Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2.
Identifieur interne : 000751 ( PubMed/Checkpoint ); précédent : 000750; suivant : 000752Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO4/2.
Auteurs : Jerzy J. Chru Ciel [Pologne] ; Marzena Fejdy [Pologne] ; Witold Fortuniak [Pologne]Source :
- Polymers [ 2073-4360 ] ; 2018.
Abstract
Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO4/2 (Q), both MeHSiO (DH) and Me₂SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me₃SiO0.5 (M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150⁻155 °C. Yields of PMHS-Q reached from 55⁻69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7⁻13.1 cP. Molecular weights (MW) of PMHS-Q (Mn = 2440⁻6310 g/mol, Mw = 5750⁻10,350 g/mol) and polydispersities of MW (Mw/Mn = 2.0⁻2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, ¹H- and 29Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of 29Si-NMR results and compared with literature data.
DOI: 10.3390/polym10050484
PubMed: 30966518
Affiliations:
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<front><div type="abstract" xml:lang="en">Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO<sub>4/2</sub>
(Q), both MeHSiO (D<sup>H</sup>
) and Me₂SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me₃SiO<sub>0.5</sub>
(M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150⁻155 °C. Yields of PMHS-Q reached from 55⁻69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7⁻13.1 cP. Molecular weights (MW) of PMHS-Q (M<sub>n</sub>
= 2440⁻6310 g/mol, M<sub>w</sub>
= 5750⁻10,350 g/mol) and polydispersities of MW (M<sub>w</sub>
/M<sub>n</sub>
= 2.0⁻2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, ¹H- and <sup>29</sup>
Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of <sup>29</sup>
Si-NMR results and compared with literature data.</div>
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<Abstract><AbstractText>Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO<sub>4/2</sub>
(Q), both MeHSiO (D<sup>H</sup>
) and Me₂SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me₃SiO<sub>0.5</sub>
(M) were prepared by a hydrolytic polycondensation method of appropriate organic chlorosilanes and tetraethyl ortosilicate (TEOS), in diethyl ether medium at temperature below 0 °C. Volatile low molecular weight siloxanes were removed by a vacuum distillation at 150⁻155 °C. Yields of PMHS-Q reached from 55⁻69 wt%. Their dynamic viscosities were measured in the Brookfield HBDV+IIcP cone-plate viscometer and ranged from 10.7⁻13.1 cP. Molecular weights (MW) of PMHS-Q (M<sub>n</sub>
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= 5750⁻10,350 g/mol) and polydispersities of MW (M<sub>w</sub>
/M<sub>n</sub>
= 2.0⁻2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, ¹H- and <sup>29</sup>
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Si-NMR results and compared with literature data.</AbstractText>
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