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Reactive distillation method for preparing methyl chloroacetate

A technology of methyl chloroacetate and reactive distillation, which is applied in the field of reactive distillation for preparing methyl chloroacetate, can solve the problems of high process energy consumption, secondary pollution, complicated distillation process, etc., and achieves simple production process, No secondary pollution, high product purity

Inactive Publication Date: 2015-05-06
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

Moreover, due to more alkali and less water, esters, salts, alkalis, and water pastes are formed, 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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  • Reactive distillation method for preparing methyl chloroacetate
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Examples

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Effect test

Embodiment example 1

[0031] New method flow chart of the present invention sees figure 1 , chloroacetic acid and methanol are stirred and mixed in the raw material tank 1 at 25°C according to the molar ratio of 0.3:1, and injected into the top of the reaction section of the reactive distillation tower through the raw material pump 3, and the middle part of the reactive distillation tower is pyridine trifluoromethanesulfonate The acid polymerization ionic liquid catalyst and filler are mixed, and the upper layer and the lower layer are equipped with seasoning. The temperature of the tower bottom is controlled at 120°C, and the temperature of the tower body is controlled at 110°C. The gas-phase mixed product is condensed by the condenser at the top of the reactor, and then enters the ester-water separator, and the content of each component in the upper and lower layers is detected by gas chromatography. The lower layer is divided into two paths, part of which flows back to the top of the tower with...

Embodiment example 2

[0033] New method flow chart of the present invention sees figure 1 , chloroacetic acid and methanol are stirred and mixed in the raw material tank 1 at 25°C according to the molar ratio of 0.4:1, and injected into the top of the reaction section of the reactive distillation tower through the raw material pump 3, and the middle part of the reactive distillation tower is pyridine trifluoromethanesulfonate The acid polymerization ionic liquid catalyst and filler are mixed, and the upper layer and the lower layer are equipped with seasoning. The temperature of the tower bottom is controlled at 125°C, and the temperature of the tower body is controlled at 115°C. The gas-phase mixed product is condensed by the condenser at the top of the reactor, and then enters the ester-water separator, and the content of each component in the upper and lower layers is detected by gas chromatography. The lower layer is divided into two paths, part of which flows back to the top of the tower with...

Embodiment example 3

[0035] New method flow chart of the present invention sees figure 1 , chloroacetic acid and methanol are stirred and mixed in the raw material tank 1 at 25°C according to the molar ratio of 0.5:1, and injected into the top of the reaction section of the reactive distillation tower through the raw material pump 3, and the middle part of the reactive distillation tower is pyridine trifluoromethanesulfonate The acid polymerization ionic liquid catalyst and filler are mixed, and the upper layer and the lower layer are equipped with seasoning. The temperature of the tower bottom is controlled at 130°C, and the temperature of the tower body is controlled at 120°C. The gas-phase mixed product is condensed by the condenser at the top of the reactor, and then enters the ester-water separator, and the content of each component in the upper and lower layers is detected by gas chromatography. The lower layer is divided into two paths, part of which flows back to the top of the tower with...

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Abstract

The invention relates to a new method for preparing methyl chloroacetate. The method is characterized in that chloroacetic acid and methanol are used as raw materials, a reactive distillation tower is adopted, and a pyridine trifluoromethanesulfonic acid polymeric ion liquid catalyst is used as mixed filler in a reaction section to perform gas-liquid-solid three-phase reaction. The reaction can be finished by adopting a one-section reactive distillation reactor, a water carrying agent does not need to be added in the process, the reaction temperature is low, the flow is simple, the investment cost is reduced, the energy consumption is low, the conversion rate is more than 99.5%, and the selectivity is 100%.

Description

[0001] Technical field: the invention belongs to the technical field of chemical industry, and relates to a reactive distillation method for preparing methyl chloroacetate. 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 ester be promoted a...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/08C07C67/54
CPCC07C67/08C07C67/54C07C69/63Y02P20/10
Inventor 张娟梁润娟莫显恩张国帅胡颜荟闫瑞一张锁江
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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