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A kind of synthetic method of methylphosphorus dichloride

A technology of methyl phosphorus dichloride and a synthesis method, which are applied in the synthesis of methyl phosphorus dichloride and the synthesis field of glufosinate-ammonium intermediate methyl phosphorus dichloride, can solve the problem of difficult to realize industrialized production and reduce solid side effects. products, increasing the amount of solid waste generated, etc., to achieve the effect of reducing the amount of production, reducing production costs, and improving utilization.

Active Publication Date: 2021-05-14
NANJING HUAZHOU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to add additional aluminum powder to reduce the ternary complex of +5 valence P, and the aluminum trichloride produced by the oxidation of aluminum powder has not been effectively utilized, and the generation of solid waste has been greatly increased, which is difficult Realize industrial production
Patent CN105669748A has improved this method, using petroleum ether as a solvent, adding diethyl phthalate and other catalysts to increase the yield to 91%, and an average of 1t of methyl phosphorus dichloride will produce 3t of solid waste substances, but also failed to avoid or reduce solid by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add aluminum trichloride, aluminum powder and phosphorus trichloride in a closed reaction kettle according to the molar ratio of 1:2:4, add dichloromethane twice the mass of the total mass of the material as a solvent, vacuumize to remove the air, and stir evenly Introduce methyl chloride in an amount five times that of aluminum trichloride, heat the material to 85°C, and then inert nitrogen to pressurize to 0.5MPa. The reaction was stopped after 6 hours, and the temperature was raised to 100-120°C for distillation under reduced pressure to fully remove the solvent and unreacted phosphorus trichloride.

[0026] After the ternary complex is heated to 150°C, sodium chloride is added, and distilled while reacting to obtain methyl phosphorus dichloride with a purity of 99.6% and a yield of 91.2%.

Embodiment 2

[0028] Add aluminum trichloride, aluminum powder and phosphorus trichloride in a closed reactor according to the molar ratio of 1:2.1:3, add dichloromethane twice the mass of the total mass of the material as a solvent, vacuumize to remove the air, and stir evenly Introduce methyl chloride in an amount three times that of aluminum trichloride, heat the material to 85°C, and inert nitrogen to pressurize to 1.0MPa. The reaction was stopped after 6 hours, and the temperature was raised to 100-120°C for distillation under reduced pressure to fully remove the solvent and unreacted phosphorus trichloride.

[0029] After the ternary complex is heated to 150°C, sodium chloride is added, and distilled while reacting to obtain methyl phosphorus dichloride with a purity of 99.8% and a yield of 90.6%.

Embodiment 3

[0031] Add aluminum trichloride, aluminum powder and phosphorus trichloride in a closed reactor according to the molar ratio of 1:1.9:8, add dichloromethane twice the mass of the total mass of the material as a solvent, vacuumize to remove the air, and stir evenly Feed in chloromethane in an amount 8 times that of aluminum trichloride, heat the material to 95°C, and then feed inert nitrogen to pressurize to 0.3 MPa. The reaction was stopped after 5 hours, and the temperature was raised to 100-120°C for distillation under reduced pressure to fully remove the solvent and unreacted phosphorus trichloride.

[0032] After the ternary complex is heated to 150°C, sodium chloride is added, and distilled while reacting to obtain methyl phosphorus dichloride with a purity of 98.3% and a yield of 91.1%.

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Abstract

The invention relates to a new method for synthesizing glufosinate-ammonium intermediate methyl phosphorus dichloride. The method is realized by the following technical scheme: using aluminum powder, aluminum trichloride, methyl chloride and phosphorus trichloride as raw materials , under the pressure of 0.3-1.0MPa, the ternary complex of +3-valent phosphorus is directly obtained through one-step reaction for 3-6h, then sodium chloride is added, and the reaction is carried out at 150 ° C to obtain methyl phosphorus dichloride. In the synthesis method adopted in the invention, aluminum powder and aluminum trichloride are used as reaction raw materials at the same time, and the yield in terms of aluminum element can reach 90%, the utilization rate of aluminum is improved, and the ternary complex reaction and ligand reduction are reduced. The combination of the two-step reaction simplifies the operation process, can significantly reduce the amount of solid waste generated, and effectively reduces the production cost.

Description

technical field [0001] The invention relates to a synthesis method of a glufosinate-ammonium intermediate, methyl phosphorus dichloride, and belongs to the field of synthesis of glufosinate-ammonium intermediates, in particular to a synthesis method of methyl phosphorus dichloride. Background technique [0002] Methyl phosphorus dichloride is a colorless, transparent liquid with a strong pungent odor, which can be used to prepare a new type of high-efficiency herbicide glufosinate-ammonium. [0003] The synthesis methods of methyl phosphorus dichloride reported so far include methane method, methyl iodide complexation method, methyl chloride complexation method and some other synthetic methods, among which the methyl chloride complexation method has become more competitive in the domestic market in recent years . U.S.Patent3,840,576[P].1974-10-8. Invented a method for synthesizing methyl phosphorus dichloride. Firstly, methyl sesquialuminide was prepared from aluminum powde...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/52
Inventor 王佳张先龙周林军赵广福胡其钊
Owner NANJING HUAZHOU PHARMA