Synthesis of Multifunctional Oligomethylsilsesquioxanes by Catalyst-Free Hydrolytic Polycondensation of Methyltrimethoxysilane under Microwave Radiationстатья
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Аннотация:The catalyst-free hydrolytic polycondensation of methyltrimethoxysilane under microwaveradiation has been studied. The effect of molar ratios of the reagents (MTMS/H2O = 1/0.5–1/9),radiation power (20–300 W), temperature (30–50 ◦C) and duration of exposure (2.5–90 min) onthe course of the process is considered. It has been shown that the use of microwave radiationpromotes the activation of the process, and almost complete conversion of the monomer can beachieved in 5 min at 30 ◦C, 20 W and an MTMS/H2O ratio of 1/3. The optimal radiation powerfor the maximum conversion of the monomer and MeO-groups is in the range from 20 to 100 W.An increase in the water amount, the duration and temperature of the process contribute to anincrease in the monomer conversion, a decrease in the content of residual MeO-groups and the yieldof non-volatile oligomethylsilsesquioxanes. The limits of this approach using to the synthesis ofmultifunctional branched polyorganosilsesquioxanes are determined. Depending on the processconditions, homogeneous water–alcohol solutions of oligomethylsilsesquioxane with a concentrationof 20 to 50 wt.% can be obtained. The OH-group content and the molecular weight of the obtainedoligomers vary from 10 to 30 wt.% and from 1000 to 600 Da, respectively.