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Synthesis method of methyl phosphorus dichloride

A technology of methylphosphorus dichloride and a synthesis method, applied in the field of organophosphorus chemical synthesis, can solve problems such as occupational injury, the irritation of toxic chloroform, etc., and achieve the effect of small safety risk

Active Publication Date: 2016-06-15
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are technical problems that are difficult to solve in industrialization. The ligands prepared by this method need to be filtered and transferred to reduction analysis to obtain methyl phosphorus dichloride. It is difficult to avoid the fugitive emission of organic waste gas during the solid-liquid separation process, especially It is tetrachloroethane with a high boiling point, which is toxic and irritating to chloroform, and is likely to cause occupational injuries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] This example proposes a synthesis method of methyl phosphorus dichloride, using methyl chloride, aluminum trichloride and phosphorus trichloride as raw materials, and using petroleum ether as a solvent to generate ligand CH 3 PCl 4 ·AlCl 3 After distilling and recovering petroleum ether, adding aluminum powder and sodium chloride, under the action of a catalyst, reducing to obtain the product methyl phosphorus dichloride.

Embodiment 2

[0028] On the basis of Example 1, this example is further limited. Petroleum ether and phosphorus trichloride are added to the reaction kettle. After stirring, aluminum trichloride and methyl chloride are added, and the ligand CH is generated after stirring. 3 PCl 4 ·AlCl 3 .

Embodiment 3

[0030] On the basis of embodiment 2, the present embodiment defines that the reactor satisfies:

[0031] Before feeding, evacuate to reach a pressure of <10Pa, and fill with nitrogen after removing all the air;

[0032] After feeding, the reaction temperature is controlled at normal temperature, and the reaction pressure is controlled at 0.02MPa.

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PUM

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Abstract

The invention discloses a synthesis method of methyl phosphorus dichloride. According to the synthesis method, methyl chloride, aluminum trichloride and phosphorus trichloride serve as raw materials, petroleum ether serves as a solvent, ligands CH3PCl4.AlCl3 are generated through reaction, after petroleum ether is recycled through distillation, aluminum powder and petroleum ether are added, and the methyl phosphorus dichloride is obtained through reduction under the action of a catalyst. The synthesis method of methyl phosphorus dichloride can replace an existing technology to solve the problem of emission of organic waste gas in the preparation process, and the method is a complete synthesis technology process according with the clean production principle better. Besides, compared with the prior art, the synthesis method has a better production effect, and in other words, the yield of the methyl phosphorus dichloride can reach 91% (denoted by phosphorus dichloride).

Description

technical field [0001] The invention relates to a method for synthesizing methylphosphorous dichloride, in particular to a method for synthesizing an important organophosphorus intermediate, methylphosphorous dichloride, and belongs to the technical field of organophosphorus chemical synthesis. Background technique [0002] Methyl phosphorus dichloride is an intermediate for the synthesis of organophosphorus compounds and an important intermediate for the herbicide glufosinate. Glufosinate-ammonium is an ideal herbicide for transgenic resistant crops, with the characteristics of high efficiency, low toxicity and broad herbicidal spectrum. With the rapid development of genetically modified crops, such as genetically modified glufosinate-resistant rice and genetically modified glufosinate-resistant soybeans, the market demand for glufosinate is also increasing rapidly. Methyl phosphorus dichloride is active in chemical properties, easily reacts with water and oxygen in the ai...

Claims

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Application Information

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IPC IPC(8): C07F9/52
CPCC07F9/509C07F9/52
Inventor 姜永红廖霞罗均
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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