A kind of method for preparing diphenylsilanediol

Abstract

The invention belongs to the field of organic chemistry and discloses a method for preparing diphenylsilanediol. The method is to add diphenyldialkoxysilane and organic solvent into the reaction vessel, stir evenly, then add deionized water and acid catalyst, heat up to 55-65°C and reflux for 4-6 hours, cool, age, and filter , rotary evaporation to obtain diphenylsilanediol; said diphenylsilanediol is a needle crystal. The present invention uses diphenyldialkoxysilane as a raw material, and the prepared diphenylsilanediol has a high conversion rate and a product content of 99.7%. The raw material used does not contain chlorine, which effectively avoids the introduction of chloride ions; the present invention The reaction temperature is relatively mild, and it adopts normal temperature crystallization, which is easy to be separated by filtration.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a method for preparing diphenylsilanediol by a crystallization method. Background technique [0002] Diphenylsilanediol can be used as a silicone rubber structure control agent to reduce the structural phenomenon of silicone rubber and improve the processing performance of silicone rubber; it can be used to synthesize phenyl silicone oil, phenyl silicone resin, phenyl silicone rubber, etc.; it can also be Used as a modified intermediate for polyurethane resin, epoxy resin, acrylic resin, PP, PET, PE, etc., endowing new products with properties such as high and low temperature resistance, radiation resistance, and aging resistance. [0003] The synthesis of diphenylsilanediol is based on diphenyldichlorosilane, which is hydrolyzed in a mixture of water, alcohol, and aromatic solvents. At the same time, a large amount of hydrochloric acid is produced by-product, which n...

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Problems solved by technology

[0003] The synthesis of diphenylsilanediol is based on diphenyldichlorosilane, which is hydrolyzed in a mixture of water, alcohol, and aromatic solvents. At the same time, a large amount of hydrochloric acid is produced by-product, which needs to be absorbed by a large amount of alkali. Equipment requirements High, high pollution, and because the purity of diphenyldichlorosilane is not high and there are many impurities, the hydrolyzed diphenylsilanediol has yellow color, many impurities and low purity

"Simple and economical synthesis method of diphenylsilanediol" (Chen Yulian et al., "Applied Chemistry", 2010, 39(7), 1039-1041) using diphenyldichlorosilane as raw material, in the aqueous solution of sodium hydroxide Diphenylsilanediol was synthesized by direct hydrolysis in the reaction system, the concentration of alkali in the reaction system was 5%, the reaction temperature was 0-2°C, and the product yield was 92%. Hydrochloric acid is continuously released in the medium, which makes it impossible to maintain the concentration of the sodium hydroxide aqueous solution in a stable state. Unless the amount of sodium hydroxide is continuously added, it cannot be realized in production, and the reaction is carried out at 0-2 °C, and the conditions are relatively harsh.

[0004] Diphenylsilanediol can also be obtained by hydrolysis using diphenyldialkoxysilane as a raw material, but diphenylsilanediol is insoluble in water, and it is easy to form a suspension that is difficult to separate. It needs to be extracted with toluene, and diphenylsilanediol Phenylsilanediol is dissolved in toluene. In the presence of a hydrolysis catalyst, intermolecular dehydration condensation easily occurs to generate phenylcyclosiloxane and linear phenyl silicone oil, which are difficult to separate and reduce the product yield. This reaction also requires Carried out at a low temperature of 0-2°C