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A preparation method and preparation system for one-step synthesis of methylphosphine dichloride

A technology of methyl phosphine dichloride and preparation system, which is applied in the field of preparation method and preparation system for synthesizing methyl phosphine dichloride by one-step method, can solve the problems of cumbersome operation in production process, low production efficiency, small production capacity of a single set of equipment, etc. question

Active Publication Date: 2021-05-14
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is currently the mainstream production process of methylphosphine dichloride in China, but its production process is cumbersome and involves difficult problems such as solid material transportation and transfer of flammable and explosive intermediates. At present, it can only be produced by batch method. The efficiency is low, the production capacity of a single set of equipment is small, and the process safety risk is very high. It is urgent to improve the domestic production technology of methyl phosphine dichloride through process innovation and equipment system integration optimization.

Method used

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  • A preparation method and preparation system for one-step synthesis of methylphosphine dichloride
  • A preparation method and preparation system for one-step synthesis of methylphosphine dichloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] In this example, the preparation system provided by the specific implementation method is used to synthesize methylphosphine dichloride, and the synthesis process specifically includes the following steps:

[0088] (1) 270g aluminum powder, 0.1g methyl iodide, 2065.5g phosphorus trichloride, 614.25g sodium chloride and 540g xylene are added in the reaction device, the stirring device 3 is opened, and the heating medium is injected into the jacket 2 of the reaction device , inject cooling medium into the condensation device 4 . Feed methyl chloride gas into the reaction device at a mass flow rate of 3 g / min, and control the reaction temperature in the reaction device at 50° C. and the reaction pressure at 0.2 MPa by controlling the flow rate of the heating medium and the feed rate of methyl chloride. When the amount of methyl chloride introduced reaches 1.1 times of the theoretical amount, the introduction of methyl chloride is stopped, and the reaction temperature of 60...

Embodiment 2

[0099] In this example, the preparation system provided by the specific implementation method is used to synthesize methylphosphine dichloride, and the synthesis process specifically includes the following steps:

[0100] (1) Add 270g aluminum powder, 0.5g iodine, 2065.5g phosphorus trichloride, 614.25g sodium chloride and 300g trimethylbenzene into the reaction device, open the stirring device 3, and inject heating medium into the jacket 2 of the reaction device , inject cooling medium into the condensation device 4 . Feed methyl chloride gas into the reaction device at a mass flow rate of 3 g / min, and control the reaction temperature in the reaction device at 80° C. and the reaction pressure at 0.3 MPa by controlling the flow rate of the heating medium and the feed rate of methyl chloride. When the amount of methyl chloride introduced reaches 1.2 times of the theoretical amount, the introduction of methyl chloride is stopped, and the reaction temperature of 80° C. is maintai...

Embodiment 3

[0105] In this example, the preparation system provided by the specific implementation method is used to synthesize methylphosphine dichloride, and the synthesis process specifically includes the following steps:

[0106] (1) 270kg aluminum powder, 100g methyl iodide, 2065.5kg phosphorus trichloride, 614.25kg sodium chloride and 500kg xylene are added in the reaction unit, the stirring device 3 is opened, and the heating medium is injected into the jacket 2 of the reaction unit, Inject the cooling medium into the condensation device 4 . Feed methyl chloride gas into the reaction device at a mass flow rate of 5 kg / min, and control the reaction temperature in the reaction device at 120° C. and the reaction pressure at 0.4 MPa by controlling the flow rate of the heating medium and the feed rate of methyl chloride. When the amount of methyl chloride introduced reaches 1.05 times of the theoretical amount, the introduction of methyl chloride is stopped, and the reaction temperature...

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Abstract

The invention provides a preparation method and preparation system for synthesizing methylphosphine dichloride in one step. Nitrogen replaces the air in the reaction device, feeds methyl chloride into the reaction device for mixed reaction, and the reaction product is distilled and condensed to obtain the methyl phosphine dichloride. The present invention will react raw material Al, PCl 3 and NaCl are pre-placed in the reaction device, and then replaced with nitrogen, stirred to fully disperse and suspend, then feed in methyl chloride gas for reaction, and control the flow rate of methyl chloride according to the reaction temperature, which is convenient to control, high in safety, and overall production efficiency and The product yield is higher. After the reaction is completed, the methyl phosphine dichloride product is obtained by condensation.

Description

technical field [0001] The invention belongs to the technical field of methyl phosphine dichloride synthesis, and relates to a preparation method and a preparation system of methyl phosphine dichloride, in particular to a preparation method and a preparation system for one-step synthesis of methyl phosphine dichloride. Background technique [0002] The pure product of methylphosphine dichloride is a colorless transparent liquid with a boiling point of 82-84°C. It is extremely active in chemical properties. It explodes in water and is easily oxidized in the air. It is an important intermediate for the synthesis of organophosphorus compounds. Indirect synthesis of hundreds of organophosphorus compounds, widely used in flame retardants, pesticides, pharmaceuticals and other industries. In particular, methylphosphine dichloride is an important intermediate of glufosinate-ammonium, the second most resistant transgenic herbicide in the world. With the rapid development of the gluf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/52
CPCC07F9/52
Inventor 周曙光秦龙余神銮姜胜宝祝小红王萍付萍闫涛涛
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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