Method for preparing diphenyl silanediol

A technology of diphenylsilicon diol and diphenyl dialkoxysilane is applied in the field of preparing diphenylsilicon diol by a crystallization method, and can solve the problems of low purity, difficult separation, intermolecular dehydration and condensation, and the like, Achieve the effect of easy filtration and separation, high conversion rate, and avoid the introduction of impurity ions

Inactive Publication Date: 2015-12-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 5L flask, add 1000g diphenyldimethoxysilane (99.5% by mass), 1000g acetone, stir evenly (the stirring speed is 80 rpm, and the stirring time is 10min), then add 150g of dimethoxysilane Ionized water and 0.021g acetic acid, heat the solution to 60°C and reflux for 4h (50 minutes after the start of reflux, the solution in the flask turns from transparent to cloudy, with precipitation); cool to room temperature, age for 5h, let diphenylsilane The diol is fully crystallized and precipitated, then the solution is filtered out with a 500-mesh filter cloth, the filter cake is centrifuged (centrifugal speed is 2000 rpm, and the centrifugation time is 30min), and it is rotated at -0.099MPa and 40°C for 4h to remove Moisture and solvent adsorbed on the surface yielded dry needle-shaped crystals, namely diphenylsilanediol, weighing 867g, yield 97.97%, content 99.5%, melting point 141°C.

Embodiment 2

[0027] In a 5L flask, add 1000g diphenyldimethoxysilane (mass percentage is 99.5%), 2000g acetone, stir evenly (stirring speed is 100 rpm, stirring time is 10min), then add 160g of Ionized water and 0.1g acetic acid, heat the solution to 58°C and reflux for 5h (48min after the start of reflux, the solution in the flask turns from transparent to cloudy, with precipitation); cool to room temperature, age for 6h, let diphenylsilane The diol is fully crystallized and precipitated, and then the solution is filtered out with a 600-mesh filter cloth, the filter cake is centrifuged (centrifugal speed is 1800 rpm, and the centrifugation time is 40min), and it is rotated at -0.098MPa and 50°C for 4h to remove Moisture and solvent adsorbed on the surface yielded dry needle-like crystals, namely diphenylsilanediol, weighing 870g, yield 98.3%, content 99.6%, melting point 141°C.

Embodiment 3

[0029] In a 5L flask, add 1000g diphenyldimethoxysilane (mass percentage is 99.8%), 3000g acetone, stir evenly (stirring speed is 120 rpm, stirring time is 8min), then add 180g of Ionized water and 1g of acetic acid, heat the solution to 56°C and reflux for 6h (55 minutes after the start of reflux, the solution in the flask turns from transparent to cloudy, with precipitation); cool to room temperature, age for 8h, let diphenylsilane Alcohol is fully crystallized and precipitated, then filter the solution with a 800-mesh filter cloth, and carry out centrifugal drying of the filter cake (centrifugal speed is 1600 rpm, centrifugation time is 45min), rotary evaporation at -0.095MPa and 60°C for 5h, remove Moisture and solvent adsorbed on the surface yielded dry needle-like crystals, namely diphenylsilanediol, weighing 864g, yield 97.63%, content 99.7%, melting point 141°C.

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Abstract

The invention belongs to the field of organic chemistry, and discloses a method for preparing diphenyl silanediol. The method comprises the following steps: adding diphenyl dialkoxysilane and an organic solvent into a reaction vessel, uniformly stirring, adding deionized water and an acid catalyst, heating to 55-65 DEG C, refluxing for 4-6 hours, cooling, aging, filtering, and carrying out rotary evaporation to obtain the diphenyl silanediol. The diphenyl silanediol is an acicular crystal. By using the diphenyl dialkoxysilane as the raw material, the prepared diphenyl silanediol has high conversion rate, and the product content is up to 99.7%; and the adopted raw material is free of chlorine, thereby effectively avoiding the introduction of chlorine ions. The method has the advantage of mild reaction temperature; and due to the adoption of normal temperature crystallization, the diphenyl silanediol is easy for filtration and separation.

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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08
Inventor 涂伟萍朱淮军戴子林
Owner SOUTH CHINA UNIV OF TECH
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