Method for preparing trichlorideacetyl chloride from mother liquor of chloroactic acid

A technology of mother liquor of trichloroacetyl chloride and chloroacetic acid, which is applied in the general field of organic chemistry, can solve the problems of potential safety hazards, complex intermediate product components, complex production equipment, etc., and achieve stable operation safety performance, high product purity and yield , The effect of low production cost

Inactive Publication Date: 2005-01-12
大庆市富杰化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Existing open method for preparing trichloroacetyl chloride has multiple, as: the patent No. is: the patent publication document of 96116022.5,00107419.9,99118287.1,99113977.1, but above-mentioned preparation method all exists problem in varying degrees, as: pressure is higher, The production equipment is relatively complex, the reaction cycle is long, the operation is difficult, there are potential safety hazards, the composition of the intermediate product is complex, and it is not easy to separate, etc.

Method used

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Examples

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Effect test

Embodiment 1

[0010] The method for preparing trichloroacetyl chloride with chloroacetic acid mother liquor of the present invention is: carrying out 140 degree centigrade distillation refining of chloroacetic acid mother liquor to remove low-boiler impurities; refined chloroacetic acid mother liquor is passed through chlorine gas under the effect of sulfur monochloride to carry out Acid chlorination to obtain a mixture of acid chlorides, and then rectification to obtain a mixture of monochloroacetyl chloride and dichloroacetyl chloride; the mixture of acid chlorination reaction is chlorinated by passing chlorine gas under the action of pyridine as a catalyst and activated carbon as a cocatalyst. After distillation, the product of trichloroacetyl chloride is obtained.

Embodiment 2

[0012] The composition of the chloroacetic acid mother liquor includes: 5-10% of acetic acid, 35-45% of chloroacetic acid, 40-50% of dichloroacetic acid, and 5% of impurities (moisture, glacial acetic acid and other low boilers). The feed ratio of chlorine gas, refined chloroacetic acid mother liquor and sulfur monochloride in the acid chloride reaction is 0.85:1.0:0.3, the reaction temperature is 47-53 degrees Celsius, and the reaction time is 10-16 hours. The weight ratio of the catalyst pyridine in the chlorination reaction to the mixture of monochloroacetyl chloride and dichloroacetyl chloride is 0.0025: 1.0, and the weight ratio of the promoter activated carbon to the mixture of monochloroacetyl chloride and dichloroacetyl chloride is 0.1: 1.0. The end point of the chlorination reaction is that the content of monochloroacetyl chloride and dichloroacetyl chloride in the reactant is not more than 1.0%, and the fraction of the trichloroacetyl chloride product separated by rec...

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PUM

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Abstract

Mother liquor is refined by distilation at temp. of 140 deg.C to remove low boiling point matters, then under the function of sulfur monochloride, pumping in chlorine gas to proceed acyl-chlorization to abtain acetic chloride mixture. After rectifications, the mixture of monoacetic chloride and diacetic chloride is obtained. The mixture is then chloridized by pumping-in chlorine gas using catalyst of pyridine and assistant catalyst active carbon. After rectification the final product trichloro-acetic chloride is obtd. The advantages are: raw material is available easily, simple process, safety, high pureness and high yield.

Description

technical field [0001] The invention belongs to the general method of organic chemistry, in particular to a method for preparing trichloroacetyl chloride with chloroacetic acid mother liquor. Background technique [0002] Existing open method for preparing trichloroacetyl chloride has multiple, as: the patent No. is: the patent publication document of 96116022.5,00107419.9,99118287.1,99113977.1, but above-mentioned preparation method all exists problem in varying degrees, as: pressure is higher, The production equipment is relatively complex, the reaction cycle is long, the operation is difficult, there are potential safety hazards, and the intermediate products have complex components and are not easy to separate. Contents of the invention [0003] The present invention aims at solving the deficiencies in the prior art, has designed a kind of method for preparing trichloroacetyl chloride with chloroacetic acid mother liquor, comprises following process: [0004] a, the c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C53/48
Inventor 孙玉波
Owner 大庆市富杰化工有限公司
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