Preparation of acetoxylsilane

A technology of acetoxysilane and organochlorosilane, applied in the field of preparation of acetoxysilane, can solve the problems of high chloride ion content, high production cost, affecting the storage of finished silicone rubber products, etc., and achieves high purity and low cost. , good quality effect

Active Publication Date: 2008-12-17
湖北环宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a preparation method of acetoxysilane to solve the technical problems such as the high production cost of the existing acetoxysilane, the high chloride ion content in the obtained product, and the impact on the storage of finished silicone rubber products.

Method used

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  • Preparation of acetoxylsilane

Examples

Experimental program
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Effect test

Embodiment 1

[0013] Example 1: Preparation of methyltriacetoxysilane. Add 1mol methyltrichlorosilane and 150ml solvent gasoline into the reaction vessel (such as a four-necked flask with a thermometer, condenser, stirring, constant pressure cylindrical funnel and cylindrical packing tower), under stirring conditions, the above liquid After gradually increasing the temperature to boiling, start to add 3.3 mol of acetic acid to react with methyl trichlorosilane, and the boiling reaction is 8 hours to obtain the methyl triacetoxy silane solution. At the same time, the HCl gas is collected during the reaction to obtain the by-product hydrochloric acid; Control the temperature at 100-110℃, and recover the solvent gasoline in the acetoxysilane solution by distillation under normal pressure. After the solvent gasoline recovery rate reaches 93%, keep the temperature at 110℃, and distill under reduced pressure to remove the residual low boilers in the reaction vessel. , Until there is no distillate, a ...

Embodiment 2

[0014] Example 2: Preparation of ethyltriacetoxysilane. Add 1 mol of ethyl trichlorosilane and 160 ml of solvent gasoline into the reaction vessel. Under stirring conditions, the above liquid is gradually heated to boiling, then 3.1 mol of acetic acid is added dropwise to react with ethyl trichlorosilane, and the boiling reaction is carried out for 8 hours. Obtain the methyl triacetoxysilane solution, and collect HCl gas during the reaction to obtain the by-product hydrochloric acid; then control the temperature at 100-110°C and distill at atmospheric pressure to recover the solvent gasoline. After the solvent gasoline recovery rate reaches 93%, the The temperature is maintained at 110° C., and the low boilers remaining in the reaction vessel are removed by distillation under reduced pressure until there is no distillate to obtain a colorless and transparent product. Analysis by gas chromatograph shows that the effective content of ethyltriacetoxysilane in the product is ≥94%.

Embodiment 3

[0015] Example 3: Preparation of vinyl triacetoxysilane. Add 1 mol vinyltrichlorosilane and 180ml solvent gasoline into the reaction vessel. Under stirring conditions, the above liquid is gradually heated to boiling, then 3.2mol acetic acid is added dropwise to react with vinyltrichlorosilane, and the reaction is boiling for 8 hours Obtain methyltriacetoxysilane solution, and collect HCl gas during the reaction to obtain hydrochloric acid as a by-product; then control the temperature at 100-110°C and distill at atmospheric pressure to recover solvent gasoline. After the solvent gasoline recovery rate reaches 93%, The temperature is maintained at 110° C., and the low boilers remaining in the reaction vessel are removed by distillation under reduced pressure until there is no distillate to obtain a colorless and transparent product. Analysis by gas chromatograph shows that the effective content of vinyltriacetoxysilane in the product is ≥93%.

[0016] In the above embodiments, solve...

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Abstract

The invention discloses a preparation method of organoacetoxysilane, which adopts organochlorosilane and acetic acid as raw materials. The method comprises the following steps: the organochlorosilane and an organic solvent are added into a reaction vessel and the organic solvent is selected from one of solvent naphtha, hexane, hexamethylene, toluene, xylene and dichlorethane. The acetic acid is slowly added into the reaction vessel and reacts with the organochlorosilane and boiled for eight hours to obtain organoacetoxysilane solution; the organic solvent in the organoacetoxysilane solution is distilled at ordinary pressure and then recycled. Matters with low boiling point, remaining in the reaction vessel, are removed by distillation at reduced pressure to obtain colorless and transparent finished products. As the acetic acid has lower cost than acetic oxide and the preparation method of the invention optimizes each technological parameter, the preparation method of the invention is characterized by low cost, high efficiency, good quality, etc. In the finished product obtained, the effective content of organoacetoxysilane is more than 93 percent while the content of chloridion is less than 50PPM.

Description

Technical field [0001] The invention relates to a preparation method of acetoxysilane, in particular to a preparation method of acetoxysilane using organochlorosilane and acetic acid as raw materials. Background technique [0002] Silicone rubber (RTV) has outstanding high and low temperature resistance, maintains good flexibility in the temperature range of -70-+260℃, and has the advantages of resistance to ozone and weathering. This material does not need to be heated at room temperature. , It can be cured on the spot under pressure and is extremely convenient to use, so it is often used as an adhesive, sealant, protective coating, potting and molding material. An important raw material for the production of silicone rubber (RTV) is acetoxy silane. At present, alkyl acetoxy silane is mainly produced by the acetic anhydride method, which is made by reacting organochlorosilane and acetic anhydride. The chemical reaction formula is as follows: RSiCL 3 +3(CH 3 OC) 2 O=RSi(CH 3 COO)...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 杨世明袁发强黄国辉丁艳芳刘春香
Owner 湖北环宇化工有限公司
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