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Synthetic method of phenyl chloroformate by taking phenol as raw material

A technology for the synthesis of phenyl chloroformate, which is applied in the preparation of phosgene or haloformate, organic chemistry, etc., can solve the problems of low production efficiency, achieve the effects of avoiding poisonous gas, avoiding waste water, and improving purity

Active Publication Date: 2016-11-09
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, phenol can produce by-product diphenyl carbonate (DPC) under the condition of high temperature and acid-binding agent with product phenyl chloroformate ,Right now

Method used

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  • Synthetic method of phenyl chloroformate by taking phenol as raw material

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Experimental program
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Effect test

Embodiment 1

[0021] First, add 94Kg phenol in the molten state in the phenol dropping tank, first open the A and B circulation refrigerators connected to the reaction tank, lower the temperature of the lower part of the reaction tank to 0 ° C, then add triphosgene to the lower part of the reaction tank, and The add-on of triphosgene is 299Kg, simultaneously in retort inner bottom, adds catalyzer, and the reaction time is 7 hours, gets middle control sample, gas phase normalization analyzes the area percentage of phenyl chloroformate and main by-product diphenyl carbonate; Next, Extract the above-mentioned central control sample once every 1 hour, so that step 3 continues to react until the area percentage of phenyl chloroformate and the main by-product diphenyl carbonate no longer increases, and the number of extractions is 10 times; again, the reaction tank after the above-mentioned extraction is used nitrogen gas After degassing, the tail gas is passed into the phosgene decomposition towe...

Embodiment 2

[0026] Add 94Kg phenol in the molten state to the phenol dropping tank, first turn on the A and B circulation refrigerators connected to the reaction tank, lower the temperature of the lower part of the reaction tank to 0 ° C, and then add triphosgene to the lower part of the reaction tank, and triphosgene The add-on of chloroformate is 297Kg, simultaneously adds catalyzer to the lower part in the retort, and the reaction time is 7 hours, gets in control sample, gas phase normalization analyzes the area percent of chloroformic acid phenyl ester and main by-product diphenyl carbonate; Next, above-mentioned The central control sample is extracted once every 1 hour, so that step 3 continues to react until the area percentage of phenyl chloroformate and the main by-product diphenyl carbonate no longer increases, and the number of extractions is 10 times; again, the reaction tank after the above extraction is purged with nitrogen gas Finally, pass the tail gas into the phosgene deco...

Embodiment 3

[0031] Add 94Kg phenol in the molten state to the phenol dropping tank, first turn on the A and B circulation refrigerators connected to the reaction tank, lower the temperature of the lower part of the reaction tank to 0 ° C, and then add triphosgene to the lower part of the reaction tank, and triphosgene The add-on of chloroformate is 298Kg, simultaneously adds catalyzer to bottom in reaction tank, and the reaction time is 7 hours, gets middle control sample, gas phase normalization analyzes the area percentage of phenyl chloroformate and main by-product diphenyl carbonate; Next, above-mentioned The central control sample is extracted once every 1 hour, so that step 3 continues to react until the area percentage of phenyl chloroformate and the main by-product diphenyl carbonate no longer increases, and the number of extractions is 10 times; again, the reaction tank after the above extraction is purged with nitrogen gas Finally, pass the tail gas into the phosgene decompositio...

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Abstract

The invention provides a synthetic method of phenyl chloroformate by taking phenol as a raw material. The method comprises the following steps: processing 94 Kg of phenol to a fusion state for standby; transferring the above phenol to a phenol addition pot, transferring a catalyst to a catalyst spraying pot; reducing the temperature at the bottom of a reaction pot to 0 DEG C, then adding triphosgene to the bottom of the reaction pot; finally employing nitrogen for expelling gas for the above reaction pot, and performing underpressure distillation to obtain phenyl chloroformate. The method can avoid the generation of a by-product diphenyl carbonate, avoids waste water generation, and further increases the purity of the product phenyl chloroformate.

Description

technical field [0001] The invention relates to the production field of fine chemicals, in particular to a method for synthesizing phenyl chloroformate using phenol as a raw material. 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 ...

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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