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Synthesis method of 2, 2, 2', 4'-tetrachloroacetophenone

A technology of tetrachloroacetophenone and synthesis method, applied in 2 fields, can solve problems such as waste of resources, high catalyst usage, general effect, etc., to reduce the generation of by-products, improve the utilization rate of raw materials, and complete the degree of reaction Effect

Inactive Publication Date: 2021-03-16
JIANGXI YONGTONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some enterprises have made great improvements in equipment and the use of rectification towers, which can achieve a certain increase in selectivity and yield, but the effect is still mediocre, and the amount of catalyst used remains high, which not only wastes resources, but also The cost control of industrial production has brought enormous pressure. In addition, there are reports in the synthesis process that the molecular sieve catalyst is used to direct the isomerization of by-products to improve the yield and purity. However, due to the limited porosity of the molecular sieve catalyst and the Experiments have found that the thermal reaction stability of this type of molecular sieve is average, resulting in unsatisfactory conversion results.
[0003] Therefore, in order to solve 2,2,2',4'-tetrachloroacetophenone synthesis process catalyst consumption is many, the product yield is general and the problems such as poor purity, the present invention proposes a kind of 2,2,2',4 The synthetic method of '-tetrachloroacetophenone to overcome the deficiencies in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A kind of 2,2,2', the synthetic method of 4'-tetrachloroacetophenone, comprises the following content:

[0028] The raw materials include 40 parts of m-dichlorobenzene, 39 parts of dichloroacetyl chloride, 26 parts of catalyst and 38 parts of water in parts by weight; the specific method is:

[0029] (1) Add the above-mentioned m-dichlorobenzene into the reaction tank, add 25% of the above-mentioned catalyst by weight, heat to 48°C while stirring at a speed of 200rpm and a heating rate of 3°C / min, and stir at a constant temperature for 10 minutes Then add 50% of the above weight part of the catalyst and slowly add 50% of the above weight part of dichloroacetyl chloride dropwise, continue stirring for 15 minutes, slowly add the remaining dichloroacetyl chloride dropwise within 35 minutes, raise the temperature to 68 ° C, keep the temperature for 20 minutes, and add the remaining catalyst , 5°C / min to raise the temperature to 100°C, stir and react at this temperature for ...

Embodiment 2

[0043] A kind of 2,2,2', the synthetic method of 4'-tetrachloroacetophenone, comprises the following content:

[0044] The raw materials include 70 parts by weight of m-dichlorobenzene, 66 parts of dichloroacetyl chloride, 35 parts of catalyst, and 68 parts of water; the specific method is:

[0045] (1) Add the above-mentioned m-dichlorobenzene into the reaction tank, add 25% of the above-mentioned catalyst by weight, heat to 54°C while stirring at a speed of 320rpm and a heating rate of 6°C / min, and stir at a constant temperature for 15 minutes Then add 50% of the above weight part of the catalyst and slowly add 50% of the above weight part of dichloroacetyl chloride dropwise, continue stirring for 25min, slowly add the remaining dichloroacetyl chloride dropwise within 55min, raise the temperature to 80°C, keep the temperature for 30min, and add the remaining catalyst , 10°C / min to raise the temperature to 105°C, stir and react at this temperature for 6 hours, and the stirrin...

Embodiment 3

[0059] A kind of 2,2,2', the synthetic method of 4'-tetrachloroacetophenone, comprises the following content:

[0060] The raw materials include 55 parts of m-dichlorobenzene, 52 parts of dichloroacetyl chloride, 30 parts of catalyst and 53 parts of water in parts by weight; the specific method is:

[0061] (1) Add the above-mentioned m-dichlorobenzene into the reaction tank, add 25% of the above-mentioned catalyst by weight, heat to 51°C while stirring at a speed of 260rpm and a heating rate of 5°C / min, and stir at a constant temperature for 12 minutes Then add 50% of the above weight part of the catalyst and slowly dropwise drop 50% of the above weight part of dichloroacetyl chloride, continue to stir for 20 minutes, slowly add the remaining dichloroacetyl chloride dropwise within 45 minutes, raise the temperature to 74 ° C, keep the temperature for 25 minutes, and add the remaining catalyst , 8°C / min to raise the temperature to 102°C, stir and react at this temperature for ...

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Abstract

The invention provides a synthesis method of 2, 2, 2', 4'-tetrachloroacetophenone, which effectively enhances the utilization ratio of the catalyst and promotes the reaction degree to be more thoroughby utilizing the temperature change and adding the catalyst in different time periods according to the proportion. Meanwhile, anhydrous aluminum trichloride is adopted as the catalyst, and the anhydrous aluminum trichloride is deposited on the high-stability carrier, so that the activity of the anhydrous aluminum trichloride is improved, the yield is increased, and the influence on the reaction degree due to the fact that the reaction rate is slowed down due to concentrated deposition of the catalyst in the reaction process is avoided; and besides, in the reaction process, the modified molecular sieve catalyst is used for carrying out directional isomerization treatment on the by-product, the treated modified molecular sieve catalyst has high stability and high selectivity, the p-dichlorobenzene by-product and the o-dichlorobenzene by-product in the reaction process are converted into the reaction raw material m-dichlorobenzene, the utilization rate of the raw material is increased, and the generation of the by-product is reduced.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, in particular to a method for synthesizing 2,2,2',4'-tetrachloroacetophenone. Background technique [0002] 2,2,2',4'-tetrachloroacetophenone is an important fine chemical intermediate, widely used in medicine, pesticide and other fields; such as: 2,2,2',4'-tetrachloro Acetophenone can be used to synthesize carcarb, chlorpyramid, etc. At present, most of the synthesis of 2,2,2',4'-tetrachloroacetophenone is based on m-dichlorobenzene and dichloroacetyl chloride, and the acetylation reaction is carried out under the catalysis of Lewis acid aluminum chloride to obtain 2 , 2,2',4'-Tetrachloroacetophenone. Although some enterprises have made great improvements in equipment and the use of rectification towers, which can achieve a certain increase in selectivity and yield, but the effect is still mediocre, and the amount of catalyst used remains high, which not only wastes resources, but als...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/46C07C49/80B01J27/125B01J27/224B01J27/24B01J29/40
CPCC07C45/46B01J27/125B01J27/24B01J27/224B01J29/40B01J29/405
Inventor 刘忠春
Owner JIANGXI YONGTONG TECH