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Method for producing trichloro-acetic chloride with by-product in organic acyloxy silicone hydride production process

A technology of organic acyloxysilane and trichloroacetyl chloride, applied in the field of preparing trichloroacetyl chloride, can solve problems such as the outlet of by-product acetyl chloride, and achieve the effects of high conversion rate of raw materials, simple and easy production process, and few impurities

Inactive Publication Date: 2008-06-11
ZHEJIANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] The present invention is to solve the outlet problem of the by-product acetyl chloride in the production process of organic acetoxysilane products, and also to overcome the shortcomings of the existing trichloroacetyl chloride production process

Method used

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  • Method for producing trichloro-acetic chloride with by-product in organic acyloxy silicone hydride production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]The reaction device is shown in Figure 1, and the method of the present invention adopts an ultraviolet lamp as the reactor light source. Add 700g of by-products in the production process of organoacyloxysilane to a 1000ml reactor, first pass a small amount of chlorine gas to replace the air in the reaction system, then control the temperature of the reactor at 70°C, and open the condensing reflux device. After the reaction kettle temperature and reflux in the system are stable, slowly open the chlorine gas valve, and the reaction proceeds immediately at this time. The temperature of the photochlorination gas phase reactor is 65° C. and there are liquid droplets on the wall of the reactor, and the tail gas is strongly acidic. At this time, the heating speed should be controlled to make the reflux moderate. At the same time, the flow rate of chlorine gas should be controlled so that the mass ratio of trichloroacetyl chloride to chlorine gas is about 1:4. As the reaction c...

Embodiment 2

[0038] The reaction device is shown in Figure 1, and an ultraviolet lamp is used as the reactor light source. Add 800g of by-products in the production process of organoacyloxysilane to a 1000ml reactor, first pass a small amount of chlorine gas to replace the air in the reaction system, then control the temperature of the reactor at 72°C, and open the condensing reflux device. After the reaction kettle temperature and reflux in the system are stable, slowly open the chlorine gas valve, and the reaction proceeds immediately at this time, the temperature of the photochlorination gas phase reactor is 67° C. and there are liquid droplets on the wall of the reactor, and the tail gas is strongly acidic. At this time, the heating speed should be controlled to make the reflux moderate, and the flow rate of chlorine gas should be controlled at the same time, so that the mass ratio of trichloroacetyl chloride to chlorine gas is about 1:6. As the reaction continues intensely, the temper...

Embodiment 3

[0041] The reaction device is shown in Figure 1, and an incandescent lamp is used as the reaction light source. Add 700g of by-products in the production process of organoacyloxysilane to a 1000ml reactor, first pass a small amount of chlorine gas to replace the air in the reaction system, then control the temperature of the reactor at 70°C, and open the condensing reflux device. After the reactor temperature and reflux in the system are stable, slowly open the chlorine gas valve, and the reaction proceeds immediately at this time, the temperature of the gas phase reactor is 62° C. and there are liquid droplets on the wall of the reactor, and the tail gas is strongly acidic. At this time, the heating rate should be controlled to make the reflux moderate, and the flow rate of chlorine gas should be controlled at the same time, so that the mass ratio of trichloroacetyl chloride to chlorine gas is about 1:6. As the reaction continues intensely, the temperature in the gas phase re...

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Abstract

The invention discloses a method for preparing trichloroacetyl chloride by utilizing by-product in the production procedure of organic acyloxy radical silane. The by-product from the production procedure of organic acyloxy radical silane is contacted with chlorine gas under light source irradiation to do photo-chlorination reaction. The mass ratio of the by-product in the production procedure of organic acyloxy radical silane to chlorine gas is 1: 1-9. The photo-chlorination gas phase reaction temperature is 60-200 DEG C and the photo-chlorination reaction time is 1-24 h. The invention is not only simple and feasible in producing flow path, easy in industrialization, low in equipment investment cost, stable in operational security property, but also high in raw material conversion rate, less in impurity of reaction product, easy in purification and separation and the like.

Description

technical field [0001] The invention relates to the field of synthesis of fine organic products, in particular to a method for preparing trichloroacetyl chloride by using by-products in the production process of organic acyloxysilanes. Background technique [0002] Methyltriacetoxysilane, ethyltriacetoxysilane and vinyltriacetoxysilane are a kind of crosslinking agent or coupling agent for one-component room temperature vulcanized silicone rubber, which are widely used. In order to obtain the above-mentioned high-quality products with high purity and low chloride ion content, most manufacturers use methyltrichlorosilane and acetic anhydride, ethyltriacetoxysilane and acetic anhydride, or vinyltrichlorosilane and vinegar. Anhydrides are obtained by reacting raw materials, and their main chemical reaction equations are as follows: [0003] C 2 h 5 SiCl 3 +3(CH 3 CO) 2 O→C 2 h 5 Si(OCOCH 3 ) 3 +3CH 3 COCl [0004] CH 3 SiCl 3 +3(CH 3 CO) 2 O→CH 3 Si(OCOCH 3 ) ...

Claims

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Application Information

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IPC IPC(8): C07C53/48C07C51/58C07F7/18
Inventor 谭军范宏李伯耿
Owner ZHEJIANG UNIV
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