Preparation method of vinyl tri(dimethylsiloxane) silane
A technology of vinyltrimethoxysilane and dimethylsiloxane, which is applied in the field of preparation of vinyltrisilane, can solve the problems of lower product yield, slow reaction, serious exothermic heat, etc., and the temperature is easy to control, The effect of short process and mild reaction temperature
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Embodiment 1
[0032] (1) Add 5g of concentrated sulfuric acid, 64g of methanol, and 81g of water into a 1000mL three-necked flask equipped with a magnetic stirrer, a thermometer, a condenser tube, and an oil bath heating device to obtain a mixed solution A, and add 268.7g of tetramethyl Disiloxane, stirred and heated up to 40°C to react to obtain mixed liquid B;
[0033] (2) Add 74g of vinyltrimethoxysilane dropwise to the mixed solution B to continue the reaction for 2h, the reaction is completed to obtain the mixed solution C, and the gas chromatography detects the reaction situation, wherein the product content is 60%;
[0034] (3) The mixed solution C is separated, washed twice with 500g of water, and the supernatant is filtered after drying with anhydrous magnesium sulfate for 3h, and the filtrate is transferred to the distillation equipment, and the solvent methanol is separated by atmospheric distillation first, and the Pressure distillation separated the front fraction and the produ...
Embodiment 2
[0036] (1) Add 0.33g of hydrochloric acid, 16g of methanol, and 36g of water into a 1000mL three-neck flask equipped with a magnetic stirrer, a thermometer, a condenser tube, and an oil bath heating device to obtain a mixed solution A, and add 201.5g of tetramethyl Disiloxane, stirred and heated to 20°C to react to obtain mixed liquid B;
[0037] (2) Add 74g of vinyltrimethoxysilane dropwise to the mixed solution B to continue the reaction for 6h. After the reaction is completed, the mixed solution C is obtained. The reaction situation is detected by gas chromatography, and the product content is 48%;
[0038] (3) The mixed solution C is separated, washed twice with 500g of water, and the supernatant is filtered after drying with anhydrous magnesium sulfate for 3h, and the filtrate is transferred to the distillation equipment, and the solvent methanol is separated by atmospheric distillation first, and the Pressure distillation separated the front fraction and the product, and...
Embodiment 3
[0040] (1) Add 7.4g sodium methoxide, 160g methanol, and 108g water into a 1000mL three-neck flask equipped with magnetic stirring, thermometer, condenser and oil bath heating device to mix to obtain mixed solution A, and add 403g tetramethyl Disiloxane, stirred and heated up to 50°C for reaction to obtain mixed liquid B;
[0041] (2) Add 74g of vinyltrimethoxysilane dropwise to the mixed solution B to continue the reaction for 3h. After the reaction is completed, the mixed solution C is obtained. The reaction situation is detected by gas chromatography, and the product content is 37%;
[0042] (3) The mixed solution C is separated, washed twice with 500g of water, and the supernatant is filtered after drying with anhydrous magnesium sulfate for 3h, and the filtrate is transferred to the distillation equipment, and the solvent methanol is separated by atmospheric distillation first, and the Pressure distillation is separated front cut and product, and remaining high-boiling co...
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