Synthesis, Characterization and Microstructure of New Liquid Poly(methylhydrosiloxanes) Containing Branching Units SiO(4/2)

Six liquid branched poly(methylhydrosiloxanes) of new random structures (PMHS-Q), containing quadruple branching units SiO(4/2) (Q), both MeHSiO (D(H)) and Me(2)SiO (D) chain building units (or only mers MeHSiO), and terminal groups Me(3)SiO(0.5) (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 (M(n) = 2440–6310 g/mol, M(w) = 5750–10,350 g/mol) and polydispersities of MW (M(w)/M(n) = 2.0–2.8) were determined by a size exclusion chromatography (SEC). All polymers were characterized by FTIR, (1)H- and (29)Si-NMR, and an elemental analysis. A microstructure of siloxane chains was proposed on a basis of (29)Si-NMR results and compared with literature data.