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Treatment method of ethyl chloroformate rectifying still residues

A technology of ethyl chloroformate and treatment method, which is applied in the field of waste treatment in chemical production, and can solve the problems of not providing phosgene treatment scheme and low quality of diethyl carbonate

Pending Publication Date: 2021-11-26
NINGXIA RUITAI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The application provides a treatment method for ethyl chloroformate rectification still residue, which solves the problem that the phosgene method of ethyl chloroformate rectification still residue treatment scheme is not provided in the prior art, and diethyl carbonate is produced as a by-product after simple rectification. Problems such as low ester quality

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  • Treatment method of ethyl chloroformate rectifying still residues
  • Treatment method of ethyl chloroformate rectifying still residues
  • Treatment method of ethyl chloroformate rectifying still residues

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] To the 500L reactor, oxycetate is 300 kg of chloroformate, 45kg of ethyl chloroformate, stirring, and 38.33 kg of anhydrous ethanol, ethanol and othyl chloroformate, to 2: 1. The temperature rose to 60 ° C, the reaction time is 5h. The synthesis liquid was removed under 10 kPa, and the top of the column was removed and a small amount of light components, and the top of the column was substantially uncondensation, and the ethanol content of the tower is 0.2%. The tower is distilled into the molecular distiller at a certain speed, and the light component, the diethyl carbonate primary fraction and the recombination are collected. The molecular distillation apparatus is 10 Pa, the temperature is 80 ° C, the material residence time is 30s; the diethyl carbonate is 99.97%, and the remaining indicators satisfy the high-pure level quality index, the diethyl carbonate is 85.2%.

Embodiment 2

[0037]In Example 1 was investrated in Example 1 in Example 1 300 kg (lower), 25kg of chloroformate, mixed with ethyl chloroformate, stirred, and 0.2 kg of anhydrous ethanol, ethanol and chloroform acid. Ethyl ester mol ratio was 1: 1; heated to 70 ° C, the reaction time was 8 h. The synthesis liquid was removed under 100 kPa, and a small amount of light components were taken to the top of the tower, and the tower is basically uncondensible, and the ethanol content of the tower is 0.05%. The tower is distilled into the molecular distiller at a certain speed, and the light component, the diethyl carbonate primary fraction and the recombination are collected. The molecular distillation device is vacuum having a vacuum having a temperature of 70 ° C, and the material residence time is 100 s; the diethyl carbonate is 99.95%, and the remaining index satisfies the quality index requirements of excellent quality, the diethyl carbonate yield is 80.3%.

Embodiment 3

[0039] In Example 1 in Example 1 was 300 kg of ethyl chloroformate in Example 1, 45 kg of ethyl chloroformate was converted, and 192 kg of anhydrous ethanol was added to the kettle, ethanol and chloroformate MOL ratio. 10: 1; heated to 80 ° C, the reaction time was 4 h. The synthesis liquid was removed under 20 kPa, and the top of the tower was subjected to excess ethanol and a small amount of light components, and the top of the tower was basically removed, and the ethanol content of the tower was 0.13%. The tower is distilled into the molecular distiller at a certain speed, and the light component, the diethyl carbonate primary fraction and the recombination are collected. The molecular distillation apparatus is vacuum is 20 Pa, temperature 90 ° C, the material residence time is 200 s; the primary fraction of diethyl carbonate is 99.99%, and the remaining index satisfies the electronic level mass index requirements, the diethyl carbonate yield is 83.3%.

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Abstract

The invention discloses a method for treating ethyl chloroformate rectifying still residues. The ethyl chloroformate rectifying still residues are further reacted with ethanol, so that ethyl chloroformate in the still residues can be basically reacted completely, the content of diethyl carbonate is increased, the components of the still residues are relatively single, and preparation of high-quality diethyl carbonate is facilitated. The residues subjected to ethanol treatment are subjected to continuous molecular distillation after desolvation and ethanol removal, the system temperature is low, the retention time is short, the heating time of diethyl carbonate is short, and the chromaticity, content, stability and the like of the product are remarkably superior to those of a traditional rectification process. The ethyl chloroformate rectifying still residues are subjected to effective resourceful treatment, high-quality diethyl carbonate is obtained, the amount of three wastes is greatly reduced, and the added value of the product is improved.

Description

Technical field [0001] The present application relates to the field of waste treatment in chemical production, and more particularly to the treatment of ethyl chloroformate. Background technique [0002] Ethyl chloroformate, for colorless transparent liquid, mainly used as an intermediate, organic synthesis, chemical solvent, production medicine and herbicide (Pioneer 5), tetrazole Acetic acid, 嘧磺, etc., can also be used as a solvent and an amino protector. Diethyl carbonate is used in chemical production for solvents for nitrocellulose, synthetic resins, and natural resins for producing pyrethroid, sealed fixation, and the like, high purity carbonate dieter is mainly used for lithium ion battery electrolytes. [0003] At present, the preparation method of ethyl chloroformate is mainly synthesized from ethanol and phylogenetic tower, synthetic liquid, reflarmed, refilled. In the synthesis, a small amount of chloroformate is a side reaction with the raw material ethanol, further r...

Claims

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Application Information

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IPC IPC(8): C07C68/00C07C68/08C07C69/96
Inventor 严绘石苏洋王明晨侯嘉韩小文李梅马荣慧殷恒志
Owner NINGXIA RUITAI TECH
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