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Ethyl chloroacetate synthesis method and device

A technology of ethyl chloroacetate and synthesis method, which is applied in the field of synthesis method and device of ethyl chloroacetate, can solve the problems of low molar yield, low production efficiency, waste of resources, etc., and achieve high molar yield and high production efficiency , the effect of saving resources

Pending Publication Date: 2021-06-22
宁夏森萱药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The application provides a synthetic method of ethyl chloroacetate, which solves the problem that the synthetic method of ethyl chloroacetate in the prior art cannot be continuously produced so that the production efficiency is low, and the waste of resources is caused after the reaction liquid is directly discharged, and the molar yield lower question

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] A kind of synthetic method of ethyl chloroacetate, comprises the following steps:

[0023] S1: Mix chloroacetic acid and ethanol at a ratio of 1:1.05 and add them into the esterification reactor for reaction. The top temperature of the esterification reactor is 105℃~115℃, and the liquid level in the esterification reactor is 70~ 75%, the temperature inside the esterification reactor is 120℃~135℃, the output of the esterification reactor is 300~350L / hour, the molar ratio of chloroacetic acid and ethanol is 1:1~1.1, after the reaction, Crude ethyl chloroacetate;

[0024] S2: Separating the crude ethyl chloroacetate from oil and water to obtain crude esters, rectifying the crude esters to obtain ethyl chloroacetate and ethanol liquid, and recovering the ethanol liquid into the esterification reaction kettle.

Embodiment 1

[0025] Example 1: Open and adjust the cooling water of the tower top condenser of the esterification reactor through the DCS control system, the opening of the cooling water adjustment valve is interlocked with the temperature at the top of the esterification reactor, and the temperature at the top of the esterification reactor is controlled at 108 ℃. When the liquid level in the esterification reactor drops to 70%, the feed regulating valve of the chloroacetic acid / ethanol mixed solution is opened through the DCS control system, and the opening of the feed regulating valve is interlocked with the liquid level in the esterification reactor to make the reactor The internal liquid level is maintained at 71%; the opening of the steam valve is adjusted through the DCS control system, and the steam regulating valve is interlocked with the temperature of the reactor to keep the temperature of the reactor at 125°C. Open the discharge valve of the esterification reactor tower through ...

Embodiment 2

[0028] Embodiment 2: Open and adjust the cooling water of the tower top condenser of the esterification reactor through the DCS control system, the opening of the regulating valve of the cooling water is interlocked with the temperature at the top of the esterification reactor, and the temperature at the top of the esterification reactor is controlled at 110 ℃. When the liquid level in the esterification reactor drops to 70%, the feed regulating valve of the chloroacetic acid / ethanol mixed solution is opened through the DCS control system, and the opening of the feed regulating valve is interlocked with the liquid level in the esterification reactor to make the reactor The internal liquid level is maintained at 73%; the opening of the steam valve is adjusted through the DCS control system, and the steam regulating valve is interlocked with the temperature of the reactor to keep the temperature of the reactor at 130°C. Open the discharge valve of the esterification reactor towe...

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PUM

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Abstract

The invention discloses an ethyl chloroacetate synthesis method which comprises: S1, uniformly mixing chloroacetic acid and ethanol according to a ratio of 1: 1.05, adding into an esterification reaction kettle, and carrying out a reaction according to the molar ratio of the chloroacetic acid to the ethanol of 1: 1-1.1 to obtain an ethyl chloroacetate crude product; and S2, carrying out oil-water separation on the ethyl chloroacetate crude product to obtain crude ester, rectifying the crude ester to obtain ethyl chloroacetate and an ethanol solution, and recovering the ethanol solution into the esterification reaction kettle. The synthesis method solves the problems of low production efficiency caused by incapability of continuous production in the synthesis method of ethyl chloroacetate in the prior art, resource waste caused by direct discharge of the reaction liquid, and low molar yield.

Description

technical field [0001] This application relates to, relate in particular to a kind of synthetic method and device of ethyl chloroacetate. Background technique [0002] Ethyl chloroacetate is an important intermediate for the synthesis of medicines, pesticides and spices, and can also be used as an industrial solvent. Ethyl chloroacetate is obtained by esterification of chloroacetic acid and ethanol under the catalysis of sulfuric acid. In the synthesis process, chloroacetic acid, ethanol and catalyst are added into the esterification pot for stirring, heating, distillation and other reactions to obtain the finished product ethyl chloroacetate. However, this synthetic method cannot be continuously produced so that the production efficiency is low, and the reaction solution is directly discharged to cause waste of resources, and the molar yield is low. [0003] For this reason, the application provides a kind of synthetic method and the device of ethyl chloroacetate to solve...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C67/54C07C69/63G05D27/02
CPCC07C67/08C07C67/54G05D27/02C07C69/63
Inventor 林国平孙冬兵尹建炉
Owner 宁夏森萱药业有限公司