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Preparation method for synthesizing isopropyl chloroformate through reaction of isopropanol and phosgene

A technology using isopropyl chloroformate and isopropanol, which is applied in the field of chemical synthesis, can solve the problems of low reaction rate, leakage and explosive accidents in the synthesis process, high phosgene reactivity, etc. The effect of air leakage

Pending Publication Date: 2021-09-17
上海祖玥新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional preparation method of isopropyl chloroformate is to add isopropanol in a phosgene kettle, start stirring, and then feed phosgene through a phosgene flowmeter. The reactivity of phosgene is too high. Leakage and explosive accidents are prone to occur in the medium, causing great harm to people and the environment, so the risk factor of this method is high; at the same time, the reaction rate of the traditional synthesis process is low, which affects the preparation efficiency

Method used

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Embodiment Construction

[0018] The invention provides a technical scheme: a preparation method for synthesizing isopropyl chloroformate using isopropanol and phosgene, comprising the following specific steps:

[0019] S1: Add an appropriate amount of solid phosgene to the flask, and add an appropriate amount of dichloromethane into the flask, stir to dissolve, and cool the solution to -3°C to -1°C;

[0020] S2: Add an appropriate amount of dimethylformamide to the above-mentioned cooled solution, keep the temperature at 3°C--1°C, and continue stirring for 20-30min to obtain a phosgene solution;

[0021] S3: Mix an appropriate amount of isopropanol with dichloromethane, and stir to obtain a mixed solution;

[0022] S4: Add the phosgene solution into the reaction kettle, start stirring, then set a dropping funnel above the reaction kettle, pour the mixed solution obtained in step S3 into the dropping funnel, open the valve of the dropping funnel, and control the leakage Speed, the mixed solution is ad...

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PUM

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Abstract

The invention belongs to the field of chemical synthesis, and particularly discloses a preparation method for synthesizing isopropyl chloroformate through reaction of isopropyl alcohol and phosgene, which comprises the following steps: adding a proper amount of solid phosgene into a flask, adding a proper amount of dichloromethane into the flask, and adding a proper amount of dimethylformamide into the cooled solution; then mixing a proper amount of isopropanol and dichloromethane, adding a phosgene solution into a reaction kettle, pouring the mixed solution into a dropping funnel, and adding the mixed solution into the reaction kettle under intense stirring for reaction. According to the invention, the triphosgene is used as a reactant, the dichloromethane is used as a solvent, the dimethylformamide is used as an initiator, and the triphosgene, the dichloromethane and the dimethylformamide are mixed with the dissolved triphosgene, so that the leakage of the triphosgene is effectively avoided, the safety is high, and the reaction rate is increased; then the isopropanol and dichloromethane are mixed and introduced into the dropping funnel, so that the reaction speed is convenient to control, the mixture is mixed with the phosgene solution under intense stirring, the reaction is sufficient and rapid, the operation is simple, the controllability is strong, and the synthesis efficiency is high.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method for synthesizing isopropyl chloroformate by reacting isopropanol and phosgene. Background technique [0002] Isopropyl chloroformate, also known as isopropionyl carbonyl, is a colorless and transparent liquid, generally present in 1.0mol / L isopropyl chloroformate toluene solution, nD1.485, relative density 0.892, and is irritating. Isopropyl chloroformate is mainly used as an initiator in the polymerization of polyvinyl chloride resin, and can also be used as a pesticide intermediate, ore flotation agent, etc.; it is also an intermediate of the fungicide Dimethocarb; it can also be used as a free radical polymerization reaction Initiator, such as the initiation of vinyl chloride polymerization. [0003] The traditional preparation method of isopropyl chloroformate is to add isopropanol in a phosgene kettle, start stirring, and then feed phosgene through a p...

Claims

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Application Information

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IPC IPC(8): C07C68/02C07C69/96
CPCC07C68/02C07C69/96
Inventor 王祖玥王磊
Owner 上海祖玥新材料科技有限公司
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