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  • 101
    Electronic Resource
    Electronic Resource
    Polybutadiène hydroxytéléchélique, 6Partie 5: cf. J. Gonzalez de la Campa, Q. T. Pham, Makromol. Chem. 182, 1415 (1981).. Cinétiques et thermodynamique de condensation de quelques monoalcools et du polybutadiéne hydroxytéléchélique anionique avec les monoisocyanates en l'absence de catalyseur (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1669-1683 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The kinetics and thermodynamics of the spontaneous condensation between monoalcohols (trans-2-hexene-1-ol, 1-octanol, geraniol) and commercial hydroxytelechelic polybutadiene G1000 with propyl isocyanate and phenyl isocyanate in toluene were examined. In all the condensations studied, the third order law is fulfilled. Deviations from the second order law are observed for conversions higher than 60 to 80%. In all cases, autoassociation of the alcohols plays an important role. The rate constants increase with decreasing concentration of hydroxyls and autocatalysis is noticeable. In comparison with the monoalcohols, the different behaviour of the G1000 diol should be due to its trend to be strongly associated by its two hydroxylated chain ends.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840813
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  • 102
    Electronic Resource
    Electronic Resource
    Structural investigations on cellulose tricarbanilate: Conformation and liquid crystalline behaviourDedicated to professor Dr. H.-J. Cantow on the occasion of his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1749-1760 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The phase behaviour of cellulose tricarbanilate (CTC) in ethyl methyl ketone (MEK) solutions was studied in the concentration range of 0,2 - 0,8 g/ml as a function of the temperature. By analyzing the textures in the polarizing microscope and by differential scanning calorimetry experiments several different phase transitions and mesophases were detected. At a concentration below 0,6 g/ml CTC in MEK, phase transitions were observed from the crystalline through a liquid crystalline (cholesteric) to the isotropic state. At concentrations higher than 0,6 g/ml, a different behaviour of the CTC solutions was detected and several transitions were found, but only the cholesteric-isotropic transition could be identified. The concentration dependence of the cholesteric-isotropic transitions was determined over the whole concentration range. The conformation of the CTC molecule was studied and a stiff, almost cylindrically shaped 3/2 helix with a repeat distance of 15,25 Å is proposed.
    Additional Material: 14 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840818
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  • 103
    Electronic Resource
    Electronic Resource
    Polymerization of methyl methacrylate initiated by a Rh(I) complex and benzoyl peroxide (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1901-1906 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The polymerization of some vinyl monomers initiated by carbonylchlorobis(triphenylphos-phine)rhodium(I) (RhCl(CO)(P(C6H5)3)2) and benzoyl peroxide (BPO) was studied. The polymerization ability was found to decrease in the following order: methyl methacrylate (MMA) 〉 styrene 〉 vinyl acetate 〉 isobutyl vinyl ether. In the polymerization of MMA, the average molecular weight increases with an increase in monomer conversion. On the basis of the kinetic studies of the polymerization of MMA initiated by RhCl(CO)(P(C6H5)3)2 and BPO (the mole ratic [BPO]/[RhCl(CO)(P(C6H5)3)2]) was between 1 and 7, the rate of polymerization, Rp' can be expressed by the following equation: \documentclass{article}\pagestyle{empty}\begin{document}$$R_{\rm p} = k\left[ {{\rm RhCl}\left( {{\rm CO}} \right)\left( {{\rm P}\left( {{\rm C}_6 {\rm H}_5 } \right)_3 } \right)_2 } \right]^{0,25} \cdot \left[ {{\rm BPO}} \right] \cdot \left[ {{\rm MMA}} \right]$$\end{document} The overall activation energy for the MMA polymerization was found to be 75,3 kJ/mol within the temperature range of 50 to 80°C. The composition curve of the copolymerization of styrene with MMA using RhCl(CO)(P(C6H5)3)2 and BPO agrees with that of the ordinary radical polymerization. On the basis of these results the initiation mechanism is discussed.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840916
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  • 104
    Electronic Resource
    Electronic Resource
    The solid-state polymerization, physical properties, and crystal structures of diacetylene mixed crystalsDedicated to Prof. Dr. H.-J. Cantow on the occasion of his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1945-1955 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Suitable substituted diacetylenes, 2,4-hexadiynylene di-p-toluenesulfonate (1a) and 2,4-hexadiynylene di-p-fluorobenzenesulfonate (1b), were cocrystallized to form substitutional solid solutions. By solid state polymerization of mixed crystals of 1a and 1b single crystals of the corresponding copolymers were obtained. The polymerization rate can be varied over a wide range by admixture of the comonomer 1b in the lattice of 1a. The crystal structures of monomer 1b and of the corresponding polymer, 2b, were determined. It was found that the packing of the reactive triple bond systems is identical in both monomers. Comonomer 1b acts as a defect site with a high probability of chain termination.
    Additional Material: 9 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840921
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  • 105
    Electronic Resource
    Electronic Resource
    Polymerization of lactams, 64Part 63: cf.22. Nonactivated anionic polymerization of 2-pyrrolidone in the presence of quaternary ammonium cationsDedicated to Professor O. Wichterle on the occasion of his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1987-1996 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The effect of addition of quaternary ammonium halides was studied in the nonactivated polymerization of 2-pyrrolidone (1) initiated with the potassium salt of 2-pyrrolidone (2-oxo-1-pyrrolidinylpotassium) (2). The polymerization was accelerated upon small additions of Me4NCl, whereas addition of Et4NBr and Bu4NBr rather had a retardation effect and reduced the molecular weight of polymer. The formation of the corresponding quaternary ammonium salts of 2-pyrrolidone in situ is analogous to the formation of the pure salts in their synthesis from the ammonium halides. The nonactivated polymerization of 1 initiated with the pure tetramethylammonium salt of 2-pyrrolidone (3) showed all kinetic features of other nonactivated polymerizations of 1. High yields and molecular weights of poly(2-pyrrolidone) and a higher number of growth centers during polymerization are evidence of a higher dissociation of 3 dissolved in 1 in comparison with 2 as the initiator. The activation energy of polymerization activated with 3 (47,9 kJ · mol-1 in the range 35 to 55°C) and the reaction order with respect to 3 (1,3 at 45°C) were determined.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841004
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  • 106
    Electronic Resource
    Electronic Resource
    Hydrolysis of phenyl esters catalyzed by alternating copolymers containing imidazolyl and carboxyl groups (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2041-2047 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The alternating copolymer, poly(N-vinylimidazole-co-maleic acid) (4), and the random copolymer, poly(N-vinylimidazole-co-acrylic acid) (5), with nearly the same ratio of carboxyl groups to imidazolyl groups, were found to catalyze the hydrolysis of 3-acetoxy-N-trimethyl-anilinium iodide (1), 4-nitrophenyl acetate (2), and 4-acetoxy-3-nitrobenzoic acid (3). For these esters, the catalytic activity of 4 at pH 〉9 was found to be in the following order: 3 〉 2 〉 1 that for 1 being a retarding one. Copolymer 5 shows a reverse catalytic activity of the order 1 〉 2 〉 3. The catalytic site of the alternating copolymer 4 is the free imidazolyl group, and the reaction rate is enhanced by the carboxylate anion, whereas the reaction rate in the presence of the random copolymer 5 is controlled predominantly by electrostatic interaction forces between the substrate and sequential carboxylate anions.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841009
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  • 107
    Electronic Resource
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    Orientation of ketones embedded in a polyethylene matrix. Infrared dichroic studyDedicated to the 70th birthday of Prof. O. Wichterle (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2075-2080 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Low-molecular weight ketones embedded in polyethylene films were oriented by cold drawing of the films and the effect of temperature on the orientation was studied by IR dichroism. The loss of orientation of the low-molecular weight ketones with temperature is discussed on the basis of the Cohen-Turnbull model of “free volumes”.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841012
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  • 108
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    Determination of the polarization direction of the UV bands of chromophore molecules by use of cyclodextrins (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2123-2132 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Cyclodextrins (CDxs) were utilized to determine the polarization direction in the UV bands of aromatic compounds. By choosing CDxs of suitable size for an axial inclusionAxial inclusion is the inclusion in which the long-axis of arenes is parallel to the axis of the CDxs' cavity., the induced circular dichroism (ICD) bands of the included chromophore molecules are well resolved. Thus, except for the bands which consist of two or more perpendicularly polarized transitions with quite a different oscillator strength, the polarization direction is simply determined from the sign of ICD spectra: a plus sign is produced by transitions polarized parallel to the long-axis while a negative sign by those polarized along the short-axis. Besides being simple, this method is applicable to bands as short as 195 nm, since water is used as solvent. Thus, several UV bands of some compounds were recorded for the first time and even their polarization directions were determined. Merit and limitation of this method are discussed and compared with other methods.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841016
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  • 109
    Electronic Resource
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    Announcements of conferences on macromolecular science in 1984 (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2193-2194 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841023
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  • 110
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    Study on the molecular weight dependence of dilute solution properties of narrowly distributed polystyrene in toluene and in the unperturbed stateDedicated to Prof. Dr. H.-J. Cantow on the occasion of his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2173-2186 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Intrinsic viscosities [η], second and third virial coefficients A2 and A3, respectively, and mean square radius of gyration 〈RG2〉 of a polymer homologous series of narrow-molecular-weight-distribution polystyrene samples in a molecular weight range of 2000 up to 24 · 106 were determined in toluene at 25°C by light scattering and viscometry measurements. The results are (3 · 104 〈 Mw 〈 24 · 106, Mw/Mn ≤ 1,3): \documentclass{article}\pagestyle{empty}\begin{document}$$\begin{array}{l} \left[ \eta \right]{\rm /}\left( {{\rm cm}^3 .{\rm g}^{{\rm - 1}} } \right){\rm = 8,62 } \cdot {\rm 10}^{{\rm - 3}} \cdot M_{\rm w}^{0,736} \\ A_2 /\left( {{\rm mol} \cdot {\rm cm}^3 .{\rm g}^{{\rm - 2}} } \right){\rm = 5,24} \cdot {\rm 10}^{{\rm - 3}} \cdot {\rm }M_{\rm w}^{ - 0,21} \\ A_3 /\left( {{\rm mol} \cdot {\rm cm}^6 .{\rm g}^{{\rm - 3}} } \right){\rm = 9,12} \cdot {\rm 10}^{{\rm - 6}} \cdot {\rm }M_{\rm w}^{0.58} \\ \left\langle {R_{\rm G}^2 } \right\rangle _{\rm W}^{{1 \mathord{\left/ {\vphantom {1 2}} \right. \kern-\nulldelimiterspace} 2}} /{\rm cm = 1,10} \cdot {\rm 10}^{{\rm - 9}} \cdot M_{\rm W}^{0.603} \\ \end{array} $$\end{document}These results were obtained by consideration of the limit of the dilute solution regime, the determination of zero-shear rate intrinsic viscosities, and the molecular weight dependence of the refractive index increment dn/dc. It was found that dn/dc increases slightly up to Mw = 1,8 · 106. A comparison of the [η]-Mw-relationship with literature data is given. In addition the unperturbed (theta) dimension parameters K0, 〈h2〉0/M, the characteristic ratio C∞, the steric factor σ, and the thermodynamic interaction parameter B were calculated from the modified Burchard-Stockmayer-Fixman procedure using polymolecularity correction and the results compared with experimental data from the literature.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841021
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  • 111
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    Syntheses and chelating properties of polymer-supported macrocyclic polythioethers (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2431-2436 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polymer-supported macrocyclic polythioethers (7a, b, and 8) were prepared from chloromethylated polystyrene resins (6) and 14- or 20-membered a hydroxyl group containing polythioethers (3a, b, and 5), which were synthesized by the reaction of the corresponding dithiols with 1,3-dichloro-2-propanol (2). The polymer-supported polythioethers were found to be highly efficient adsorbents of Ag(I), moderately effective for Cu(II), but less effective for Cd(II). For Ag(I) the binding ability of 7a is almost independent of the morphology of the polymer support, whereas for Cu(II) the binding ability depends on the morphology. Adsorbed Ag(I) or Cu(II) were removed by treatment with an ammonia solution from the polymer-supported macrocyclic polythioethers, which can be re-used without a significant decrease in binding ability.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841204
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  • 112
    Electronic Resource
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    Alternating copolymers of vinyl chloride and isobutylene with alkyl acrylates: Synthesis with an ethylaluminium dichloride catalyst and 13C NMR characterization (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2457-2466 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Copolymerizations of alkyl acrylates (alkyl: ethyl, butyl, isobutyl, tert-butyl, and 2-ethylhexyl) with vinyl chloride and isobutylene in the presence of catalytic amounts of C2H5AlCl2 were studied. Depending on the inonomer feed, equimolar or acrylate-rich copolymers were obtained in most of these reactions. Only tert-butyl acrylate does not produce any copolymers, due to its decomposition under the action of C2H5AICI2. 2-Ethylhexyl acrylate forms with isobutylene only acrylate-rich copolymers. By 13C NMR spectroscopy it could be shown that equimolar copolymers have an alternation structure.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841207
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  • 113
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    Elementary reactions in the cationic polymerization of oxepane. Comparison with the polymerization of tetrahydromfuran (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2497-2518 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: In the polymerization of oxepane (OXP), initiated with derivatives of trifluoromethanesulfonic acid, covalent and ionic active centers were simultaneously observed by 1H and 19F NMR spectroscopy. A higher proportion of secondary oxonium ions (these species detected by 19F NMR were independently observed by proton trapping with R3P in the 31P NMR spectrum). The proportion of ionic species decreases with monomer conversion, indicating a substantial contribution of bimolecular ionization of the monomer. The effective molarity in oxepane polymerization [OXP]eff ⋍ 1 mol ·I-1 was found to be lower by a factor of 102 than [THF]eff in the polymerization of THF. The rate constant of the covalent propagation in the polymerization of OXP is similar to that measured for THF, however, due to the reduced reactivity of the oxepanium cation, the relative reactivity of the covalent active centers becomes higher than that of the ions. Thus, for OXP, in CH3NO2 at 25°C, Kpc = 3 · 10-4 mol-1 · 1 · s-1, kpi = 2 · 10-4 mol-1 · 1 · s-1 whereas for THF kpc = 5 · 10-4 mol-1 · 1 · s-1 and kpi = 2 · 10-2 mol-1 · 1 · s-1 under similar conditions. The rates of ionization and temporary termination, measured by the “temperature jump” technique, allow to determine the contributions of inter-and intramolecular ionizations. These rates becomes equal at [OXP] = 1 mol · 1-1 (= [OXP]eff).
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841211
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  • 114
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    Non-newtonian flow behaviour of poly(decyl methacrylate) solutions (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2539-2551 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The viscosity of solutions of poly(decyl methacrylate)s, PDMA, in 1-pentanol (thermodynamically poor solvent) and in toluence or isooctane (good solvents) was measured up to shear rates of 3 · 104s-1 by means of rotational viscosimeters. The observed pronounced shear thinning is for all solutions well described by the theory of Graessley, with the extension, introduced by Ito. Two parameters, resulting from the evaluation of the flow curves on the basis of the above theory, are discussed: τ0, a characteristic relaxation time of the polymer chain, is found to be in the range of ms. ηfric, a frictional parameter, independent of shear rate, amounts upto 50% of the zero-shear viscosity for the measured solutions. Both, τ0 and ηfric, increase with decreasing solvent quality, increasing molecular weight, and increasing concentration, in accord with theory. A comparatively sharp downward bend, separating two power-law regimes, shows up with moderately concentrated solutions, as the shear rate exceeds about 103 to 104 s-1. This transition is tentatively interpreted as an orientation of the long side chains of PDMA.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841214
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  • 115
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    Poly(ethylene glycol)s grafted onto crosslinked polystyrenes, 2Part 1: cf. 1.. Multidetachably anchored polymer systems for the synthesis of solubilized peptidesProfessor Hans-Joachim Cantow zum 60. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2603-2617 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Poly(ethylene glycol)s grated onto suitably functionalized, crosslinked polystyrenes were introduced as a new class of multidetachably immobilized hydrophilic macromolecular supports for the synthesis of peptides. This new polymeric carrier system facilitates both the homogeneous solvation of the reaction site and the insolubilization of the substrate, which are prerequisites for an efficient multistep synthesis using polymeric supports. In these support systems, a strongly solvated hydrophilic linear chain molecule, poly(ethylene glycol) (PEG)Systematic IUPAC name: α-Hydro-ω-hydroxypoly(oxyethylene)., is attached to an insoluble, crosslinked polystyrene through suitable anchoring linkages. At the free chain end of this supported PEG, amino acid residues were stepwise incorporated following the standard synthetic methodology for peptides. A special feature of these new carriers is that the use of an orthogonal set of anchoring linkages to connect the polystyrene, PEG and the peptide provides access to the PEG-bound solubilized peptide or to the free peptide, as desired. The applications of these new polymeric supports are illustrated by the synthesis of thioredoxin partial sequences in the free and PEG-bound solubilized forms.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841219
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  • 116
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    Perméabilité des matériaux copolymères: modélisation moléculaire, 1. Essai d'application d'un modèle de percolation (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2661-2667 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The diffusion of small molecules across a copolymer membrane is simulated as a site percolation problem, assuming that in copolymers consisting of A and B units, B are active sites and A are inactive sites. Molecular modeling is conducted in three steps: (i) generation of a copolymer by a Monte-Carlo process, taking into account the sequence distribution of the copolymer, (ii) organization of the material through a slipping process of the linear chain towards maximization of the dipolar interactions between the A units, and (iii) the site percolation itself. A quantitative application is carried out for acrylonitrile/methyl acrylate copolymers. The results show that the influence of the slipping process upon the internal organization of the material is most important.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021841223
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  • 117
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    Propylene polymerization on titanium-magnesium catalysts, 2Part 1: cf.9.. Study of catalyst formation (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2421-2429 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Formation of a supported titanium-magnesium catalyst for propylene polymerization was studied using highly dispersed magnesium chloride (surface area ca. 100 m2/g). By means of X-ray diffraction, chemical analysis, and measurement of the surface area it was found that: i) interaction of ethyl benzoate (EB) with MgCl2 results in the formation of a compound EBEB·MgCl2 (1:1 by mole); ii) milling of products nEB · MgCl2 (n 〈 1) results in the decomposition of the lattice of the compound EB · MgCl2 and in the decrease of the size of MgCl2 crystallites; iii) treatment of the product nEB · MgCl2 with titanium tetrachloride results in the removal of a part of EB in the form of an EB·TiCl4, complex from the support, the decomposition of the lattice of the compound EB·MgCi2 an increase of the size of the MgCl2 crystallites, and a sharp increase of the surface area; iv) a small amount of EB (EB/MgCl2 = 0,1 to 0,2) considerably increases the isoptacticity of polypropylene. The high activity of catalysts prepared by milling is due to a higher surface area of these catalysts compared to unmilled samples.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841203
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  • 118
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    Synthese der cyclischen oligomere des butylenterephthalatsTeil der Dissertation F. J. Müller, RWTH Aachen 1978.Herrn Prof. Dr. H. J. Cantow zum 60. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2487-2495 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Cyclic oligomers of butylene terephthalate (16a - d) were synthesized by cyclocondensations of the corresponding dicarboxylic acid dichlorides (2 or 13) with diols (4, 10, or 15). The linear educts 2, 4, 10, 13, and 15 were obtained by stepwise synthesis. The resulting cyclic esters 16a - d were characterized by IR, NMR, and mass spectroscopy.
    Additional Material: 2 Tab.
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    Interaction between polynucleotides in aqueous NaCl solution, 5Part 4: cf. 6.. Temperature dependence of the heat of formation of poly(I) · poly(C) duplex (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2529-2538 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The heat of mixing of equimolar solutions of poly(I) and poly(C) containing various NaCl concentrations was measured at 288 and 308 K, and the heat of formation of Poly(I) · poly(C) duplex from the randomly coiled constituents, poly(I) and poly(C), was estimated from the heat of mixing with the aid of CD measurements. The temperature dependence of this heat of formation, ΔH, differs at lower and higher NaCl concentrations: In the region of NaCl concentration less than 0,5 mol · dm-3, ΔH increases with temperature, while in the region of NaCl concentrations higher than 0,5 mol · dm-3, ΔH decreases with temperature. The free energy change, ΔG, of the formation of poly(I) · poly(C) duplex decreases as the NaCl concentration increases, that is, the stability of poly(I) · poly(C) duplex increases with NaCl concentration. Moreover, the conformation of poly(I) · poly(C) duplex seems to differ at lower and higher NaCl concentration as derived from the CD spectra and the thermodynamic quantities.
    Additional Material: 7 Ill.
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    Proton NMR studies on n-paraffins in restricted molecular motion (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2581-2592 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The 1H NMR spectra of guest molecules, n-paraffins (n-C5H12, n-C6H14, n-C7H16, n-C9H20, nC10H22, nC11H24, n-C12H26, n-C15H32, n-C16H34, n-C21H44 and n-C22H46), were measured in poly(γ-benzyl-L-glutamate) liquid crystalline solution. The methylene signal of n-paraffins is a doublet due to magnetic dipole-dipole interaction. These results suggest that an n-paraffin takes predominantly the extended form in the restricted molecular motion state and that its long axis orients in the same direction as the helical axis of poly(γy-benzyl-L-glutamate) parallel to the magnetic field. The results are compared with the molecular motion and conformation of η n-paraffins in α-chloronaphthalene.
    Additional Material: 9 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841217
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    Instantaneous shape and relative orientation of model chains as a function of their intermolecular separationDedicated to Prof. Dr. H.-J. Cantow on occasion of his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2619-2634 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Ensembles of self avoiding five-way cubic lattice chains consisting of 50 segments were generated for athermal and θ-conditions, and the instantaneous shape and the orientation of each chain were characterized by evaluation of the squared three axes L21, L22, and L23 of its equivalent ellipsoid and their orientation in space; the variation of these quantities within allowed pair configurations (relative to their values in isolated chains) was studied as a function of the separation R between the two centers of gravity of the two members of all isolated chain pairs, which could be formed from the ensemble. For small R (when R is smaller than the average radius of gyration of isolated chains 〈s2〉1/20) L23, the squared longest axis of the equivalent ellipsoid, is strongly expanded for athermal as well as for θ-conditions, while the squared two shortes axes, L21 and L22, are much less enlarged or even decreased in this range, thus emphasizing the prolate character of the ellipsoids on approaching R = 0. Furthermore the angle between the two L3-axes of the two chains forming a compatible pair is remarkably increased at vanishing separation (by ca. 10° in athermal systems and by ca. 7° in θ-systems). Thus, chains forming compatible pairs at R = 0 not only have to increase their dimensions (as already described earlier) but also have to change their instantaneous shape (towards a still higher anisotropy of the equivalent ellipsoids) and their relative orientation (the longest axes L3 tend towards orthogonal orientation) in order to relieve the thermodynamic stress which they impose on each other. By integration of the effects over all separations the concentration dependence of all quantities was determined in the limit of zero concentration. Most quantities are subject to an appreciable, non-zero concentration dependence. Contrary to most theoretical predictions this is also true for θ-conditions.
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    Differential scanning calorimetric studies on bound water in 1,4-dioxane acidolysis lignin (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1265-1274 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The amounts of three different types of water adsorbed on hydrolyzed lignin, which was obtained by acid hydrolysis of softwood meal in 1,4-dioxane containing trace amounts of hydrochloric acid (in the following called DL), and on its derivatives, i.e., methylated and acetylated lignins, were determined by differential scanning calorimetry (DSC). The first type of water is non-freezing water, the glass transition of which was detected by DSC. The second type of water corresponds to a kind of bound water which was detected from a crystallization peak in the vicinity of 225 K (peak II). This peak appeared when the water content exceeded a critical amount of non-freezing water. The third type of water is free water, the crystallization peak (peak I) of which was found at the same temperature as that of pure water. From the enthalpies of crystallization of the above two types of water and the known weight of sorbed water, the amount of bound water in DL was determined to be 0,10 (weight of bound water/weight of dry sample). Furthermore, it was found that bound water breaks hydrogen bonds in DL and decreases its glass transition temperature (Tg) from 425 K to 330 K. The amount of hydroxyl groups, which varies with the degree of methylation or acetylation, was also found to affect the bound water content and inevitaby to decrease T g.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021840616
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    High conversion copolymerization, 1. Kinetics of the copolymerization of styrene and maleic anhydride (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1295-1302 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The copolymerization of styrene (S) with maleic anhydride (MAn) in 1,4-dioxane at 60, 70 and 80°C up to high conversion (≈ 98%) was followed by differential scanning calorimetry. The rate of copolymerization increases up to 20 - 40% conversion of both monomers and then gradually decreases to zero. The increase in the copolymerization rate is more pronounced for equimolar ratios [S]/[MAn] as compared to ratios with an excess of S. For a given mole ratio of S and MAn the copolymerization rate in 1,4-dioxane is higher at higher total monomer concentrations and/or at higher temperatures. The heat of copolymerization is 81,6 kj · mol-1 for the equimolar [S]/[MAn] mixture. For mixtures with [S]/[MAn] 〉 1 the heat of reaction is between 70 and 80 kj · mol-1. The limitingconversion of styrene for [S]/[MAn] = 1 is about 98%, and for [S]/[MAn] 〉 1 it is a function of the [S]/[MAn] ratio. Assuming exclusively the formation of an alternating S/MAn copolymer the following relation is derived. \documentclass{article}\pagestyle{empty}\begin{document}$$\begin{array}{*{20}c} {\ln \left[ {\left( {\bar k_p /\bar k_t^{0,5} } \right)/\left( {{\rm dm}^{3/2} \cdot {\rm mol}^{ - 1/2} \cdot {\rm s}^{ - 1/2} } \right)} \right] = 2,478 - \frac{{8570}}{{{\rm RT}/\left( {{\rm J} \cdot {\rm mol}^{ - 1} } \right)}}} \hfill \\ {\left( {{\rm R} = 9,31441{\rm J} \cdot {\rm K}^{ - 1} \cdot {\rm mol}^{ - 1} } \right)} \hfill \\ \end{array}$$\end{document} for the ratio of the apparent rate constants of propagation k̄p, and termination k̄〈/t.
    Additional Material: 4 Ill.
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    Selective step-growth phenol-aldehyde polymerization, 2Part 1: cf.1.. Synthesis of 4-tert-butylphenol novolac resins and related open chain oligomeric compounds (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1363-1378 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Constitutionally regular all-ortho 4-tert-butylphenol-formaldehyde novolac resins were prepared free from cyclic compounds, by reaction of bromomagnesium 4-tert-butylphenoxide in aprotic nonpolar media with paraformaldehyde. Short syntheses of dinuclear to decanuclear methylene-linked chain oligomers were also achieved via bromomagnesium ion-assisted reaction of suitable phenolic precursors with paraformaldehyde or 5-tert-butyl-2-hydroxybenzyl alcohol.
    Additional Material: 4 Ill.
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    Study of the nature of radical polymerization of methyl methacrylate with “aged” chromium(II) acetate/benzoyl peroxide (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1423-1439 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The polymerization of methyl methacrylate (MMA) in DMF with “aged” chromium (II) acetate (Cr(Ac2)) and benzoyl peroxide (BPO), previously formulated as a living radical polymerization, was investigated. The reaction between Cr(Ac)2 and BPO gives besides N-methylformamidomethyl benzoate (3) the N-methylformamidomethylchromium(III) cation (6) as intermediate, which itself may react with BPO with the formation of additional free radicals as compared with the thermolysis of BPO. Thus, the polymerization of MMA in this system could be shown to be a normal radical one with free and uncomplexed radicals. The increase of the degree of polymerization with aging and monomer conversion is explained by the decreasing rate of the radical forming reactions and the onset of the gel effect.
    Additional Material: 9 Ill.
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    Chiral configuration in the complexes of poly (Nε-alkyl-L-lysine)s with alkylamino azo dyes (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1479-1487 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Absorption and circular dichroism (CD) spectra were measured on the complexes of poly(Nε-alkyl-L-lysine)s and alkyl azo dyes. Absolute configuration of the complexes was examined by the exciton chirality method. Most complexes show S-chirality of the transition dipole moments of dyes. Increased hydrophobic properties of both dye molecule and polypeptide side-chains change the chirality of dye from common S- to uncommon R-chirality. The induced CD results are discussed from the point of view of hydrogen bonding, electrostatic, and hydrophobic properties of both dyes and polypeptides.
    Additional Material: 8 Ill.
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    A general method for the determination of “monomolecular property versus molar mass relationships” from measurements on polymolecular polymersHerrn Professor Dr. H.-J. Cantow mit den besten Wünschen zum 60. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1509-1518 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: “Monomolecular property (p) versus molar mass (M) relationships” of the type p = Kp · Map as would result from an experimental determination of p and M of a polymer-homologous series of strictly monomolecular polymers can also be obtained from a polymer-homologous series of polymolecular samples or fractions, provided their correct corresponding averages p and M are determined (Principle of Corresponding Averages). In order to obtain the monomolecular intrinsic viscosity [η] vs. M relationship (Mark-Houwink relationship), the corresponding averages weight-average intrinsic viscosity ([η]w ≡ [η]) and viscosity-average molar mass (M[η]) of a series of polymer-homologous, polymolecular polymer samples or fractions have to be determined experimentally. Accordingly, the corresponding monomolecular relationships sedimentation coefficient s vs. M, diffusion coefficient D vs. M, and mean-square radius of gyration 〈r2〉 vs. M are obtained by the determination of a series of couples of the corresponding averages s vs. M, D vs. M, and 〈r2〉 vs. M, respectively. The experimental determination of the corresponding averages presented is possible by different methods, including the determination of the molar mass distribution.
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    Kinetics of free-radical polymerisation at high viscosities (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1603-1621 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Methyl methacrylate und styrene were polymerised by a free-radical process in solutions which contained dissolved polymer. The molecular weights of the dissolved polymer and the concentration of the radical generator 2,2'-azoisobutyronitrile were varied. Rate data were compatible with a reaction scheme in which the mobility of some growing radicals was influenced by the solution viscosity. Correlations between radical mobility and viscosity were more consistent with the experimental results than correlations between radical mobility and volume fraction of dissolved polymer. The possibility of primary radical termination is examined and a means of clarifying the chain termination process is suggested.
    Additional Material: 5 Ill.
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    Chemical modification of polydienes, 2Part 1: cf.1. Properties of polybutadiene and nitrile rubbers grafted with poly(tetrahydrofuran) (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1645-1651 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Thermal analysis by differential scanning calorimetry (DSC) indicated that graft copolymers of poly(tetrahydrofuran) (PTHF) on a nitrile rubber containing 39 wt.-% acrylonitrile have a two-phase morphology comprising crystalline PTHF and amorphous rubber. In rubbers with an 18 wt.-% acrylonitrile content the PTHF is more compatible with the rubber and exerts a plasticising effect; crystallinity of the PTHF is not as well developed. cis-1,4-Polybutadiene and PTHF are partially miscible and in grafts on these two the melting endotherm of the latter was not detected. The relative values of the solubility parameters of PTHF and the three rubbers are consistent with this behaviour. All graft copolymers have a fairly low thermal stability and begin to decompose under N2 below 200°C. Degradation appears to be initiated at the PTHF grafts. Graft copolymers of PTHF with nitrile rubbers are less resistant to petroleum than the ungrafted rubbers.
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    Phase behaviour of liquid crystalline side chain polymersDedicated to Prof. Dale J. Meier on the occasion of his 60th birthday. (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1685-1703 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The phase behaviour of liquid crystalline side chain polymers is investigated by different experimental methods. PVT- and DSC-measurements as well as X-ray and optical investigations show that additionally to the known factors from low molecular weight liquid crystals the flexibility of the polymer backbone influences the liquid crystalline properties of the phase. Fixing a mesogenic side chain to a polymer backbone leads to a stabilisation or even a generation of a liquid crystalline phase in comparison to the corresponding low molecular weight liquid crystals.  -  The liquid crystalline phases which are known from low molecular weight liquid crystals are also found for liquid crystalline polymers (nematic, chiral-nematic, smectic). In contrast to low molecular weight liquid crystals the phase transformations smectic to crystalline and chiralnematic to smectic show strong time dependences for polymeric substances.  -  A crystallization of the liquid crystalline side chain polymers is observed, when the polymer main chain is so flexible, that the mesogenic groups can form a crystalline order. The crystallization process leads for a smectic sample to a layer lattice structure. From X-ray investigations one can conclude that the smectic arrangement of the mesogenic side chain exhibits a preorder for the crystalline structure. As known from other substances the crystallization rate depends on temperature and pressure.  -  The transformations in the liquid crystalline region are first-order transformations and obey the Clausius-Clapeyron equation. At lower temperatures all liquid crystalline polymers solidify to anisotropic glasses. Below the glass transition temperature nematic or smectic states of order are frozen-in and preserved in this way.
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    Biodegradable random copolypeptides of β-benzyl L-aspartate and γ-methyl L-glutamate for the controlled release of testosterone (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1761-1770 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The random copolypeptides of β-benzyl L-aspartate (β-Bz L-Asp) and γ-methyl L-glutamate (γ-Me L-Glu) were synthesized and implanted subcutaneously in rats. It was found that the resulting copolypeptides are degraded and also have good biocompatibility in vivo. On the basis of these results, poly(β-Bz L-Asp-co-γ-Me L-Glu) was tried to be used as a material for a drug delivery system. Copolypeptide-testosterone composites were prepared at a pressure of 200 kg/cm2 in the presence of a slight amount of dichloroethane. The in vivo release rate of testosterone from copolypeptide-drug composites was about 5,5 times higher than that in vitro. The in vivo release rate remained relatively constant over a period of 90 days at 0,22 mg/day. The serum testosterone concentration in castrated rats was 0,40 ng/ml and the value went up to 6,8 ng/ml after the biodegradable copolypeptide-testosterone composite was implanted and was kept constant for the duration of test.
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    Polymers containing enzymatically degradable bonds, 8Part 7: cf. ref.2. Degradation of oligopeptide sequences in N-(2-hydroxypropyl)methacrylamide copolymers by bovine spleen cathepsin BDedicated to Prof. O. Wichterle on the occasion of his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2009-2020 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Three types of copolymers of N-(2-hydroxypropyl)methacrylamide(HPMA) were prepared which contain oligopeptide sequences: (a) HPMA copolymers containing oligopeptide side-chains terminated with p-nitroaniline; (b) soluble HPMA copolymers containing oligopeptide sequences in crosslinks connecting two poly(HPMA) chains; (c) a hydrophilic gel, i.e. a three dimensional copolymer of HPMA containing an oligopeptide sequence in the crosslinks. These polymeric substrates (suitable as drug carriers) containing potentially degradable oligopeptide sequences were incubated with an intracellular proteolytic enzyme, bovine spleen cathespin B. The degradation process of the substrates made it possible to reveal the relationship between the structure of oligopeptide sequences and their degradability. The results suggest an important role played by cathepsin B in the degradation of polymeric substrates investigated in this study under physiological conditions.
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    Correlation of data on intrinsic viscosities in mixed solvents by means of the modified flory-huggins equationTo Professor O. Wichterle on the occasion of his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2081-2096 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: An equation for the total sorption potential Y derived from the modified Flory-Huggins equation and containing concentration-dependent interaction parameters, including the ternary parameter χT, was used to correlate reported data on intrinsic viscosities in mixed solvents. Similarly to the evaluation of data on preferential sorption, the assumption of proportionality between the ternary parameter and the interaction parameter of components of the mixed solvent, g12, was successfully applied to the case of total sorption. The assumption proved to be useful in the treatment of 12 ternary systems, if the single-liquid approximation was employed. The calculated proportionality constant between the ternary parameter and g12 has properties similar to that evaluated from the data on preferential sorption. The conditions of occurrence of a maximum or minimum in the dependence of total sorption on composition are discussed.
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    Study of conformational transitions of graft copolymers by UV spectrophotometry, 2Part 1: cf.9. The behaviour of poly(vinyl acetate) grafted hydroxyethyl-cellulose in selective solvents (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2133-2141 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The behaviour of poly(vinyl acetate) grafted hydroxyethylcellulose (PVAc/HEC) in the binary solvent mixture ethanol-water (90:10 by vol.) was studied by absorption spectrophotometry. The macromolecules of PVAc/HEC graft copolymer exhibit a conformational transition at ca. 55°C where they pass from a monomicelle conformation to a segregated conformation. This intramolecular transition occurs both below and above the critical micellar concentration (c.m.c). In dilute solutions a critical concentration was evidenced, which is one order of magnitude higher than the c.m.c.
    Additional Material: 9 Ill.
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    Hyperfeinstruktur in den ESR-spektren von thermisch behandeltem polyphenylacetylen (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2187-2192 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A highly resolved ESR spectrum of dissolved polyphenylacetylene has been measured at 120°C. It was found by simulation that the protons of three phenyl groups and two protons of the carbon chain contribute to the spectrum. The structure of the corresponding paramagnetic centre is given.
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    Action de différentes especes d'amorçage dans la polymérisation hydrolytique du dodécanelactame-12 (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2199-2212 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The study of the initiation step in the hydrolytic polymerization of 12-dodecanelactam showed the prominent role of chain-ends in the monomer consumption and especially that of amino end groups. Different initiators, dodecylamine hydrochloride, 12-aminododecanoic acid, or lauric acid, where employed and in some experiments water was added. This led to the formation of new end groups and thus to an enhancement of the monomer consumption rate. It could be shown that during this process large changes in the polymer chain length distribution occur.
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    Preparation and properties of poly(p-phenylene) and polynaphthylene (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2241-2249 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Poly(p-phenylene), poly(2,6-naphthylene), poly(2,7-naphthylene), poly(1,5-naphthylene), and poly(1,4-naphthylene) were prepared by nickel-catalyzed polycondensation of Grignard reagents from the corresponding dibromides. The polymers were annealed in vacuo. Doping with SbF5 markedly increase the conductivity of the polymers. Annealed poly(2,6-naphthylene) is the most conductive among the four isomers after SbF5 doping. The conductivity of doped poly(2,6-naphthylene) and poly(p-phenylene) is about 10-1 S · cm-1. Annealed poly(p-phenylene) shows a broad single line ESR signal which changes to a narrow single line upon doping. Superposition of the two signals is observed at the initial stage of doping. Simultaneous conductivity and ESR measurements indicate that the narrow signal is closely related to conductivity.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841106
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  • 138
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    Novel monomeric and polymeric azo initiators (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2285-2296 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 1-Methyl-1-(3-vinylphenylazo)ethyl acetate (1a), diphenyl-(3-vinylphenylazo)methyl acetate (1b), and α-phenylazo-α-(4-vinylphenyl)benzyl acetate (2) were prepared and copolymerized with styrene using AIBN as initiator at 50°C. The azo functions of the monomers remain unaltered during the polymerization process at this temperature. The resulting copolymers 3a, 3b, and 4 were used as initiators for the polymerization of methacrylonitrile (MAN). The grafted copolymers of styrene and MAN were separated from polystyrene and poly(methacrylonitrile). The different rates of polymerization of MAN, initiated by the azo group containing polymer 3b or 4 or by diphenylphenylazomethyl acetate, a low molecular model initiator, and the different molar masses obtained allow a discussion of the mechanism involved.
    Additional Material: 3 Ill.
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  • 139
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    Optically active vinyl polymers, 25Part 24: cf.2b.. Chiroptical Properties and Conformation of Copolymers from 4-Methyl-1-penten-3-one and (S)-4-Methyl-1-hexen-3-oneDedicated to Prof. Dr. O. Wicheterle on the occasion of his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2347-2359 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The molar optical rotation at 589 nm, the UV-, CD-and ORD-spectra of atactic and highly isotactic random copolymers of 4-methyl-1-penten-3-one (4MP3O) and (S)-methyl-1-hexen-3-one ((S)-4MH3O) were measured in different solvents at different temperatures. The ellipticity observed in the isotactic copolymers between 240 and 320 nm is much larger than that calculated for a mixture of the two homopolymers, showing that in the isotactic (but not in the atactic) copolymers chiral conformations, giving contributions of negative sign to the CD, prevail also in the monomeric units arising from the non-chiral monomer. The decrease of the ellipticity with increasing temperature for the copolymers is not linear; the average value between 20°C and 60°C is larger for the copolymers than for the homopolymers. The results indicate that in the isotactic copolymers main-chain helical conformations of one handedness are favoured over those of the opposite screw sense, and that achiral units incorporated in helical sections are forced to assume chiral conformations similar to the conformations that chiral units assume in the same helical section.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841115
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  • 140
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    Thermomechanical study of oriented poly(ethylene terephthalate): Effect of homogeneous deformation and moisture absorption (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2391-2399 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The homogeneous drawing behaviour of poly(ethylene terephthalate) (PET) at T=80°C has been studied by glass transition temperature analysis. At the first stage of homogeneous drawing (draw ratios λp up to 3,0), the results as compared to the statistical Gibbs-DiMarzio theory, suggest that the rate of the segmental motion increases with the draw ratio. In a second zone of moderate and high draw ratios (λp 〉 3) a non-negligible loss-entropy component occurs as predicted by the Gibbs-DiMarzio theory of isovolume strained network chains. The moisture absorption at room temperature causes a decrease in glass transition temperature which is more pronounced at higher draw ratios.
    Additional Material: 7 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841118
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  • 141
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    Polyarylenealkenylenes and polyheteroarylenealkenylenes, 15Part 14: cf. G. Koßmehl, P. Beimling, G. Manecke, Makromol. Chem. 184, 627 (1983).. Syntheses and electrical conductivities of alkoxylated poly(2,5-thiophenediylvinylene-1,4-phenylenevinylene)s (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2437-2445 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Poly(2,5-thiophenediylvinylene-1,4-phenylenevinylene)s with one or two alkoxy groups as side chains of variable lenghts (8a, b and 9a - c) were prepared by Wittig-reaction of 2,5-thiophenedicarbaldehyde with the corresponding “bis(Wittig-salt)s”. To establish the structure of the polymers, model compounds 10 and 11 were synthesized. Charge-transfer (donor-acceptor) complexes were prepared by iodine doping of the polyvinylenes 8 and 9. The room temperature conductivity, σ298K, of the original polymers was found to be increased by several orders of magnitude upon doping. It was not possible to remove all the iodine from the charge-transfer complexes in vacuum.
    Additional Material: 4 Tab.
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  • 142
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    Polyméres porteurs de dérivés du glycérol, 3Partie 2: cf.1.. Modification chimique du méthacrylate d′époxy-2,3 propyle et de son polymére par i′acide phényl-2 butyriqueDédié au Prof. Dr. O. Wichterle à l'occasion de son 70e anniversaire (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2467-2476 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The influence of time, temperature, and concentration on the addition rate of 2-phenylbutyric acid (1) to 2,3-epoxypropanol (4), 2,3-epoxypropyl methacrylate (2), and its polymer 3 was studied in chloroform and 1, 4-dioxane. The variation of the yeld with time and concentration of catalyst (tetramethyl ammonium salt of 1) can be fairly well represented by the equation v = k [Acid] · [Epoxide] · [Catalyst], with k ∼ 0,6 to 0,8 12 · mol -2 ·h-1 at T = 60°C and [Acid] ≈ 1 mol · 1-1. The Arrhenius activation energy was found to be 70 to 80 kJ · mol-1. With variation of the epoxide and acid concentrations, deviations were observed.
    Additional Material: 6 Ill.
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  • 143
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    Polymer-solvent interactions in mixed solvents, 5Part 4, cf. 1.. Ionized ethyl, butyl, and hexyl vinyl ether-maleic acid alternating copolymers in water/2-chloroethanol mixtures (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2519-2527 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Viscosity and preferential solvation measurements were carried out on ionized maleic acidethyl, -butyl, and -hexyl vinyl ether alternating copolymers (i-MA/EVE, i-MA/BVE, and i-MA/HVE, respectively) in water-2-chloroethanol mixtures. i-MA/EVE and i-MA/BVE are completely coiled and their preferential and absolute solvation by water and 2-chloroethanol reflects their more or less hydrophilic or hydrophobic nature. For i-MA/HVE, the viscosimetric and preferential solvation measurements suggest that, in 2-chloroethanol rich mixtures, the polymer retains a hypercoiled conformation in which an important part of the hexyl side chains are screened form contact with both componenets of the solvent mixture.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841212
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  • 144
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    Free-radical polymerization kinetics of methyl methacrylate at very high conversionsPart of a poster presentation at “Makromolekulares Kolloquium”, Freiburg/Brsg., Germany, March 4-6, 1982.Herrn Professor Dr. H.-J. Cantow mit den besten Wünschen zum 60. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2563-2579 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The free-radical polymerization of methyl methacrylate (MMA) at very high conversions (x 〉 0,8) was studied in the temperature range 60C° to 160C°. 2,2′-Azodiisobutyronitrile (AIBN) and benzoyl peroxide (BPO) were used as initiators. In the case of the latter, decomposition kinetics at very high monomer conversions was investigated, too. For temperatures T ≤ 120C° where depropagation can be neglected a simple kinetic model based on “reaction diffusion” and free volume theory was developed. The model contains only a single adjustable parameter, the critical free volume fraction V*. Good agreement between model predictions and experiments was obtained. V* is independent of initial initiator concentration and reaction temperature, and there is some evidence that V* is also independent of the chemical nature of the initiator.
    Additional Material: 9 Ill.
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  • 145
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    Properties of liquid crystalline polymers in solution, 2Part 1: cf. 1.. Viscosimetric investigations of polymethacrylates with mesogenic sidegroupsDedicated to Professor Dr. O. Wichterle on his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2635-2642 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Dilute solutions of poly(methacrylic acid) derivatives with mesogenic side groups of the benzoic acid phenyl ester type are structurally viscous. This property due to aggregation appears during storage and is attributed to the geometric shape of the dissolved particles. While solutions of freshly polymerized samples show no, or only a slight temperature dependence of the intrinsic viscosity between 298 and 368 K, the intrinsic viscosity of the stored samples decreases suddenly at temperatures above 348 K.
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841221
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  • 146
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    Structure and properties of segmented poly(ether-ester)s, 7Part 6: cf. 10.. Model triblock copolyesters of monodisperse block length (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2669-2677 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Synthesis and characterization of model triblock copolyesters, in which the two end-blocks are based on tetramethylene terephthalate and the middle block is oligo(oxytetramethylene), are described. These model copolyesters, which are essentially monodisperse, and similarly prepared segmented block copolyesters with monodisperse blocks exhibit the same dependency of the melting temperature on the degree of polymerization of the ester blocks as polydisperse technical copoly(ether-ester)s.
    Additional Material: 2 Ill.
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  • 147
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    Crystallization and stereo assocation of stereoregular PMMA, 2Part 1: cf. 13.. Crystallization behavious of the stereocomplex in comparison with that of pure stereoregular PMMADedicated to Prof. Dr. H.-J. Cantow on the occasion of his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2679-2691 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The crystallization behaviour of stereoregular PMMA was studied by means of DSC and X-ray measurements. Both nucleation and crystallization rates of i-PMMA. are slower by orders of magnitude compared with s-PMMA and with the 1:1-i/s-stereocomplex of PMMA. The investigation of the nucleation and crystallization of i-PMMA by means of the DSC method leads to the results that both nucleation and crystallization rates show a maximum in the region between melting and glass transition temperature. As a result of the fast crystallization rates of s-PMMA and the stereocomplex, however, these polymers do crystallize without annealing showing a very broad distribution of crystallite sizes. From the shape of the melting curves as a function of annealing time it can be concluded that the crystallization of i-PMMA gels leads to the formation of a physical network, which contains small and big crystallites. The results of the measurements allow the determination of the heat of stereocomplex formation. The value found of 24 J · g-1 agrees with values obtained directly on mixing dilute solutions of i- and s-PMMA. As a result of calorimetric measurements the liquidus curves of the quasi-binary systems of solvent (o-xylene) and stereoregular PMMA are obtained. Taking into account data of former work for the quasi-binary system of i-PMMA and s-PMMA, the shape of the liquidus surface in the quasi-ternary system of i-PMMA, s-PMMA, and solvent (o-xylene) can be constructed.
    Additional Material: 15 Ill.
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    URL: http://dx.doi.org/10.1002/macp.1983.021841225
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  • 148
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    Effect of zinc chloride on the radical polymerization of cyclohexyl acrylate (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 29-40 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The paper presents a study of the radical polymerization of cyclohexyl acrylate (CHA) in the presence of ZnCl2. It was found by IR, 1H NMR, and 13C NMR spectroscopy that a complex of ZnCl2 with CHA is formed. For copolymerization of CHA with vinylidene chloride, both the Q- and e-value of CHA increased with the ZnCl2 concentration. The initiation rate and kp2/kt were determined using DPPH as an inhibitor. It was found that ZnCl2 did not affect the initiation rate. The kp value of CHA was determined to be about 2720 1 · mol-1 · s-1 in the absence and 4710 1 · mol-1 · s-1 in the presence of ZnCl2 by the rotating sector method. The enhanced polymerization rate of CHA in the presence of ZnCl2 can be ascribed to the large kp value. The termination rate constant is not significantly affected by the presence of ZnCl2.
    Additional Material: 7 Ill.
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  • 149
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    Polymerization of lactams, 54Part 53: cf.1. Anionic polymerization of 2-pyrrolidone accelerated with CO2, part 3 (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 59-62 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Intrinsic viscosities in m-cresol and weight average molecular weights, M̄w, were measured for samples of high molecular weight poly(2-pyrrolidone) (poly (1)) prepared by anionic polymerization of 2-pyrrolidone (1) accelerated with CO2. It was proved that the earlier found relationship [η] = 4 · 10-2 · M0,77 (in cm3 · g-1) holds for M̄Mw up to 8 · 105 g. mol-1. The probable reason for the formation of poly (1) with an exceptionally high molecular weight is discussed.
    Additional Material: 1 Tab.
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    Studies of siloxane-acid model system: Hexamethyldisiloxane-trifluoroacetic acid (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 77-90 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The equilibrium in the system containing hexamethyldisiloxane, trifluoroacetic acid, and the inert solvent methylene chloride is studied. The system may serve as a model of reactions which play an important role in the cationic polymerization of cyclic siloxanes. The kinetic studies confirm that analogous reactions control the concentrations of silanol and silyl ester end groups as well as of acid and water during the polymerization. Allowing for some hydrogen bonding formation in the analysis of these equilibria the respective equilibrium constants can be obtained preserving almost constant values in the total range of concentrations studied.
    Additional Material: 6 Ill.
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  • 151
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    Preparation of regularly sequenced polyamides with definite numbers of oxyethylene units and their application as phase transfer catalysts (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 535-543 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyamides (1-3) having oligo(oxyethylene) segments in the main chain were prepared from α-(2-aminoethyl)-ω-aminooligo(oxyethylene)s (4) and dicarboxylic acid chlorides (5). Their ability to form complexes with alkali metal ions was examined by the picrate extraction method. The polyamides were found to catalyze the nucleophilic displacement reaction of hexyl bromide by potassium acetate in acetonitrile. An intramolecular co-operative action of oligo(oxy-ethylene) segments in complexation of potassium ion is proposed to account for the observed “polymer effect” in the catalytic activity.
    Additional Material: 4 Ill.
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    Über polyarylenalkenylene und polyheteroarylenalkenylene, 1413. Mitteilung: cf.2.. Synthesen und charakterisierung von poly(thieno[2′,3′:1,2]benzo[4,5-b]thiophen-2,6-diylvinylenarylenvinylen)en, poly(4,8-dimethoxythieno[2′,3′:1,2]benzo[4,5-b]thiophen-2,6-diylvinylenarylenvinylen)en und einigen modellverbindungenHerrn Professor Dr. H.-J. Cantow zum 60. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 627-650 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Wittig-reactions of thieno[2′,3′:1,2]benzo[4,5-b]thiophene-2,6-dicarboxaldehyde (8a) with “mono- and bis-Wittig-salts” 12a-c and 9a-c poly(thieno[2′,3′:1,2]benzo[4,5-b]thiophene-2,6-diylvinylenearylenevinylene)s 10a-c and some model compounds 13a-c were obtained. Analogous reactions of 4,8-dimethoxythieno[2′,3′:1,2]benzo[4,5-b]thiophene-2,6-dicarboxaldehyde (8b) gave the corresponding poly(4,8-dimethoxythieno[2′,3′:1,2]benzol[4,5-b]thiophene-2,6-diylvinylenearylenevinylene)s 11a-c and their model compounds 14a-c. Wittig-reactions of benzo[b]thiophene-2-carboxaldehyde (15) with “mono- and bis-Wittig-salts” gave model compounds 16a-c and 17a, c. A new synthesis of thieno[2′,3′:1,2]benzo[4,5-b]thio-phene (4) was worked out. 4,8-Dimethoxythieno[2′,3′:1,2]benzo[4,5-b]thiophene (7) and dicarboxaldehydes 8a and 8b were synthesized for the first time. The structures of all compounds were confirmed by elemental analyses, IR and electronic spectra, those of the model compounds additionally by mass spectra, and in case of sufficient solubility by 1H NMR spectra. The electrical conductivities of all polymers and their model compounds were investigated.
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    Preparation of poly[(3S)-1,2,3,4-tetrahydroisoquinoline-2,3-diylmethylene] and its use as chiral catalyst in the addition of arenethiols to 2-cyclohexen-1-one (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 675-679 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Poly[(3S)-1,2,3,4-tetrahydroisoquinoline-2,3-diylmethylene] (4) and (3S)-3-(1,2,3,4-tetrahydroisoquinolin-2-ylmethyl)-2-methyl-1,2,3,4-tetrahydroisoquinoline (7) were prepared using (3S)-1,2,3,4-tetrahydro-3-isoquinolinecarboxylic acid (1) as starting material. The optically active amines 4 and 7 were used as asymmetric catalysts for the addition of thiophenol (8a), 4-tert-butylthiophenol (8b), or 4-chlorothiophenol (8c) to 2-cyclohexen-1-one (9). 4 yielded 3-phenylthiocyclohexanone (10a) with the highest optical yield of 24% at -25°C, showing a marked polymer effect with respect to enantiomeric excess.
    Additional Material: 1 Tab.
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    Main features of hydrolysis of polymeric enaminones based on a water-soluble copolymer from N-vinyl-2-pyrrolidone and 5-methyl-5-hexene-2,4-dione (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 701-716 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Water-soluble polymeric enaminones (2) were obtained by condensation of a copolymer (1) from N-vinyl-2-pyrrolidone and 5-methyl-5-hexene-2,4-dione with amines. It was found first that polymers 2 undergo hydrolysis by water much more slowly than low molecular weight enaminones of similar structure and, secondly, their hydrolysis does not obey the pseudo-first-order rate law. These differences in the kinetic behaviour of polymers and model compounds are due, respectively, first to a steric hindrance of the attack of water at the polymer chains and, secondly, to the association of low molecular reaction products with the monomeric units of N-vinylpyrrolidone in the copolymers. A detailed study of the hydrolysis of polymeric enaminones of amino acids, characterized by extraordinary high hydrolysis rates confirmed the existence of the intramolecular base catalysis of the attack of water at the protonated enaminone by their own carboxylate groups.
    Additional Material: 5 Ill.
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    Reactions of macro-ions resulting in the formation of block and graft copolymers. Grafting of polymers with aromatic groups (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 527-534 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Grafting of poly(oxytetramethylene) (polytetrahydrofuran) chains containing living oxonium end groups onto polymers containing aromatic rings was investigated. The rate of grafting was found to be slow, but under favourable conditions several moles of polytetrahydrofuran can be grafted to one mole of polystryrene. Macrocations may also be grafted to the surface of in-soluble polymers dispersed in a solution of grafting ions. This was proved by grafting living polytetrahydrofuran onto poly(phenylene oxide) or random poly(1-butene-co-styrene). Macro-cations can be prepared from an anionic living polymer via transformation of the growing centers. Thus, poly(dimethylsiloxane), whose original anionic centers were transformated into cationic ones, was grafted to polystyrene. Exchange reactions were found to take place in the living system on polytetrahydrofuran or poly(dimethylsiloxane) grafts, thus influencing their length. The graft copolymers are strong surfactants. Separation from their mixture with homo-polymers by a repeated extraction of homopolymers with a solvent is difficult and sometimes impossible.
    Additional Material: 4 Ill.
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    Etude par 13C NMR d'alcanes lourds mono- et diramifiés. Modèles de polyoléfines (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 569-583 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 13C NMR spectra were obtained for a series of branched, heavy alkanes at 37°C and 100°C, which provide a model set for describing the branched sequences in low density polyethylene (LDPE) and copolymers of α-olefines. In addition, they provide a model set for revising the empirical Grant-Paul and Lindeman-Adams additive coefficients and corrective terms for pre-dicting 13C chemical shifts of alkanes. The resulting revised parameters (for 37°C and 100°C) produce more accurate predictions of 13C NMR spectra for branched alkanes and it is noted that some corrective terms can be temperature-sensitive.
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    Determination of poly(ethylene oxide) crystallinity by inverse gas chromatography (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 605-611 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Specific retention volumes Vg for acetone, 1-propanol, ethyl acetate, hexane, and tetrahydrofuran were obtained by inverse gas chromatography using poly(ethylene oxide) as stationary phase. Measurements were done at different flow rates, different injected sample amounts, and with three columns of different packing. Retention volumes were measured above and below the melting temperature of the polymer. The shape of the flow diagram and the variation of retention time tr with the sample amount depend on the temperature, flow rate, and the nature of the probe. Moreover, and due to the polymer polarity, the retention volume is a linear function of the column coating. All these factors must be controlled in order to obtain an accurate value of Vg which allows the determination of the crystallinity of the stationary phase. Above Tm, Vg is independent of flow, packing, and amount of the injected sample.
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    Polymer conformation and NMR chemical shifts, 8Part 7: cf.7.. Monomer- and stereo-sequence dependences of 13C NMR spectrum of poly(methyl acrylate-co-styrene) (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 821-827 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The 13C NMR spectra of poly(methyl acrylate-co-styrene) are interpreted by a theoretical procedure which consists of conformational analysis of the random copolymer chain and shielding calculation. The conformational probabilities of the diad sequences constituting poly(methyl acrylate-co-styrene) are calculated by a matrix method which is conducted by the statistical mechanics of polymer chains. All the elements of the matrices are determined by the force field method. As significant shielding factors for 13C nuclei, paramagnetic, diamagnetic, and anisotropic terms are taken into account. The calculation is used to assign the observed split peaks for the carbonyl carbon and methoxyl carbon in the copolymer. A good agreement between calculation and observation of the peak splittings due to the distribution of the monomer sequence as well as that of the stereo sequence was obtained by considering the feasibility of rotational isomerization at the side chain ester group in two successive MA units.
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  • 159
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    Crystallinity of methylene-oxyethylene-methylene triblock oligomers derived from pentadeca(ethylene glycol) (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 861-877 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Block oligomers of the general formula CH3(CH2)nO[CH2CH2O]15(CH2)nCH3 where n + 1 = nc = 1 to 18 and 21 have been prepared. Both the oxyethylene and the methylene blocks are monodisperse. Examination of their crystallinity (by differential scanning calorimetry (DSC); X-ray scattering; IR, Raman, and 1H NMR spectroscopy) shows two important structures I and II.I: 3 ≤ nc ≤ 6: oxyethylene blocks crystalline, methylene blocks non-crystalline;II: 13 ≤ nc ≤ 18: oxyethylene and methylene blocks crystalline.Samples with nc = 1 or 2 crystallise essentially as poly(oxyethylene). Samples with 7 ≤ nc ≤ 12 are intermediate in structure between I and II. Structure II has 7/2 helical oxyethylene blocks in high density crystalline layers, with a structure closely related to that of monoclinic poly(oxyethylene), and planar zig-zag methylene blocks in low density crystalline layers. The oxyethylene helices are normal to the lamella end-planes, or almost so, and the methylene planar zig-zags are tilted. The enthalpies of fusion of the type II block oligomers show an even-odd effect. There is evidence of chain folding in the block oligomer with nc = 21.
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    Copolymerization of vinyl chloride and methyl acrylate catalyzed by ethylaluminium compounds (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 913-924 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The copolymerization of vinyl chloride (VC) and methyl acrylate (MA) in the presence of ethylaluminium compounds (C2H5AlCl2, (C2H5)2AlCl, and (C2H5)3Al) at low ethylaluminium compound (EAC)/MA mole ratios was investigated. An alternating copolymer was produced in this reaction when an excess of VC in the initial monomer feed was used. The addition of dibenzoyl peroxide (BPO) to the systems containing EAC resulted in an increase of the alternating copolymer yield. In polymerization systems containing EAC resulted in an increase of the alternating copolymer yield. In polymerization systems containing EAC combined with VOCl3 an enhancement of the alternating copolymer yield and formation of VC-rich copolymers were observed. In the polymerization system with (C2H5)3Al—VOCl3 a VC-rich copolymer was the main product. It was concluded that VC-rich copolymers are formed in the random radical copolymerization which occurs when most of EAC is complexed by the alternating copolymer chain. The structure of alternating and VC-rich copolymers was studied in detail by means of 13C NMR spectroscopy.
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    Kinetics of the nitrogen dioxide initiated polymerization of acrylic acid (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 955-959 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Acrylic acid (AA) was polymerized with NO2 in tetrahydrofuran (THF) and in 1,4-dioxane. The effects of monomer and initiator concentration and of temperature on polymer conversion, initial rate of polymerization, and molecular weight were studied. The overall activation energy of polymerization was found to be 16,3 kcal mol-1 (68,23 kJ · mol-1) and 15,54 kcal · mol-1 (65,05 kJ · mol-1) in THF and in 1,4-dioxane, respectively. High molecular weight polymers (M ca. 105) were obtained. The polymerization appears to be initiated by free radicals.
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  • 162
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    Caractérisation physico-chimique d'un polymère phosphore (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 991-1003 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A mixture, probably composed of a poly(chlorotrimethylsilyloxy)phosphazene and a compound with the general formula H2Cl2NOP (inactive toward THF) was used to initiate the polymerization of tetrahydrofuran. The resulting polymer (PTHFP) contains phosphorus associated with nitrogen, as assessed by IR, 31P and 1H NMR spectroscopy. The thermal stability of PTHFP, observed by thermogravimetry, was found to be much higher than that of polytetrahydrofuran (PTHF). At the end of its decomposition a solid residue remains, which was identified as a poly(phosphazene oxide) (PNO)n. The combustion behaviour is also modified in that the cool flame combustion area is raised up in the pressure-temperature coordinates. In addition, the disappearance of the so-called secondary cool flame (SCF) phenomenon is in favour of the heterogeneous action of the phosphorus derivatives during the inhibition of combustion at higher temperatures. The thermochemical analysis (DSC-Rheovibron) shows the existence of a semi-cristalline structure proportional to the amount of phosphorus introduced into the PTHF chain. The glass transition temperature of PTHFP was found to be slightly higher than that of PTHF without any apparent relation to their structures. The same conclusion arises from the viscoelastic measurements.
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    Behaviour of poly(N-vinylcarbazole) in 1,3-dichlorobenzene/methanol mixtures (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1035-1042 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The behaviour of poly(N-vinylcarbazole) in a mixture of 1,3-dichlorobenzene and methanol (solvent/non-solvent system) is studied. The non-solvent, methanol, is more strongly adsorbed than 1,3-dichlorobenzene as judged from changes in the unperturbed dimensions and intrinsic viscosity. Therefore the Mark-Houwink-Sakurada constant and the flexibility parameter decrease with increasing methanol contents. A relation between the preferential adsorption parameter and the segment density is given.
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    Active centre determination in ziegler-natta polymerization. An examination of the allene inhibition method (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1469-1478 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A study of the adsorption of allene on VCl3, TiCl3 Type 1.1, and TiCl3 Type H catalysts has been made. In the absence of cocatalyst, allene adsorption is observed and in the case of the TiCl3 Type 1.1 catalyst rapid oligomerization of allene occurs. Activation with Al(C2H5)3 leads to a slow consumption of allene with VCl3 and TiCl3 Type H, but shows no distinct change for the TiCl3 Type 1.1 catalyst. The amount of “adsorbed” allene is generally higher than the number of active sites and this is attributed to adsorption on sites which are inactive in polymerization and to consumption of allene through side-reactions.
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    Thermoelastic behaviour of segmented polyurethane elastomers (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1519-1527 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Thermoelastic (stress-temperature) measurements in elongation were conducted on polyurethane elastomers of different chemical structure. Values of the temperature coefficient d In \documentclass{article}\pagestyle{empty}\begin{document}$ \overline {r_0^2 } /{\rm d}T $\end{document} of the unperturbed dimensions of the network chains and the fraction fe/f of the stress, which is due to energetic effects, were calculated from measurements of unswollen samples. The elastomers displayed some deviations in the thermoelastic behaviour from that predicted by the theory. It is found that the extent of those deviations depends on the chemical structure and the contents of stiff and soft segments in the polyurethane rubbers studied.
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    Cationic homopolymerization of 1,1′-diisopropenylferrocene (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1837-1848 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: 1,1′-Diisopropenylferrocene (1a) was homopolymerized using trifluoroacetic acid or boron trifluoride etherate as initiators, with excellent yields (〉90%) of polymer (8100 〈 M̄n 〈 14700). Spectroscopic evidence established an initial protonation of 1a to give a tertiary monocarbenium ion (3) which does not readily undergo intramolecular cyclization (into 4). Analysis of isolated homopolymers by 1H and 13C NMR spectroscopy revealed significant residual unsaturation, consistent with facile chain transfer. Adventitious oxidation occurred during workup to give a mixed valence (Fe(II)/Fe(III)) polymer which could be distinguished spectroscopically from the unoxidized polymer.
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    Propriétés physicochimiques d'une série de polystyrènes deutériés en solution dans le tétrahydrofuranne (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1877-1884 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The physicochemical properties of a series of deuterated polystyrenes were investigated in tetrahydrofuran by viscosity, light scattering (LS), on line LS-GPC, and size exclusion chromatography (GPC). The viscosity laws and unperturbed dimensions of deuterated (PSD) and “hydrogenated” (PSH) polystyrene were compared. There are small but distinct differences in the solution behaviour of PSH and PSD. Some optical properties of partially D-labelled polystyrenes were investigated.
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    Lamellar crystalline structure of star-shaped block copolymers with an amorphous block of polystyrene and two crystallizable blocks of poly(ethylene oxide) (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1907-1917 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Star-shaped block copolymers S(EO)2 with two poly(ethylene oxide) chains (PEO) linked to the same end of a polystyrene chain (PS) exhibit a lamellar liquid crystalline structure, with crystallized and folded PEO chains, in the dry state as well as in the presence of a preferential solvent of the PS block at temperatures below about 50°C. Refolding of the PEO chains was studied in terms of the PS swelling degree and in terms of the PEO content of the copolymers. A difference in length of the PEO chains was suggested, probably resulting from the different nature of the sites that initiate the EO chain polymerization. To investigate the effect of the number of the PEO chains fixed to the PS block, two block copolymers S(EO)2 and SEO of the same relative molecular mass and composition were studied.
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    Wide-angle X-ray scattering for swollen and glassy poly(2-hydroxyethyl methacrylate) (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1937-1943 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The wide angle X-ray scattering from glassy poly(2-hydroxyethyl methacrylate) (1) is presented together with that obtained from oriented and swollen samples. The scattering is compared with that previously reported for poly(methyl methacrylate) (PMMA) and the structure discussed in relation to this polymer. The chain conformation is similar to that of PMMA, although some measure of molecular interlocking appears to reduce the main interchain peak while correlated regions of inaccessible free volume between the substantial side groups are held responsible for the main peak at s = 1,25 Å-1.
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    Molecular weight distributions of poly(methyl methacrylate) produced at high viscosities (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1623-1643 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The molecular weight distribution of poly(methyl methacrylate), which is produced by the free-radical polymerisation of methyl methacrylate, is influenced by the presence of poly(methyl methacrylate) which is dissolved in the monomer prior to the polymerisation. An experimental technique has been devised which permits a distinction to be made between polymer which is present at the start of the reaction and the polymer which is formed by the reaction. Mathematical analyses of alternative reaction schemes have been made. These predicted changes that would occur in the molecular weight distribution of the new polymer when the solution viscosity increased. Comparison with experimental measurements of molecular weights makes possible the distinction between the alternative reaction schemes. The results are compatible with a reaction mechanism in which the mobilities of the growing radicals are not influenced equally by the solution viscosity. The results are not those which would be expected by the simple inclusion of primary radical termination in the reaction scheme. In some cases, analysis by gel permeation chromatography showed that the molecular weight distribution of the poly(methyl methacrylate) formed by the reaction is bimodal. This is consistent with predictions from the mathematical analysis.
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    Copolymere aus methacrylsäure und dimethacryloylimid und die abhängigkeit ihrer NMR-spektren vom neutralisationsgradHerrn Prof. Dr. H.-J. cantow zu seinem 60. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1705-1726 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The chemical structure of syndiotactic methacrylic acid-dimethacryloylimide (MAA-MAI) copolymers is studied by the NMR-spectra of products obtained by polymeranalogous reactions and from MAA-MAI copolymers prepared according to a different route. The kinetics of formation of the imide rings is compared with kinetic equations, confirming thereby the random formation of rings along the chain. 13C NMR spectra of MAA-MAI copolymers depend on the degree of neutralization, α, in aqueous solution and show large changes for the carbonyl resonance region. Resolution into triads is found in organic solvents, whereas in aqueous solutions there is splitting into pentads on going from α = 0 to α = 1. The pentad assignment is made by observing the movement of the peaks with changing α and by comparison with pentad probabilities derived by a Monte-Carlo simulation. The great changes in the chemical shift are caused to a large extent by a change in the charge of the carboxyl groups. Discontinuous changes in charge, conformation, and solvation are not found.
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    Synthesis and characterization of some aliphatic polyamides containing 4,4′-azodiphenylene units (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2225-2230 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyamides containing azo groups were prepared by the phosphorylation method from 4,4′-diaminoazobenzene and malonic, succinic, glutaric, adipic, azelaic, sebacic, or chlorosuccinic acid. The polymers were characterized by their viscosity and solubility, and by UV-visible and IR spectroscopy, TG, and DTA.
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    End groups in poly(vinyl chloride) and their influence on the thermal stability (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2261-2273 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: End groups in a low molecular weight fraction of a commercial suspension poly(vinylchloride) were analysed by means of 1H NMR and IR spectroscopy and by size exclusion chromatography. The following groups were identified and quantified: ethoxycarbonyloxy (1), 1,2-dichloroethyl (2), trans- and cis-4-chloro-2-butenyl (3 and 4), 2-chloroethyl (5), and 2-chloroethylidene (6). The influence of these groups on the degradation at 180°C was determined.
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    Study of photopolymers, 18Part 17: cf.16.. Synthesis and photochemical reaction of novel polymers with pendant photosensitive and photosensitizing groups (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2297-2312 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Self-sensitized photosensitive polymers with pendant photosensitive and photosensitizing groups were prepared by reaction of polystyrene containing pendant chloromethyl and photosensitizing groups, with the potassium salts of photosensitive compounds such as cinnamic acid, crotonic acid, or 2-cyano-3-(α-styryl)acrylic acid in DMF using tetrabutylammonium bromide as phase transfer catalyst. The photochemical reactivity and the practical photosensitivity of the resulting polymers were measured by IR spectrometry and by the gray-scale method, respectively. Pendant 4-nitro-1-naphthyloxy and 4-nitrophenoxy groups in the polymers show the highest photosensitizing activity for pendant cinnamoyl groups. The photochemical reactivity and the sensitivity of these polymers are affected by the content of photosensitizing units in the polymer skeleton, the glass transition temperature of the polymers, however, is not influenced. Pendant 2-benzoylbenzoyl groups act as excellent photosensitizers for pendant crotonoyl groups, however, the photochemical reactivity of this polymer was found to be lower than that of the polymer with pendant cinnamoyl and suitable photosensitizing groups. Pendant 2-cyano-3-(α-styryl)acryloyl groups in the polymer, which exhibit high photochemical activity, are also sensitized by pendant methyleosin moieties.
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    Decay of the spin echo in a pulsed magnetic field gradient NMRDedicated to Prof. O. Wichterle on the occassion of his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2377-2390 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The additional attenuation of the spin echo of a pulsed magnetic field gradient NMR caused by the diffusion of the spins carrying molecules is calculated for a time dependent diffusion coefficient. The cases of a Constant D0, of an exponential decay with time, and an abrupt drop from D0 to zero at time t0 are considered. In all cases the time dependence of the experimentally observed attenuation is less steep than that of D. The time scale, however, Changes very little. The calculation was based on the consideration that the diffusion transports the precessing spins to a location with a different Larmor frequency so that a complete reversal after the 180° pulse is not possible any more. Hence, any deviation from a straight line in a plot of the excess attenuation versus δ2(1 - δ/3Δ) may by interpreted in terms of a time dependence of the diffusion coefficient.
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    Photostability of trityl salts with different anions under argon (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2231-2239 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The visible light-induced photolysis of trityl salts with anions such as PF⊖6, FeCl⊖4, BF⊖4 or AsF⊖6 was investigated in an inert atmosphere. The rates of decoloration of the dichloroethane solutions of the trityl cation (10-5 mol · 1-1) in the presence of different anions are compared. The results indicate that the order of photostability is (C6H5)3 C⊕PF⊖6. 〉 (C6H5)3 C⊕FeCl⊖4 ≥ (C6H5)3 C⊕ BF⊖4 〉 (C6H5)3 C⊕ AsF⊖6 ≥ (C6H5)3 C⊕SbCl⊖6. A comparison of the overall rate of photolysis of (C6H5)3 C⊕SbCl⊖6 in argon and oxygen suggests that the photo-induced reactions are both of radical and ionic type. The composition of the reaction mixtures after photolysis was determined.
    Additional Material: 4 Ill.
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  • 177
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    Furan and pyran derivatives as modifiers of propylene polymerization catalysts (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2275-2284 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Studies of various tetrahydrofuran and tetrahydropyran derivatives as modifiers of Zieglertype propylene polymerization catalysts are reported. Among methyl derivatives, ethers containing two methyl substituents on carbon atoms adjacent to the etheric oxygen provied the best activity-stereospecificity combinations (e.g. 2,5-dimethyltetrahydrofuran (1c) and 2,2,4,4-tetramethyltetrahydrofuran) (4). Significantly better stereospecificity with some loss in activity is realized when bulkier ethers such as isochroman (5) or 2-(tetrahydrofurfuryloxy)tetrahydropyran (6) are used. On the other hand, combination of one of the preceding ethers with a second modifier (bis(tributyltin) sulfide, tributyl phosphite, or triethyl thiosphosphate) results in catalyst systems characterized by very attractive activity-stereospecificity combinations. Systems of this type, containing 1c or 4, exhibit higher activity and about equal or better stereospecificity than the systems modified only with the second modifier; whereas 5 and 6 depress somewhat the activity of the latter systems but provide substantially improved stereospecificity. The steric and electronic effects introduced by the ether modifiers in the single and binary modifier systems investigated are discussed.
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  • 178
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    Small angle neutron scattering studies of poly(ethylene oxide) in the meltThe neutron scattering experiments were carried out at the ILL, Grenoble, France. To Prof. Dr. H.-J. Cantow with best wishes on his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2325-2334 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The neutron scattering from mixtures of deuterated and undeuterated poly(ethylene oxide), (D-PEO, H-PEO), in the small angle and intermediate angle region has been measured in the melt. We found no indications of a molecular segregation. The value of molecular weight evaluated agreed with that obtained by other methods. For a sample with a molar mass of 120000 g/mol the radius of gyration 〈rw2〉1/2 was found to be 13,6 nm, which corresponds to a characteristic ratio of C = 6,9. The form factor of a single chain can be described by the Debye equation for a random coil with the same unperturbed dimensions. Our results are compared with rotational isomeric state calculations and measurements in solvents.
    Additional Material: 5 Ill.
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  • 179
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    Optically active vinyl polymers, 24Part 23: cf. P. Pino, A. Allio, A. Klaus, Helv. Chim. Acta, in press.. Copolymers of 4-methyl-1-penten-3-one and (S)-4-methyl-1-hexen-3-oneDedicated to Prof. Dr. H.-J. Cantow on the occasion of his 60th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2335-2346 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Copolymers of 4-methyl-1-penten-3-one and (S)-4-methyl-1-hexen-3-one have been synthesized by radical- and anionic initiation and their composition has been determined by 13C NMR and 1H NMR spectroscopy. A comparison between the composition of the initial monomer mixture, F, and the composition of the monomeric units in the copolymers, f, indicates Bernoullian copolymerization statistics with both types of initiators. The intrinsic viscosity, the number-average molecular weight, and the second virial coefficient of the osmotic pressure were measured and an unusually high increase of the intrinsic viscosity with f was noticed. The results can be interpreted by assuming a strong increase in the unperturbed chain dimensions with increasing content of optically active monomeric units in the copolymer.
    Additional Material: 3 Ill.
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  • 180
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    Resines époxydes, 1. Mécanisme de polycondensation entre le bis[(époxy-2,3 propoxy)-4 phényl]-2,2 propane et la m-phénylénediamine par 13C NMR (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2477-2485 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Curing of 2,2-bis[4-(2,3-epoxypropoxy)phenyl]propane (diglycidyl ether of bisphenol A) (1) with m-phenylenediamine (2) was performed in a variable temperature probe of a 13C FT NMR spectrometer (62,89 MHz). The formation of an initial adduct was directly observed and the progress of polymerisation was followed by recording the 13C NMR spectra at time intervals. Unreacted epoxide carbon atoms were detected in one sample as well as in a sample of 1 cured by a standard procedure.
    Additional Material: 6 Ill.
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  • 181
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    Kristallisation und schmelzverhalten von fraktionen verzweigten polyethylens, 1. Darstellung und charakterisierung der fraktionen (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2553-2561 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A branched polyethylene with broad molecular weight distribution was separated into a series of fractions by fractional precipitation from dilute solution. The fractions were characterized by viscometric and density measurements, IR-spectroscopy and calorimetry. The methyl group content and the density turned out as largely constant. Molecular weight effects show up in the melting behaviour. The main range of melting and the end of the melting curve shift to lower temperatures with decreasing molecular weight. Compared to the overall extension of the melting range these shifts are small. One has to conclude that polydispersity gives only a minor contribution to the broadening of the melting range, partial melting being mainly caused by the branches.
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  • 182
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    Chelation ion-exchange properties of salicylic acid/thiourea/trioxane terpolymers (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 717-723 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Terpolymers prepared by condensation of salicylic acid and thiourea with trioxane in presence of acid catalysts, proved to be selective chelating ion-exchange resins for certain metals. Chelation ion-exchange properties of these terpolymers were studied for Cu2+, Ni2+, Fe3+, Mn2+, Co2+, Zn2+, and UO22+ ions. A batch equilibration method was employed in the study of the selectivity of metal ion uptake involving the measurement of distribution of a given metal ion between the polymer sample and a solution containing the metal ion. The study was carried out over a wide pH range and in media of various ionic strengths. The terpolymers showed a higher selectivity for Cu2+, Fe3+, and UO22+ ions than for Mn2+, Co2+, and Zn2+ ions.
    Additional Material: 3 Tab.
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  • 183
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    Polymerisationsauslösung mit substituierten ethanen, 6Teil 5: cf.3.. Polymerisation von methylmethacrylat mit verschiedenen tetraphenylethanen (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 745-754 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The polymerization of methyl methacrylate (MMA) was initiated with 1,1,2,2-tetraphenyl-1,2-diphenoxyethane (TPPA), 1,1,2,2-tetraphenyl-1,2-bis(trimethylsiloxy)ethane (TPSA), and 1,1,2,2-tetraphenyl-1,2-dicyanoethane (TPCA). The polymerization with these initiators is characterised by three steps: in the first period oligomers from MMA and initiator radicals are formed by primary radical termination. These telechelics are effective initiators for the further free radical polymerization of MMA. After consumption of the initiator radicals with increasing conversion a normal polymerization occurs.
    Additional Material: 11 Ill.
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  • 184
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    Synthèse et caractérisation de réticulats-modèle de polyisoprène (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 803-810 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyisoprene model-networks were synthesized by an “endlinking” process: an efficient bifunctional initiator, developped recently, was used to polymerize isoprene to a bifunctional “living” precursor polymer. The living sites were subsequently used to initiate the polymerization of a small amount of divinylbenzene, whereby a model network is formed, the elastic chains of which are of known length and low polydispersity. Equilibrium swelling data and stretching moduli were measured. Unfortunately no reproducible results could be obtained on unswollen networks. Qualitative experience was obtained on the degree of association of lithium organic sites in benzene solution: the value of 2 is to be considered as plausible.
    Additional Material: 3 Ill.
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  • 185
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    Solution properties of ultrahigh molecular weight polymers, 1. Methyl methacrylate-styrene 50:50 random copolymers (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 829-835 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The paper is concerned with light scattering studies on solutions of ultrahigh molecular weight random copolymers of methyl methacrylate and styrene (50:50 mol/mol). The dependence of the radius of gyration and of the second virial coefficient on the weight-average molecular weight of the copolymers was established. The value of the steric factor of the copolymer compared to those of the corresponding homopolymers confirms the random character of the copolymer chain. The interpenetration function Ψ(Z), calculated on the basis of different theoretical approximations, is discussed for the expansion factor αs3 〉 7.
    Additional Material: 3 Ill.
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  • 186
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    Synthesis and investigation of the properties of cardo-copolyimides with different microstructure (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 893-893 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840422
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  • 187
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    Synthèses de polysiloxanes organofonctionnels, 4Partie 3: cf.12.. Les poly[(hydroxyméthyl)méthylsiloxane]s homogénes et hétérogènes (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1807-1816 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Transformations of oxy(halomethyl)methylsilanediyle units or oxy(acetoxymethyl)methyl-silanediyle units into oxy(hydroxymethyl)methylsilanediyle units in homogeneous and heterogeneous polysiloxanes were investigated. Si-C-cleavage and Si—O—Si-rearrangement were studied on disiloxanes and oligosiloxanes used as models of the corresponding polymers. Methanolysis of poly[(acetoxymethyl)methylsiloxane]s and their copolymers catalysed by p-toluenesulfonic acid was applied to obtain poly[(hydroxymethyl)methylsiloxane]s and their copolymers.
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  • 188
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    Specific functionalization of polyoxirane by amino, carboxyl, sulfo, and halogeno end groups (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1849-1859 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polyoxiranes with amino, carboxyl, or halogeno end groups were prepared by polymerization of oxirane with either anionic initiators substituted with functional or protected functional groups, or by reaction of functional deactivating reagents with anionically prepared polyoxiranes. For the protection of primary amino groups they were transformed into the corresponding cyclic imido derivatives. The deactivation of polyoxirane with potassium oxido end groups by bis(halogenomethyl)benzenes was studied with the three isomers.
    Additional Material: 4 Ill.
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  • 189
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    Studies on the adiabatic polymerisation of acrylamideThe studies reported here formed part of a paper given at Achema 82 Chemical Engineering Congress, Frankfurt-am-Main. (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1885-1892 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Kinetic parameters, obtained isothermally, have been used in the quantitative description of the polymerisation of acrylamide under virtually adiabatic conditions. The equations which have been derived relate the temperature rise on reaction to the decrease in reactant concentration during the course of reaction, taking account of the various energies of activation and frequency factors involved, whose values may be chosen as required. The approach used has been to find the value of the overall activation energy which gives the best agreement between theoretical and experimental temperature-time plots. Good agreement has been obtained between these when a value of 74,5 ± 0,9 kJ · mol-1 was chosen for the overall activation energy for the persulfate-initiated polymerisation of acrylamide using a wide range of initiator and monomer concentrations. This gives a value of 135,5 kJ · mol-1 for the activation energy for the thermal decomposition of the persulfate ion, which is in good agreement with the literature. Interesting implications are discussed in the context of the nature of the product formed during the course of the polymerisation.
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  • 190
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    Postirradiation polymerization and ESR studies of γ-irradiated N-tert-butylacrylamide (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1919-1926 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Postirradiation polymerization of γ-irradiated N-tert-butylacrylamide was studied at 80, 85, 90, and 100°C, and the activation energy was found to be 183 kJ · mol-1. By ESR spectroscopy, the half-life for the second order decay of the irradiated monomer was found to be 13,8 h at 25°C with a decay rate constant of 4,5 · 106 g · mol-1 · h-1. The effect of oxygen and sulfur dioxide on γ-irradiated N-tert-butylacrylamide was also studied. It was observed that oxygen reacts with N-tert-butylacrylamide free radicals resulting in a characteristic peroxyl radical spectrum. The signal decays rapidly and disappears in about 100 h. The decay was found to be of second order with a rate constant of 1,3 · 107 g · mol-1 · h-1 and a half-life of 3,8 h at 25°C. In contrast to the situation with atmospheric oxygen, an appreciable fraction of the free radicals does not react rapidly with sulfur dioxide. The changes in the ESR spectra indicate that at least a large fraction of the original N-tert-butylacrylamide radicals, generated in the irradiated sample, react with sulfur dioxide rapidly to give sulfonyl radicals. Their decay is second order with a rate constant of 4,5 · 106 g · mol-1 · h-1 and a half-life of 8,3 h.
    Additional Material: 8 Ill.
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  • 191
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    Acidolytic polymerization of N-methyldodecanelactamDedicated to Professor Dr. O. Wichterle on the occasion of his seventieth birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 1957-1965 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The polymerization rate of 1-methylazacyclotridecan-2-one (N-methyldodecanelactam) (1) initiated with dodecanoic acid (2) can be described within the whole range of conversions in terms of the simple relation In ([1]0/[1]) = k[2]0t, in spite of the complexity of the overall reaction scheme. The rate constants (k) determined for 240, 260, and 280°C are 0,32, 1,21, and 3,4 kg · mol-1 h-1, respectively, and the constants of the Arrhenius equation are A = 6,6 · 1013kg · mol-1 h-1, E = 140 kJ · mol-1. The resulting poly(N-methyldodecaneamide) (3) is a semicrystalline polymer (m.p. 65°C), soluble in polar organic solvents. The following constants of the Mark-Houwink equation were determined for solutions of this polyamide: for 5000 〈 M̄w 〈 150 000 g · mol-1 at 25°C in THF (2-propanol), K = 0,124 (0,161) cm3 · g-1, a = 0,59 (0,56); for 5 000 〈 M̄w 〈 80 000 g · mol-1 at ⊖-temperature = 30,5°C in 1,4-dioxane, K = 0,215 cm3 · g-1, a = 0,50. Analyses of molar masses, both theoretical and experimental (light-scattering, GPC, osmometry, end groups), indicate that at the polymerization temperature of 280°C side reactions already take place, reflected in random cleavage and in branching of chains.
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    Association of two-block copolymer polystyrene-block-poly(2-vinylpyridine) in tolueneDedicated to Prof. O. Wichterle on the occasion of his 70th birthday (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 2049-2059 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The association of two-block copolymers polystyrene-block-poly(2-vinylpyridine) has been studied in toluene (a solvent selective for polystyrene) by osmometry, viscometry, and light scattering. Polystyrene-block-poly(2-vinylpyridine) in toluene forms polymolecular micelles having a poly(2-vinylpyridine) core and a polystyrene shell, and micellization conforms to the model of closed association. The phenomenon of so-called anomalous micellization has been observed within a certain temperature interval where unusually large particles are formed.
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  • 193
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    Unvernetzte epoxid-amin-additionspolymere, 65. Mitteilung: cf.. DSC-untersuchungen zur kinetik der stufenadditionspolymerisation von 2,2-bis[4-(2,3-epoxypropoxy) phenyl] propan mit N,N′-dibenzylethylendiamin und benzylamin (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 113-121 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The kinetics of the linear step-growth addition polymerization of equimolar amounts of the diglycidyl ether of bisphenol-A 2,2-bis[4-(2,3-epoxypropoxy)phenyl]propane (1) with N,N′-dibenzylethylenediamine (2) and with benzylamine (4), respectively, is studied by means of differential scanning calorimetry (DSC). For conversions α ≤ 0,90 the experimental results of the isothermic measurements are in excellent agreement with values calculated from the rate equation dα/dt = (k1 + k2 αm) (1 - α)n with m + n = 2,5 (m ≍ 1,0, n ≍ 1,5). The first term of this rate equation takes into account both the catalytic and autocatalytic character of the addition polymerization while the exponent n ≍ 1,5 in the second term shows that the effective concentration of one of the addition components is given by the square root of its concentration.
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  • 194
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    Role of hydrophobic interaction in the enantioselective solvolyses of amino acid p-nitrophenyl esters by optically active imidazole-containing polymers (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 147-152 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Solvolytic reactions of N-benzyloxycarbonyl-D-phenylalanine p-nitrophenyl ester and N-benzyloxycarbonyl-L-phenylalanine p-nitrophenyl ester by optically active imidazole-containing polymers were performed at different temperatures and in aq. ethanol of different water contents. The catalyst polymers employed were homopolymers of N-methacryloyl-L-histidine (1a) and N-methacryloyl-L-histidine methyl ester (1b), as well as copolymers of 1a with dodecyl methacrylate (DMA) and 1b with DMA. In 30 vol. -% aqueous ethanol at pH 7,02 the homopolymers did not show any enantioselective catalysis. However, the copolymers did exhibit enantioselective catalysis, viz., kcat(L)/kcat(D) = 1,25 for poly (1b-co-DMA) containing 5,7 mol-% of DMA. As the reaction temperature was lowered, the reaction rate increased and the enantioselectivity was enhanced (kcat(L)/kcat(D) = 1,67 for poly (1b-co-DMA) at 10°C). When the ethanol content was decreased, enhanced reaction rates and enantioselectivity (kcat(L)/kcat(D) = 1,65 for poly (1 b-co-DMA) in 20 vol.-% aqueous ethanol) were observed. From these results it is concluded that hydrophobic interaction plays an important role in the enantioselective catalysis of optically active imidazole-containing polymers.
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    Zur polymerisation von methylmethacrylat bis zu hohen umsätzen: Experimentelle untersuchungen zur theorie des trommsdorff-effektes nach cardenas und o'driscollHerrn Professor Dr. Dres. h. c. G. V. Schulz mit den besten Wünschen zum 75. Geburtstag gewidmet (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 175-191 
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    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The kinetic model given by Cardenas and O'Driscoll, which describes the bulk polymerization of methyl methacrylate (MMA) in the region of the gel effect by the concept of chain entanglements, is extended to the region of the glass effect in accordance with a proposition made by Marten and Hamielec based on the free volume theory. Equations for the calculation of the instantaneous and cumulative molecular weight distributions are derived, too. Dilatometric measurements over the entire conversion range were performed at various temperatures and with three different initiators. For each series of measurements the three adjustable parameters of the extended model were fitted to the time-conversion data. Contrary to the assumptions, it was then found that at least one of the parameters of the model of Cardenas and O'Driscoll (α0) depends both on the concentration and the type of the initiator. The calculated molecular weight distributions are much broader than the experimental ones. Thus the model of Cardenas and O'Driscoll at its present state does not seem to describe adequately the real polymerization behavior of MMA.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840118
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  • 196
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    Study of step-growth polymerizations using epoxy-carboxy reaction, 2Part 1: cf.1.. Study of the epoxy-carboxy reaction on models in nitrobenzene (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 335-341 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: In the first part of this series devoted to epoxy-carboxy polycondensation, we showed that the overall mechanism of the amine catalyzed epoxy-carboxy reaction is complex. The present article studies the reaction of benzoic acid with 1-phenoxy-2,3-epoxypropane carried out in nitrobenzene and in the presence of N,N-dimethyldodecylamine as catalyst. In contrast to the results obtained in low polar solvents, where two equivalent reactions take place, the studies carried out in nitrobenzene show that, in this solvent, one of these two reactions is largely predominant. Its rate equation is: υ = k [epoxy][amine]. However, in the last steps of the reaction (conversion above 75% ), the system behaves as in low polar solvents. These results were obtained from studies carried out under stoichiometric and non-stoichiometric conditions. The overall rate constant depends only very slightly on the stoichiometric balance. This is in agreement with a major contribution of one of two competitive reactions.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840210
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  • 197
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    Initiation processes in polymerizations of alkyl cyanoacrylates by tertiary amines: Inhibition by strong acids (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 383-394 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Polymerizations of butyl and ethyl cyanoacrylates, in the solvent THF, initiated by pyridine and other tertiary amines, are inhibited by strong acids, which cause well-defined inhibition periods (ti) proportional to the concentration of acid added, but irrespective of its nature. The temperature and monomer concentration dependence of ti indicate that chain-initiation is a composite sequence involving two or three successive additions of monomer. A detailed theory is proposed and used to evaluate the composite initiation rate constants over the temperature range 20°C to -80°C. The influence of steric factors on the initiation by pyridine, picolines and lutidine is exemplified and discussed.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840214
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  • 198
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    Asymmetric induction in the copolymerization of (-)-3-(β-styryloxy)menthane with styrene (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 455-462 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Asymmetric induction in the copolymerization of (-)-3-(β-styryloxy)menthane (1) with styrene was investigated. The copolymers obtained in the presence of BF3 · OEt2 are optically active. The absolute value of the specific rotation of the copolymers was found to be higher than that of the homopolymeric mixture, whatever the composition. After ether cleavage reaction of the copolymers, the products are still optically active. The result suggests that an asymmetric induction takes place in the polymer main chain.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840301
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  • 199
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    Study of step-growth polymerizations using epoxy-carboxy reaction, 3Part 2: cf. 2.. General analysis of the results obtained on models in various solvents (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 343-355 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: A global analysis of the kinetic results relating to a model reaction of epoxy-carboxy polycondensation is reported. The model is the reaction of benzoic acid with 1-phenoxy-2,3-epoxypropane carried out in the presence of N,N-dimethyldodecylamine as catalyst. The hypothesis concerning the contribution of two competitive ractions as suggested in the two preceding parts of this series is subjected to a mathematical treatement. This allowed the determination of the rate constants of each reaction. All the kinetic characteristics obtained in a broad range of experimental conditions fit the reaction scheme, which is described in detail. Exceptions are found for borderline cases. The rate constants of the reaction of the classical dependence on dielectric constant and temperature. Activation parameters of each reaction are reported.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840211
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  • 200
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    Study of step-growth polymerizations using epoxy-carboxy reaction, 4Part 3: cf. 3.. Study of the epoxy-carboxy reaction carried out in the melt on high molecular weight models (1983)
    New York : Wiley-Blackwell
    Die Makromolekulare Chemie 184 (1983), S. 357-369 
    Details
    ISSN: 0025-116X
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Epoxy-Carboxy polycondensation is studied in the melt by use of the octadecanoic acid/1-dodecyloxy-2,3-epoxypropane reaction as a model. The catalyst is N,N-dimethyldodecylamine. The results obtained from these high molecular weight models show that, as for the studies performed in a solvent, two main reactions take place. The experiments are carried out under stoichiometric and non-stoichiometric conditions. It appers that, due to the strong interaction between epoxy compound and amine, a polymerization of oxirane takes place to a small extent, being a side reaction of the system. As a consequence, epoxy groups are consumed more rapidly than acid groups. Nevertheless, an approximation allowed the determination of the rate constants relative to the two main reactions. Activation parameters of these reactions are reported.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/macp.1983.021840212
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