Preparation method of multichain trapezoidal polyalkyl silsesquioxane
A polyalkylsilane and silsesquioxane technology, which is applied in the field of preparation of multi-chain ladder polyalkylsilsesquioxane, can solve unsuitable large-scale production and application, high activity of reactive monomers, and complicated operation and other problems, to achieve the effects of easy realization of large-scale production and application, narrow molecular weight distribution, and low preparation cost
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Embodiment 1
[0034] Dissolve 10 parts of phenyltrimethoxysilane in 100 parts of anhydrous methyl isobutyl ketone, stir and mix evenly, then add 1.5 parts of trichloroacetic acid and react at 20°C for 5 hours. Then dropwise add a mixed solution of 11 parts of methyltrichlorosilane and 20 parts of anhydrous methyl isobutyl ketone, dropwise addition is completed in 4 hours, continue to react for 60 hours, and distill under reduced pressure: the distillation temperature starts from room temperature, until there is no distillate Raise the temperature to 60°C when flowing out, and then raise the temperature to 80°C when no fraction flows out, and finally raise the temperature to 110°C until no fraction flows out. Dissolve the distillation residue completely with 50 parts of methyl isobutyl ketone, slowly drop it into 500 parts of anhydrous methanol to gradually produce a large amount of white precipitate, filter it with suction, and dry the filter cake in vacuum at 60°C for 24 hours to obtain a w...
Embodiment 2
[0036]Dissolve 10 parts of phenyltrimethoxysilane in 100 parts of anhydrous methyl isobutyl ketone, stir and mix evenly, then add 1.5 parts of trichloroacetic acid and react at 10°C for 5 hours. Then add dropwise the mixed solution of 11 parts of methyltrichlorosilane and 15 parts of anhydrous methyl isobutyl ketone, dropwise addition is completed in 4 hours, continue to react for 60 hours, and distill under reduced pressure: the distillation temperature starts from the greenhouse first, until there is no distillate Raise the temperature to 60°C when flowing out, and then raise the temperature to 80°C when no fraction flows out, and finally raise the temperature to 110°C until no fraction flows out. Dissolve the distillation residue completely with 50 parts of toluene, slowly drop it into 500 parts of anhydrous methanol to gradually produce a large amount of white precipitate, filter it with suction, and dry the filter cake in vacuum at 60°C for 36 hours to obtain a white powde...
Embodiment 3
[0038] Dissolve 10 parts of phenyltrimethoxysilane in 100 parts of anhydrous methyl isobutyl ketone, stir and mix evenly, then add 1.5 parts of trichloroacetic acid and react at 20°C for 5 hours. Then dropwise add a mixed solution of 11 parts of methyltrichlorosilane and 15 parts of anhydrous methyl isobutyl ketone, drop it in 12 hours, continue to react for 80 hours, and distill under reduced pressure: the distillation temperature starts from the greenhouse, until there is no distillate Raise the temperature to 60°C when flowing out, and then raise the temperature to 80°C when no fraction flows out, and finally raise the temperature to 110°C until no fraction flows out. Dissolve the distillation residue completely with 50 parts of methyl isobutyl ketone, slowly drop it into 500 parts of anhydrous methanol to gradually produce a large amount of white precipitate, filter it with suction, and dry the filter cake under vacuum at 60°C for 48 hours to obtain a white powder polymethy...
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