ALBERT

All Library Books, journals and Electronic Records Telegrafenberg

X
feed icon rss

Your email was sent successfully. Check your inbox.

An error occurred while sending the email. Please try again.

Proceed reservation?

Export
Filter
  • structural units  (2)
  • 1,1-dimethylpiperidinium  (1)
  • 13C NMR  (1)
  • 1
    Electronic Resource
    Electronic Resource
    29Si NMR investigation of condensation reactions of diphenylsilanediol in presence of Ti-, Zr-, Al-, Sn- and Si-alkoxides (1996)
    Springer
    Journal of sol gel science and technology 7 (1996), S. 217-224 
    Details
    ISSN: 1573-4846
    Keywords: metal alkoxides ; catalysis ; phenylsiloxanes ; structural units ; 29Si NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The investigation of the effects of small amounts of Ti-, Zr-, Al-, Sn- and Si-alkoxides and those of triethylamine and hydrochloric acid on the condensation reaction of diphenylsiloxanediol (DPSD) in molar ratio Si : additive = 1:0.01 and 1:0.04 by 29Si NMR shows a decrease in their activity in the order Ti≈HCl〉Al〉Sn≈N(Et)3≈Zr〉Si after 6 h reaction time. The influence of the type of alkoxide ligands attached to the metal on the condensation rate of DPSD was found relatively low compared to the different metals. In presence of Ti-alkoxide the condensation reaction of DPSD leads to di-, tri- and tetrasiloxanediols, the latter of which dominates and crystallizes from the solution as octaphenyltetrasiloxanediol. The catalysis of DPSD solutions by Al-alkoxide and HCl results preferably in tetraphenyldisiloxanediol species even after a few days. The complexity of metal alkoxides and the hydrolytic stability of heterometallic Si−O−M bonds have been discussed as possible reasons for the differences in the catalytic activity of the metal alkoxide.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00401040
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    Paper (German National Licenses)
    Fulltext
  • 2
    Electronic Resource
    Electronic Resource
    On the Hydrolytic Stability of Organic Ligands in Al-, Ti- and Zr-Alkoxide Complexes (1997)
    Springer
    Journal of sol gel science and technology 10 (1997), S. 115-126 
    Details
    ISSN: 1573-4846
    Keywords: metal alkoxide complexes ; β-keto ligands ; hydrolysis ; particle size ; IR ; 13C NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The complexation degrees of Al-, Ti- and Zr-butoxide (M) with unsaturated and saturated β-diketones (3-allylpentane-2.4-dione-APD, acetylacetone-ACAC) and β-ketoesters (methacryloxyethyl-acetoacetate-MEAA, allylacetoacetate-AAA, ethylacetoacetate-EAA) as organic ligands (L) were examined by IR and 13 C NMR spectroscopy and were found to be L:M ≥ 1.5. The hydrolytic stability of the ligands of the metal alkoxide complexes (L:M = 1) during hydrolysis/condensation reactions at the molar ratio h (H2O : OR) = 0.5–2.0 decreases with increasing H〈math〉2O:complex ratio. Furthermore, the ligand stability depends on the type of metal in the complexes and decreases in the order Al- 〉 Zr- 〉 Ti-butoxide complexes at h=1. The ACAC ligand likewise shows in the Al-, Ti- and Zr-butoxide complexes a high hydrolytic stability (95–100%) at h=1 within 7 days. The Ti- and Zr-butoxide complexes with β-ketoesters as ligand show at h=1〉 a release to a different extent e.g., up to 60% in the case of the MEAA-ligand in the Ti-butoxide complex after 2 days. In general, the hydrolytic stability of the ligands in the Ti-butoxide complexes (L:M = 1, h=1) decreases in the order ACAC 〉 APD 〉 AAA 〉 EAA ≥ MEAA. The hydrolysis/condensation reaction of complexes having a weak ligand stability leads to larger particle sizes in the sols than those with stable ACAC ligands. The results contribute to a more controlled synthesis of sols and of new inorganic-organic hybrid polymers via the sol-gel process.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1018305811088
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    Paper (German National Licenses)
    Fulltext
  • 3
    Electronic Resource
    Electronic Resource
    29Si and 17O NMR investigations on Si−O−Ti bonds in solutions of diphenylsilanediol and titanium-tetra-isopropoxide (1996)
    Springer
    Journal of sol gel science and technology 6 (1996), S. 139-149 
    Details
    ISSN: 1573-4846
    Keywords: titanosiloxanes ; siloxanes ; hydrolysis ; condensation ; structural units ; NMR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The structural units in diphenylsilanediol/titanium-isopropoxide solutions with molar ratio Si:Ti between 1:0.1 and 1:5 were examined by means of 29Si and 17O NMR. The main component in solutions with molar ratio Si/Ti=1:0.1 is the chain-like octaphenyltetrasiloxanediol. With increasing Ti-isopropoxide content (1:0.25–1:05) Si−O−Ti units of the spirocyclic titanosiloxane Ti[O5Si4(C6H5)8]2 prevail in the solutions accompanied by the chain-like tetrasiloxanediol. The 29Si NMR spectra of 1:1 solutions indicate a lot of different Si containing building units with chemical shifts mainly between-40 and-46 ppm. The signals with a chemical shift between-40 and-46 ppm are probably caused by Si atoms which are connected via oxygen bridges directly (Si−O−Ti) or indirectly (Si−O−Si−O−Ti) with titanium. Contrary to the 1:1 solutions only one or two different species with Si−O−Ti units are present in high Ti-alkoxide containing solutions (1:5). 29Si and 17O NMR results reveal a quick hydrolysis of the Ti−O−Si bonds to titanium-oxo-hydroxo-polymers and phenylsiloxanediols or their isopropyl esters after the addition of water to the solutions. This separation into species only containing either Ti−O−Ti or Si−O−Si bonds can entail a decreased homogeneity of the reaction products on a molecular level.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00425971
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    Paper (German National Licenses)
    Fulltext
  • 4
    Electronic Resource
    Electronic Resource
    [TMPA]4[Si8O20] · 34 H2O and [DDBO]4[Si8O20] · 32 H2O are heteronetwork clathrates with 1,1,4,4-tetramethylpiperazinium (TMPA) and 1,4-dimethyl-1,4-diazoniabicyclo[2.2.2]octane (DDBO) guest cations (1994)
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 620 (1994), S. 757-765 
    Details
    ISSN: 0044-2313
    Keywords: Silicate hydrate ; 1,1,4,4-tetramethylpiperazinium ; 1,4-dimethyl-1,4-diazoniabicyclo[2.2.2]octane ; 1,1-dimethylpiperidinium ; clathrate ; crystal structure ; double four-ring silicate anion ; hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: [TMPA]4[Si8O20] · 34 H2O und [DDBO]4[Si8O20] · 32 H2O sind Heteronetzwerk-Clathrate mit 1,1,4,4-Tetramethylpiperazinium (TMPA) und 1,4-Dimethyl-1,4-Diazoniabicyclo[2.2.2]octan (DDBO) Gastkationen[TMPA]4[Si8O20] · 34 H2O (1) und [DDBO]4[Si8O20] · 32 H2O (2) wurden durch Kristallisation aus wäßrigen Lösungen der entsprechenden quartären Alkylammoniumhydroxide und SiO2 erhalten. Die Kristallstrukturen wurden mittels Einkristallröntgenbeugung bestimmt. 1: Monoklin, a = 16,056(2), b = 22,086(6), c = 22,701(2) Å, β = 90,57(1)° (T = 210 K), Raumgruppe C2/c, Z = 4. 2: Monoklin, a = 14,828(9), b = 20,201(7), c = 15,519(5) Å, β = 124,13(4)° (T = 255 K), Raumgruppe P21/c, Z = 2. Die Polyhydrate sind strukturverwandte Wirt-Gast-Verbindungen mit dreidimensionalen Wirtstrukturen aus über Wasserstoffbrücken verknüpften oligomeren Anionen [Si8O20]8- und H2O-Molekülen. Die Silicat-Anionen haben eine würfelförmige Doppelvierring-Struktur und eine lokale Umgebung, die von 24 H2O-Molekülen und sechs Kationen (TMPA, [C8H20N2]2+, oder DDBO, [C8H18N2]2+) gebildet wird. Die Kationen befinden sich als Gastspezies in großen, unregelmäßigen, käfigartigen Hohlräumen. Untersuchungen mittels der 29Si-NMR-Spektroskopie und der Trimethylsilylierungsmethode haben gezeigt, daß die gesättigten Lösungen von 1 und 2 hohe Anteile an Doppelvierring-Anionen enthalten. Derartige Anionen sind auch in der gesättigten Lösung des Heteronetzwerk-Clathrats [DMPI]6[Si8O18(OH)2] · 48,5 H2O (3) mit 1,1-Dimethylpiperidinium-Kationen (DMPI, [C7H16N]+) als Gastspezies enthalten.
    Notes: [TMPA]4[Si8O20] · 34 H2O (1) and [DDBO]4[Si8O20] · 32 H2O (2) have been prepared by crystallization from aqueous solutions of the respective quaternary alkylammonium hydroxide and SiO2. The crystal structures have been determined by single-crystal X-ray diffraction. 1: Monoclinic, a = 16.056(2), b = 22.086(6), c = 22.701(2) Å, β = 90.57(1)° (T = 210 K), space group C2/c, Z = 4. 2: Monoclinic, a = 14.828(9), b = 20.201(7), c = 15.519(5) Å, β = 124.13(4)° (T = 255 K), space group P21/c, Z = 2. The polyhydrates are structurally related host-guest compounds with three-dimensional host frameworks composed of oligomeric [Si8O20]8- anions and H2O molecules which are linked via hydrogen bonds. The silicate anions possess a cube-shaped double four-ring structure and a characteristic local environment formed by 24 H2O molecules and six cations (TMPA, [C8H20N2]2+, or DDBO, [C8H18N2]2+). The cations themselves reside as guest species in large, irregular, cage-like voids. Studies employing 29Si NMR spectroscopy and the trimethylsilylation method have revealed that the saturated aqueous solutions of 1 and 2 contain high proportions of double four-ring silicate anions. Such anions are also abundant species in the saturated solution of the heteronetwork clathrate [DMPI]6[Si8O18(OH)2] · 48.5 H2O (3) with 1,1-dimethylpiperidinium (DMPI, [C7H16N]+) guest cations.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/zaac.19946200430
    Location Call Number Expected Availability
    BibTip Others were also interested in ...
    Paper (German National Licenses)
    Fulltext
Close ⊗
This website uses cookies and the analysis tool Matomo. More information can be found here...