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Preparation method of trichloro allyl phosphate

A technology of trichloroallyl phosphate and allyl phosphate, applied in the direction of phosphorus organic compounds and the like, can solve the problems of trivial preparation of trichloroallyl phosphate, difficulty in meeting industrialized production, low utilization rate of raw materials, and the like, To achieve the effect of increasing the reaction rate, improving the utilization rate, and improving the production efficiency

Inactive Publication Date: 2014-12-03
宣城市聚源精细化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation of existing trichloroallyl phosphate is relatively cumbersome, and the utilization rate of raw materials is low, and there are many by-products, so it is difficult to meet the requirements of industrial production. Therefore, it is necessary to find a new preparation method of trichloroallyl phosphate

Method used

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Effect test

Embodiment 1

[0017] A preparation method of trichloroallyl phosphate, characterized in that: mainly comprising the steps:

[0018] (1) Catalyst tetrabutylammonium chloride, auxiliary agent, phosphorus oxychloride and propylene oxide are put into reactor successively, react at 5 ℃, get reaction solution after reaction completely; Wherein phosphorus oxychloride and The mol ratio of propylene oxide is 1: 0.8, and catalyst and auxiliary agent: the mol ratio of reaction solvent is all 1: 10;

[0019] (2) Wash the reaction solution with alkali and water to obtain a solution with a neutral pH;

[0020] (3) Dehydrate and concentrate the solution in step (2) to obtain trifilter allyl phosphate.

Embodiment 2

[0022] A preparation method of trichloroallyl phosphate, characterized in that: mainly comprising the steps:

[0023] (1) Catalyst tetrabutylammonium bromide, auxiliary agent, phosphorus oxychloride and propylene oxide are put into reactor successively, react at 10 ℃, get reaction solution after reaction completely; Wherein phosphorus oxychloride and The mol ratio of propylene oxide is 1: 1.2, and catalyst and auxiliary agent: the mol ratio of reaction solvent is all 1: 20;

[0024] (2) Wash the reaction solution with alkali and water to obtain a solution with a neutral pH;

[0025] (3) Dehydrate and concentrate the solution in step (2) to obtain trifilter allyl phosphate.

Embodiment 3

[0027] A preparation method of trichloroallyl phosphate, characterized in that: mainly comprising the steps:

[0028] (1) Put the catalyst crown ether, auxiliary agent, phosphorus oxychloride and propylene oxide into the reactor successively, react at 15°C, and get the reaction solution after the reaction is complete; wherein the mixture of phosphorus oxychloride and propylene oxide The molar ratio is 1: 1, catalyst and auxiliary agent: the molar ratio of reaction solvent is 1: 15;

[0029] (2) Wash the reaction solution with alkali and water to obtain a solution with a neutral pH;

[0030] (3) Dehydrate and concentrate the solution in step (2) to obtain trifilter allyl phosphate.

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PUM

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Abstract

The invention relates to a preparation method of trichloro allyl phosphate. The preparation method mainly comprises the following steps: (1) sequentially placing a catalyst, an auxiliary agent, phosphorus oxychloride and epoxy propane into a reaction kettle, reacting at 5-30 DEG C, and acquiring reaction liquid after the reaction is completed, wherein the mole ratio of the phosphorus oxychloride to the epoxy propane is (1 to 0.8)-(1 to 1.2), and the mole ratio of the catalyst to a reaction solvent and the mole ratio of the auxiliary agent to the reaction solvent are (1 to 10)-(1 to 20) respectively; (2) carrying out alkaline wash and water wash on the reaction liquid to obtain a solution with a neutral pH value; and (3) dehydrating and concentrating the solution obtained from the step (2) to obtain the trichloro allyl phosphate. The preparation method has the beneficial effects that the phosphorus oxychloride and the epoxy propane are utilized as raw materials, so that the reaction is more sufficient; the raw materials are effectively utilized, so that the utilization ratio of the raw materials is enhanced, and the production cost is reduced; the reaction rate is greatly enhanced by utilizing tetrabutylammonium chloride and tetrabutylammonium bromide or crown ether as the catalyst, so that the production efficiency is improved.

Description

technical field [0001] The invention relates to the technical field of chemical reagents, in particular to a preparation method of trichloroallyl phosphate. Background technique [0002] Trichloroallyl phosphate, as a class of important organic synthesis intermediates, not only has important uses in the synthesis of medicine and natural products, but also in the preparation of allyl ester prepolymers, allyl ester monomer modification Other unsaturated polyester resins have also been widely used. [0003] The existing preparation of trichloroallyl phosphate is cumbersome, and the utilization rate of raw materials is low, and there are many by-products, so it is difficult to meet the requirements of industrial production. Therefore, it is necessary to find a new preparation method of trichloroallyl phosphate. Contents of the invention [0004] The technical problem to be solved by the present invention is to overcome the existing technical defects and provide a preparation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09
Inventor 王伟英
Owner 宣城市聚源精细化工有限公司
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