (Ing diastereoisomers) or configurationally (ΔEPhe, ΔZPhe) probes have unveiled large differences in the binding potencies of these rotameric probes. With the support of nmr data and energy calculations done on these SP-substituted analogues, we attempt to answer questions inherent to such study. First, none of these six probes prevents the formation of bioactive conformation(s) of the backbone of SP. Second, both diastereoisomers (S, S) and (S, R) of indanylglycine preferentially adopt, in the sequence of SP, the gauche (-) and trans side-chain orientations, respectively, as previously postulated from energy calculations with model peptides. However, in solution, the difference in energy between these rotamers included in the sequence of SP, compared to model peptides, is smaller since the other rotamer can be detected in [(2S, 3R) Ing7]SP. Finally, from this study we can hypothesize that the large variations observed in the affinities of Phe7 substituted analogues of SP must come from steric hindrance in the S7 binding site, which drastically restricts the space filling around the Cα (SINGLE BOND) Cβ bond of residue 7. © 1996 John Wiley & Sons, Inc.
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    Conformational and stacking properties of 3′-5′ and 2′-5′ linked oligoribonucleotides studied by CD (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 173-182 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Comparative CD studies have been carried out to characterize the properties of 2′-5′ and 3′-5′ oligoriboadenylates and oligoribouridylates from dimer to decamer. The CD band of the 3′-5′ oligoribonucleotides was larger than that of the 2′-5′ oligoribonucleotides and increased with the increase in chain length, while the CD band of the 2′-5′ oligoribonucleotides increased little beyond the dimer level. The CD analysis of the chain length dependency revealed that the 3′-5′ oligoribonucleotides adopt mainly the base-base stacking interaction, while the base-sugar interaction is predominant in the 2′-5′ oligoribonucleotides. The CD intensity of 3′-5′ oligoribonucleotides decreased to a larger extent at elevated temperatures or in the presence of ethanol compared to that of the 2′-5′ counterparts. Mg2+ or Mn2+ ion enhanced the magnitude of the CD of 3′-5′ octariboadenylate, while a small decrease in the CD was observed by the presence of Mg2+ or Mn2+ ion to the 2′-5′ octariboadenylate. The 3′-5′ oligoribonucleotide is likely conformationally flexible and can form helical ordered structure with strong base-base stacking depending on changes in the environment such as temperature, the presence of Mg2+ ion, or hydrophobicity of the solution. © 1996 John Wiley & Sons, Inc.
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    Characteristic interaction of Ca2+ ions with elastin coacervate: Ion transport study across coacervate layers of α-elastin and elastin model polypeptide, (Val-Pro-Gly-Val-Gly)n (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 189-198 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ion transport characteristics across a macrocoacervate layer membrane composed of aqueous elastin model polypeptides with a specific repeating pentapeptide sequence, H-(Val-Pro-Gly-Val-Gly)n-Val-OMe (n ≥ 40), were investigated. Transmembrane potential responses for NaCl, MgCl2, and CaCl2 concentration-cell systems were measured and examined systematically by comparing with those across a coacervate membrane composed of bovine neck ligamental α-elastin. In the case of the NaCl and MgCl2 systems, potential responses across these protein liquid membranes were different noticeably from each other depending upon the molecular structure with and without charged peptide side chains, whereas in the CaCl2 systems the transmembrane potential responses across the noncharged polypentapeptide coacervate membrane were comparable with those across the α-elastin coacervate membrane carrying both the positively and negatively charged amino acid residues as an amphoteric ion-exchange membrane. These results indicated that mechanisms of major Ca2+ ion transport are based on the specific and selective interactions with electrically neutral sites of elastin, such as the polypentapeptide backbone chain. © 1996 John Wiley & Sons, Inc.
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    Free energy simulations of axial contacts in sickle-cell hemoglobin (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 221-242 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Molecular dynamics simulations have been used to investigate the thermodynamic stability of axial contacts in sickle-cell hemoglobin (HbS). Free energy changes were evaluated for the point mutation β121 Glu → Gln in the axial contact region of HbS crystals. The calculations predict a free energy change of -3.6 kcal/mol per contact for the mutation, which is in qualitative agreement with experimental observations of aggravated sickling found in the double mutant Hb D Los Angeles (β6 Glu → Val, β121 Glu → Gln) relative to HbS (β6 Glu → Val). The β121 Glu is sequestered in a salt link with β17 Lys located on the same polypeptide chain, making the Glu interactions with its surroundings similar in aggregates and individual hemoglobins. Due to this cancellation of the large electrostatic Glu contributions, the weak nonspecific interactions between the Gln and the neighboring polypeptide chain are the main contributing factor to the enhanced aggregation of Hb D Los Angeles relative to HbS. Together with the previous study of the lateral contact [K. Kuczera et al. (1990) Proceedings of the National Academy of Science USA, Vol. 87, pp. 8481-8485], the present results provide a more complete picture of the forces driving the sickling aggregation. A comparison of different treatments of internal flexibility in free energy simulations and analysis of rate of convergence of the different calculated properties has also been performed. © 1996 John Wiley & Sons, Inc.
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    Molecular modeling of closed circular DNA thermodynamic ensembles (1996)
    New York : Wiley-Blackwell
    Biopolymers 39 (1996), S. 243-258 
    Details
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Many modeling studies of supercoiled DNA are based on equilibrium structures from theoretical calculations or energy minimization. Since closed circular DNAs are flexible, it is possible that errors are introduced by calculating properties from a single minimum energy structure, rather than from a complete thermodynamic ensemble. We have investigated this question using molecular dynamics simulations on a low resolution molecular mechanics model in which each base pair is represented by three points (a plane). This allows the inclusion of sequence-dependent variations of tip, inclination, and twist. Three kinds of sequences were tested: (1) homogeneous DNA, in which all base pairs have the helicoidal parameters of an ideal, average B-DNA; (2) random sequence DNA; and (3) curved DNA. We examined the rate of convergence of various structural parameters. Convergence for most of these is slowest for homogeneous sequences, more rapid for random sequences, and most rapid for curved sequences. The most slowly converging parameter is the antipodes profile. In a plasmid with N base pairs (bp), the antipodes distance is the distance dij from base pair i to base pair j halfway around the plasmid, j = i + N/2. The antipodes profile at time t is a plot of dij over the range i = 1, N/2. In a homogeneous plasmid, convergence requires that the antipodes profile averaged over time must be flat. Even in the small plasmids examined here, the average properties of the ensembles were found to differ from those of static equilibrium structures. These effects will be even more dramatic for larger plasmids. Further, average and dynamic properties are affected by both plasmid size and sequence. © 1996 John Wiley & Sons, Inc.
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