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Preparation method of ethyl chloroformate

A technology of ethyl chloroformate and ethanol vapor, which is applied in the preparation of phosgene or haloformate, the purification/separation of carbonate/haloformate, organic chemistry, etc., which can solve the problem of increased side reactions, existence safety, etc. problems, to achieve the effect of reducing the occurrence of side reactions, improving efficiency and high product purity

Active Publication Date: 2020-09-22
XINYI AGRI CHEM PLANT JIANGSU PROV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Therefore, the technical problem to be solved in the present invention is to overcome the defects that the side reactions increase and there is safety in the existing ethyl chloroformate preparation process due to the excessive amount of phosgene, thereby providing a safe and reliable method with relatively high purity and yield. Preparation method of high ethyl chloroformate

Method used

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  • Preparation method of ethyl chloroformate
  • Preparation method of ethyl chloroformate
  • Preparation method of ethyl chloroformate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The present embodiment provides a kind of preparation method of ethyl chloroformate, comprises the following steps:

[0025] Into the tower reactor with built-in heat exchange, temperature measurement, vacuum device at the bottom and condensing device at the top, ethanol vapor and phosgene with a molar ratio of 1:1.05 are continuously introduced to control the internal pressure of the tower reactor The temperature is -80kPa, the temperature is 30℃~35℃, the gaseous ethyl chloroformate is liquefied by the condensation device and enters the receiving tank, the tail gas is absorbed by deionized water to prepare hydrochloric acid (concentration is about 30%), and the remaining light The gas is absorbed by dilute lye. After the reaction, weigh the product in the receiving tank.

[0026]

Embodiment 2

[0028] The present embodiment provides a kind of preparation method of ethyl chloroformate, comprises the following steps:

[0029] Into the tower reactor with built-in heat exchange, temperature measurement, vacuum device at the bottom and condensing device at the top, ethanol vapor and phosgene with a molar ratio of 1:1.05 are continuously introduced to control the internal pressure of the tower reactor The temperature is -60kPa, the temperature is 40℃~45℃, the gaseous ethyl chloroformate is liquefied by the condensation device and enters the receiving tank, the tail gas is absorbed by deionized water to prepare hydrochloric acid (concentration is about 30%), and the remaining light The gas is absorbed by dilute lye. After the reaction, weigh the product in the receiving tank.

[0030]

Embodiment 3

[0032] The present embodiment provides a kind of preparation method of ethyl chloroformate, comprises the following steps:

[0033] Into the tower reactor with built-in heat exchange, temperature measurement, vacuum device at the bottom and condensing device at the top, ethanol vapor and phosgene with a molar ratio of 1:1.05 are continuously introduced to control the internal pressure of the tower reactor The temperature is -40kPa, the temperature is 50℃~55℃, the gaseous ethyl chloroformate is liquefied by the condensation device and enters the receiving tank, the tail gas is absorbed by deionized water to prepare hydrochloric acid (concentration is about 30%), and the remaining light The gas is absorbed by dilute lye. After the reaction, weigh the product in the receiving tank.

[0034]

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of ethyl chloroformate. According to the preparation method of ethyl chloroformateprovided by the invention, ethyl chloroformate is prepared by adopting ethanol steam to replace liquid ethanol to react with phosgene, and the reaction conditions are as follows: the pressure is -90kPa to -5kPa, the temperature is 30-80 DEG C, and the molar ratio is 1: (1.00-1.05). Reactants are mixed in a gaseous form, and the contact area is increased, so that phosgene and ethanol can completelyreact under the condition of being close to a theoretical molar ratio, the phosgene dosage is reduced on the premise of ensuring the product yield, side reactions are reduced, and the product purityis improved.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of ethyl chloroformate. Background technique [0002] Ethyl chloroformate is mainly used as chemical solvent, amino protection agent and chemical products such as medicine and herbicide. Its molecular formula is CN20S0599A 3 h 5 CN20S0599AlO 2 , with a relative molecular mass of 108.53, is a colorless transparent liquid with a pungent odor, flammable, toxic and corrosive. [0003] The industrial synthesis of ethyl chloroformate is the esterification reaction of liquid ethanol and excess 5-20% phosgene, and then the final product is obtained through refining processes such as impurity removal, dehydration, and fractionation. In order to ensure a higher yield of ethyl chloroformate, the molar ratio of phosgene to liquid ethanol is generally controlled at a higher ratio, such as 10-15% excess phosgene. But along with the excessive amou...

Claims

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Application Information

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IPC IPC(8): C07C68/02C07C68/08C07C69/96
CPCC07C68/02C07C68/08C07C69/96
Inventor 耿斌李国鹏吴瑞磊孙新
Owner XINYI AGRI CHEM PLANT JIANGSU PROV