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Method for preparing methyl chloroacetate

A technology of methyl chloroacetate and chloroacetic acid is applied in the field of esterification synthesis technology, which can solve the problems of high process energy consumption, low content of methyl chloroacetate, complicated rectification process, etc., and achieves simple production process and saving methanol consumption. , the effect of high product purity

Inactive Publication Date: 2014-11-19
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This will not only increase the neutralization process, but also use a large amount of alkali, and cause ester, salt, alkali, and water paste due to more alkali and less water, which increases the difficulty of separation.
The content of methyl chloroacetate obtained in this way is only about 80%. It is used as a solvent, which often leads to abnormal production of dimethyl phosphite, and sometimes the whole batch of feed liquid is scrapped.
The loss of methyl chloroacetate after neutralization reaches as much as 30% in each batch, and the yield is naturally very low
This process requires high energy consumption, the reaction temperature needs to be above 120°C, and the loss of chloroacetic acid is relatively large, the content of methyl chloroacetate is low, the post-treatment rectification process is complicated, and it causes secondary pollution and serious waste discharge.

Method used

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  • Method for preparing methyl chloroacetate
  • Method for preparing methyl chloroacetate

Examples

Experimental program
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Effect test

Embodiment example 1

[0030] New method flow chart of the present invention sees figure 1 , chloroacetic acid and methanol are stirred and mixed at room temperature in the raw material tank 1 according to the molar ratio of 1:1, and are injected into the bottom of the fixed-bed reactor 3 through the raw material pump 2, and the catalyst is filled in the fixed-bed reactor, and the loading amount is about 2 / 3 of the reactor volume. The reaction temperature is controlled at 80°C, and the gas-phase mixed product is condensed by the condenser at the top of the reactor, and then enters the primary ester-water separator, and the content of each component in the upper and lower layers is detected by gas chromatography. Open the water supply valve of the primary ester-water separator to replenish water for primary extraction, and use gas chromatography to detect the content of each component in the upper and lower layers. The conversion rate of chloroacetic acid was measured to be 80%, and the selectivity ...

Embodiment example 2

[0032] New method flow chart of the present invention sees figure 1 , Chloroacetic acid and methanol are stirred and mixed at room temperature in the raw material tank 1 according to the ratio of 1:2, and injected into the bottom of the fixed-bed reactor 3 through the raw material pump 2, and the catalyst is filled in the fixed-bed reactor, and the loading amount is about 2 / 3 of the container volume. The reaction temperature is controlled at 90°C, and the gas-phase mixed product is condensed by the condenser 4 at the top of the reactor, and then enters the primary ester-water separator 5, and the content of each component in the upper and lower layers is detected by gas chromatography. The conversion rate of chloroacetic acid was measured to be 90%, and the selectivity was 100%. Open the first-stage ester-water separator 5 water supply valve to replenish water for primary extraction, and use gas chromatography to detect the content of each component in the upper and lower lay...

Embodiment example 3

[0034] New method flow chart of the present invention sees figure 1 , chloroacetic acid and methanol are stirred and mixed at room temperature in the raw material tank 1 according to the ratio of 1:1.5, and then injected into the bottom of the fixed-bed reactor 3 through the raw material pump 2, and the catalyst is filled in the fixed-bed reactor. 2 / 3 of the container volume. The reaction temperature is controlled at 120°C, and the gas-phase mixed product is condensed by the condenser 4 at the top of the reactor, and then enters the primary ester-water separator 5, and the content of each component in the upper and lower layers is detected by gas chromatography. The conversion rate of chloroacetic acid was measured to be 98%, and the selectivity was 100%. Open the first-stage ester-water separator 5 water supply valve to replenish water for primary extraction, and use gas chromatography to detect the content of each component in the upper and lower layers. The lower layer en...

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Abstract

The invention relates to a novel method for preparing methyl chloroacetate. The method is characterized in that resin modified by acidic ionic liquid is taken as a catalyst and a section of fixed bed reactor is just adopted for completing the method; no aqueous solution needs to be added in the preparation process; the method is low in reaction temperature, simple in flow, low in investment cost and low in energy consumption; the conversion rate of the methyl chloroacetate is above 99.5% and the selectivity of the methyl chloroacetate is 100%.

Description

[0001] Technical field: the present invention relates to a new method for preparing methyl chloroacetate, which belongs to the technical field of esterification reaction synthesis technology. Background technique: [0002] Methyl chloroacetate is widely used in the production of pesticides, medicines, plastics, dyes, rubber, leather, cosmetics and other products. It is an important intermediate of medicine and pesticide. Due to the importance of methyl chloroacetate and its considerable economic benefits, some small and medium-sized enterprises have produced methyl chloroacetate one after another in recent years. [0003] The esterification reaction of chloroacetic acid and methanol to form methyl chloroacetate is a reversible reaction like other esterification reactions: [0004] [0005] This reaction is a reversible equilibrium reaction. Only by increasing the concentration of methanol or removing the reaction product can the conversion of chloroacetic acid into methyl ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/08
CPCC07C67/08C07C69/63
Inventor 张娟胡颜荟梁润娟韩军兴闫瑞一张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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