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Method for preparing 2-chloroethylphosphonic acid bis(2-chloroethyl)ester

A kind of technology of chloroethyl phosphine dichloride and chloroethyl phosphine dichloride by weight is applied in the field of preparation of 2-chloroethyl phosphonic acid diester, and can solve the problems of high reaction temperature, unsatisfactory yield, complicated post-processing and the like , to achieve the effect of high product purity, less side reactions and easy handling

Active Publication Date: 2015-02-25
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, there are various defects in the above methods
For example, when tris (2-chloroethyl) phosphite is used as a raw material, a large amount of heat will be released in the reaction, which needs to be removed in time. Rearrangement at high temperature has high reaction temperature, many side reactions, and low yield. Ideal and other deficiencies; when 2-chloroethylphosphonic dichloride is used as raw material to react with 2-chloroethanol, an additional acid-binding agent needs to be added, and the post-treatment is cumbersome

Method used

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  • Method for preparing 2-chloroethylphosphonic acid bis(2-chloroethyl)ester

Examples

Experimental program
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Effect test

Embodiment 1

[0017] In the dry reaction bottle, install mechanical stirring, thermometer, gas distributor and reflux condenser, place the reaction device in a low-temperature water bath, first use N 2 Replace the air in the bottle twice, add 100.00 g (0.550 mol) of freshly distilled 2-chloroethylphosphine dichloride under the protection of nitrogen, wait until the temperature in the bottle drops below 10°C, start stirring, and quantitatively introduce Ethylene oxide gas 50.88g (1.155mol), feed time about 10h, maintain the reaction temperature at 5-20°C, after feeding, keep the temperature at 30-40°C, continue the reaction for 3h, after the reaction, reduce the pressure The residual ethylene oxide was removed to obtain 146.00 g of the target product with a yield of 98.50% and a GC purity of 98.00%.

Embodiment 2

[0019] In the dry reaction bottle, install mechanical stirring, thermometer, gas distributor and reflux condenser, place the reaction device in a low-temperature water bath, and use N 2 Replace the air in the bottle twice, add 100.00 g (0.550 mol) of freshly distilled 2-chloroethylphosphine dichloride under the protection of nitrogen, wait until the temperature in the bottle drops below 10°C, start stirring, and quantitatively feed it through a gas distributor Ethylene oxide gas 49.67g (1.128mol), feed time about 10h, maintain the reaction temperature at 5-20°C, after feeding, keep the temperature at 30-40°C, continue the reaction for 3h, after the reaction, reduce the pressure The residual ethylene oxide was extracted to obtain 144.96 g of the target product, with a yield of 97.80% and a GC purity of 97.50%.

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Abstract

The invention discloses a method for preparing 2-chloroethylphosphonic acid bis(2-chloroethyl)ester. The method comprises the following steps of: adding ethylene oxide into 2-chloroethylphosphonic dichloride, reacting at the temperature of between 0 and 100DEG C for 8 to 18 hours, and removing residual ethylene oxide under reduced pressure to obtain a target product. The yield is more than or equal to 97 percent, the purity is more than or equal to 97.5 percent, the quality of the product is stable, and the product has a good application prospect.

Description

technical field [0001] The invention relates to a preparation method of 2-chloroethylphosphonic acid bis(2-chloroethyl). Background technique [0002] 2-Chloroethylphosphonic acid bis (2-chloroethyl) ester is mainly used for the production and preparation of the plant growth regulator ethephon, and it can be used as a flame retardant itself for the preparation of the flame retardant vinylphosphonic acid di (2-Chloroethyl) ester intermediate. In addition, 2-chloroethylphosphonic acid bis (2-chloroethyl) ester can also be used in the preparation of pharmaceutical resins, ion exchange resins, and fungicides, etc., and has broad market development prospects. [0003] In the prior art, 2-chloroethylphosphonic acid bis (2-chloroethyl) ester is mainly prepared by the reaction of phosphorus trichloride and ethylene oxide to obtain tris (2-chloroethyl) phosphite, the latter Rearrangement at high temperature is often divided into tank reaction with addition of solvent (o-dichloroben...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40
Inventor 刘斌赵林涛钱柯君林伟信廖本仁
Owner SHANGHAI HUAYI GRP CO
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