Phenyl chloroformate production technique

A technology of phenyl chloroformate and production process, applied in the field of production technology of phenyl chloroformate, can solve problems such as low production efficiency, and achieve the effects of being easy to control, improving purity, and shortening reaction time

Active Publication Date: 2016-09-21
ANHUI GUANGXIN AGROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] But existing technology also has by-product production, and production efficiency is also relatively low simultaneously, promptly in production process, p

Method used

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  • Phenyl chloroformate production technique

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] First, slowly raise the temperature of the stirring tank to 100°C, then pass phosgene into the stirring tank from the middle part of the side wall of the stirring tank, and the amount of phosgene introduced is 60mol, and keep feeding phosgene continuously, then Open the phenol dripping tank, start stirring and open the catalyst spray tank at the same time, and the speed of adding phenol is 70-140L / h, when the reaction time is 2 hours, take the central control sample, and analyze the phenyl chloroformate and the main The area percentage of by-product diphenyl carbonate;

[0023] Next, continue to pass into phosgene again, the rate of dripping phenol is 30L / h, when the reaction time is 4 hours, take the central control sample, and analyze the area percentage of phenyl chloroformate and main by-product diphenyl carbonate by gas phase normalization ;

[0024] Again, continue to extract the above-mentioned central control sample for 30 minutes, so that the above-mentioned c...

Embodiment 2

[0030] First, slowly raise the temperature of the stirring tank to 99°C, then pass phosgene into the stirring tank from the middle part of the side wall of the stirring tank, and the feeding amount of phosgene is 50mol, and keep feeding phosgene continuously, then Open the phenol dripping tank, start stirring and open the catalyst spray tank at the same time, and the speed of adding phenol is 70-140L / h, when the reaction time is 2 hours, take the central control sample, and analyze the phenyl chloroformate and the main The area percentage of by-product diphenyl carbonate;

[0031] Secondly, continue to feed phosgene, add phenol at a rate of 31L / h, and when the reaction time is 4 hours, take a control sample and analyze the area percentage of phenyl chloroformate and the main by-product diphenyl carbonate by gas phase normalization ;

[0032] Again, continue to extract the above-mentioned central control sample once for 30 minutes, so that the above-mentioned continued reactio...

Embodiment 3

[0039] First, slowly raise the temperature of the stirring tank to 101°C, then pass phosgene into the stirring tank from the middle of the side wall of the stirring tank, and the amount of phosgene introduced is 50mol, and keep feeding phosgene continuously, then Open the phenol drop tank, start the stirring and catalyst spray tank at the same time, and add phenol at a rate of 70L / h, and when the reaction time is 2 hours, take the central control sample, and analyze the phenyl chloroformate and the main by-products by gas phase normalization Area percentage of diphenyl carbonate;

[0040]Next, continue to pass into phosgene again, the speed of dropping phenol is 32L / h, and when the reaction time is 4 hours, take the control sample, and analyze the area percentage of phenyl chloroformate and the main by-product diphenyl carbonate by gas phase normalization ;

[0041] Again, continue to extract the above-mentioned central control sample for 30 minutes, so that the above-mention...

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Abstract

The invention provides a phenyl chloroformate production technique. The technique comprises the steps of firstly, slowly increasing the temperature of a stirring tank, then introducing phosgene constantly into the stirring tank from the middle of the side wall of the stirring tank, opening a phenol dropwise adding tank, and opening the stirring tank and a catalyst spray tank at the same time; secondly, continuing to introduce phosgene, and taking a central control sample; thirdly, continuously extracting the central control sample every other 30 min; fourthly, conducting air expelling with nitrogen on the stirring tank after final sampling is stopped; finally, conducting reduced pressure distillation on materials left after air expelling to obtain phenyl chloroformate. Compared with the prior art, the production technique has the advantages that reaction time is shortened, and purity and reaction efficiency are improved.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a production process of phenyl chloroformate. Background technique [0002] Phenyl chloroformate is an important fine chemical intermediate, which is widely used in chemical synthesis and can be used as a polymerization catalyst, plastic modifier, fiber treatment agent, and intermediate of medicine and pesticide. [0003] The main synthesis method of phenyl chloroformate is the phosgene method. Dissolve phenol in chloroform, pass through phosgene under cooling, make the ratio of the absorbed phosgene amount to phenol and other substances, and add other substances dropwise under stirring at 5-10°C The amount of N,N-dimethylaniline. Then dilute with cold water, separate the oil layer, and wash with dilute hydrochloric acid and water successively. After drying with anhydrous calcium chloride, distill to recover chloroform, and then rectify under reduced pressure to collect the fracti...

Claims

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Application Information

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IPC IPC(8): C07C68/02C07C69/96
CPCC07C68/02C07C69/96
Inventor 黄金祥过学军吴建平胡明宏杨亚明程伟家李红卫徐小兵高焰兵戴玉婷
Owner ANHUI GUANGXIN AGROCHEM
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