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Alkyl acyloxy silane mixture and preparation method thereof

The technology of alkylacyloxysilane and alkyltriacetoxysilane is applied in the field of alkylacyloxysilane mixture and preparation thereof, and can solve the problems of unstable quality, low content of effective components, color and the like, To achieve the effect of simple preparation method, lower production cost and environmental protection

Active Publication Date: 2009-09-16
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has solved the problem of product coagulation, because a large amount of low boiling matter, high boiling matter remain in the product, cause product to have active component content low (content is less than 90%), have color (light yellow or yellow), The disadvantage of unstable quality, the products synthesized by this method can only be applied to low-end one-component room temperature vulcanized silicone rubber, which cannot meet the requirements of high-end customers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A mixture of alkylacyloxysilanes containing 78% active methyltriacetoxysilane and 21% active ethyltriacetoxysilane was prepared.

[0022] (1) In the reactor of the electrified heating, stirring and rectifying device, add the raw materials methyltrichlorosilane, ethyltrichlorosilane and acetic anhydride in sequence, and the molar ratio is 1:0.25:7.5 in sequence, and stir and mix evenly , under normal pressure conditions, reflux reaction at a temperature of 80-100°C for 8-10 hours.

[0023] (2) When the temperature at the top of the rectification tower of the reactor rises to 48-51°C, stop the reflux, control the reflux ratio of 1:2, and rectify the reaction by-product acetyl chloride.

[0024] (3) After the rectification of the by-product acetyl chloride is completed, carry out rectification under reduced pressure at a temperature of 100-150°C and -0.08-0.09MPa, control the reflux ratio of 1:1, and rectify and recover the excess raw material acetic anhydride, Raw materi...

Embodiment 2

[0028] A mixture of alkylacyloxysilanes containing 78% effective methyltriacetoxysilane and 21% effective n-propyltriacetoxysilane was prepared.

[0029] (1) In the reactor of the electrified heating, stirring and rectifying device, add the raw materials methyltrichlorosilane, n-propyltrichlorosilane and acetic anhydride in sequence, and the molar ratio is 1:0.25:7.5 in sequence, and stir and mix Evenly, under normal pressure conditions, reflux reaction at a temperature of 80-100° C. for 8-10 hours.

[0030] (2) When the temperature at the top of the rectification tower of the reactor rises to 48-51°C, stop the reflux, control the reflux ratio of 1:2, and rectify the reaction by-product acetyl chloride.

[0031] (3) After the rectification of the by-product acetyl chloride is completed, carry out rectification under reduced pressure at a temperature of 100-150°C and -0.08-0.09MPa, control the reflux ratio of 1:1, and rectify and recover the excess raw material acetic anhydride...

Embodiment 3

[0035] A mixture of alkylacyloxysilanes containing 78% active methyltriacetoxysilane and 21% active allyltriacetoxysilane was prepared.

[0036] (1) In the reactor of the electrified heating, stirring and rectifying device, add the raw materials methyltrichlorosilane, allyltrichlorosilane and acetic anhydride in sequence, and the molar ratio is 1:0.25:7.5 in sequence, and stir and mix Evenly, under normal pressure conditions, reflux reaction at a temperature of 80-100° C. for 8-10 hours.

[0037] (2) When the temperature at the top of the rectification tower of the reactor rises to 48-51°C, stop the reflux, control the reflux ratio of 1:2, and rectify the reaction by-product acetyl chloride.

[0038] (3) After the rectification of the by-product acetyl chloride is completed, carry out rectification under reduced pressure at a temperature of 100-150°C and -0.08-0.09MPa, control the reflux ratio of 1:1, and rectify and recover the excess raw material acetic anhydride, Raw mater...

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Abstract

The invention relates to an alkyl acyloxy silane mixture and a preparation method thereof, belonging to the technical field of preparation of alkyl acyloxy silane mixture. In the mixture, the content of methyltriacetoxysilane is 75% to 85%, and the content of alkyltriacetoxysilane is 15% to 25%; alkyl is ethyl, ethylene, n-propyl, isopropyl or allyl, the content of active principle is greater than 98%, and the appearance is water-white transparent liquid. The preparation method of the mixture has low production cost and environment-protection benefit with excessive raw material acetic anhydride and generated by-product acetyl chloride recovered by rectification. The invention solves the difficulties of production, package transportation and application as the high-purity alkyl acyloxy silane mixture product is solid crystal at room temperature at present as well as the existing problems of low content of active principle, color, unstable quality as the mixture is not condensed into liquid product at room temperature so that the product can only be applied to low-end single-compound room temperature sulphurated siliastic. The preparation method can be applied to high-end single-compound room temperature sulphurated siliastic.

Description

Technical field: [0001] The invention relates to an alkylacyloxysilane mixture and a preparation method thereof, belonging to the technical field of preparation of alkylacyloxysilane mixtures. Background technique: [0002] The existing deacetate-type organosilicon crosslinking agent is mainly methyltriacetoxysilane. Since the freezing point of methyltriacetoxysilane is 41.3°C, the high-purity product is a solid crystal at room temperature, and the product is in It is easy to absorb moisture in the air and release sour acetic acid, so this brings difficulties to the industrial production, packaging, transportation and application of high-purity methyltriacetoxysilane products. [0003] At present, in order to solve the problem that its products solidify at room temperature, the method adopted in the industry is to prepare low-content methyltriacetoxysilane. The specific implementation method is: first put the raw materials methyltrichlorosilane and acetic anhydride into the...

Claims

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Application Information

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IPC IPC(8): C08K5/541C08L83/04C07F7/18
Inventor 阮少阳瞿小平简永强胡江华王灿甘书官尹超
Owner JINGZHOU JIANGHAN FINE CHEM
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