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Method for preparing trialkylsilanol

A technology of trihydrocarbyl silanol and hydrocarbyl chlorosilane, which is applied in the field of preparation of trihydrocarbyl silanol, can solve the problems of low reactivity, achieve the effects of improving yield and purity, avoiding condensation reaction, and being easy to control

Active Publication Date: 2017-01-04
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods all have too low or too high reactivity, and carbon dioxide gas will be generated during the reaction, which puts higher requirements on the production equipment and will also bring a lot of safety hazards.

Method used

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  • Method for preparing trialkylsilanol
  • Method for preparing trialkylsilanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 109 g of trimethylchlorosilane and 80 g of ammonium acetate into a 1000 mL four-neck flask, heat up to 130° C. under stirring, and react for 2 hours to obtain a solid-liquid mixture. At 30° C., 194 g of hexamethyldisilazane and 90 g of deionized water were added dropwise to the mixture at the same time, and the drop was completed in about half an hour. The obtained emulsion continued to stir and react for 3 hours to complete the hydrolysis reaction. Separate the upper liquid and dry it overnight in anhydrous sodium sulfate. After filtering, 291g of colorless and transparent liquid, i.e. trimethylsilanol, was obtained, with a yield of 95% and a purity of 98%. (GC).

Embodiment 2

[0018] Add 54 g of trimethylchlorosilane and 50 g of sodium acetate into a 500 mL four-necked flask, heat up to 80° C. under stirring, and react for 3 hours to obtain a solid-liquid mixture. At 25° C., 81 g of hexamethyldisilazane and 300 g of deionized water were added dropwise to the mixture at the same time, and the drop was completed in about half an hour. The obtained emulsion was stirred and reacted for 3 hours to complete the hydrolysis reaction, the upper liquid was separated and dried overnight in anhydrous sodium sulfate, and 125 g of colorless transparent liquid, i.e. trimethylsilanol, was obtained after filtration, with a yield of 92% and a purity of 97%. (GC).

Embodiment 3

[0020] Add 54 g of trimethylchlorosilane and 49 g of potassium acetate into a 500 mL four-neck flask, heat up to 100° C. under stirring, and react for 2.5 hours to obtain a solid-liquid mixture. At 25°C, 81 g of hexamethyldisilazane and 20 g of deionized water were simultaneously added dropwise to the mixture, and the drop was completed in about half an hour. The obtained emulsion was stirred and reacted for 1 hour to complete the hydrolysis reaction, filtered, and the upper layer liquid was separated and dried in anhydrous magnesium sulfate for 2 hours. After filtering, 122 g of a colorless transparent liquid, i.e., trimethylsilanol, was obtained, with a yield of 90%. Purity 96% (GC).

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Abstract

The invention provides a method for preparing trialkylsilanol. In the method, trialkylchlorosilane reacts with carboxylate, and after reaction is complete, solid-liquid mixture is obtained; hexaalkyl disilazane and deionized water are then dripped into the mixture, agitation is continued for reaction after dripping is complete, supernatant liquid is separated after reaction is complete, and after drying agent is added for sufficient drying, the trialkylsilanol is obtained. The preparation method provided by the invention is safe and easy to operate, and can help to realize industrial production.

Description

technical field [0001] The invention relates to a method for preparing trihydrocarbyl silanol by using trihydrocarbyl chlorosilane and hexahydrocarbyl disilazane as main raw materials. Background technique [0002] Trihydrocarbylsilanols are a class of very useful compounds that can be used as silylating agents, intermediates in the synthesis of various organosilicon compounds, or coating additives. Its main synthesis methods are: (1) Hydrolysis of hexaalkyldisilazane in the presence of hydrochloric acid, further extraction and fractionation to obtain trialkylsilanol (R.O.Sauer.J.Am.Chem.Soc, 1944, 66, 1707.). (2) Trihydrocarbyl silanol is produced by a method of hydrolyzing a trihydrocarbyl chlorosilane compound in the presence of a base. (L. H. Sommer, E. W. Pietrusza, F. C. Whitmore. J. Am. Chem. Soc, 1946, 68, 2282.). However, the above two methods have a violent reaction process and need to use organic solvents such as butyl ether for extraction and separation, and th...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0836
Inventor 余神銮姜哲白俊玲刘继曾莉周建梅
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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