Method for synthesizing methyl phosphine dichloride

A technology for synthesizing methylphosphine dichloride and methylphosphine dichloride, which is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., and can solve the problem of high environmental pressure and high cost , Low continuous production capacity and other issues

Active Publication Date: 2020-11-10
SICHUAN FOURSTAR BIOTECH RANDD CORP
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Problems solved by technology

[0004] The present invention mainly aims at the problems of high reaction temperature, certain reaction pressure, easy generation of solid impurities, low continuous production capacity, high cost and high environmental pressure in the process of synthesizing methylphosphine dichloride by high temperature method, and provides a Methane and phosphorus trichloride are used as raw materials to react under the action of ultraviolet light to generate methyl phosphine dichloride. The method maintains the reaction selectivity and yield, does not add toxic initiators, and reduces the need for reaction. The pressure, temperature and other conditions can avoid the problem of the reduction of reaction conversion rate caused by the deactivation of the surface of the solid catalyst, and the degree of continuity is higher

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  • Method for synthesizing methyl phosphine dichloride
  • Method for synthesizing methyl phosphine dichloride
  • Method for synthesizing methyl phosphine dichloride

Examples

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Effect test

Embodiment 1

[0033] like figure 1 Shown, a kind of method for synthesizing methyl phosphine dichloride comprises the following steps:

[0034] A. Replace the quartz glass reactor (volume 2.45L, length 40cm) with nitrogen to fill the whole reactor with nitrogen, then turn on the ultraviolet lamp, the wavelength of ultraviolet light is 100nm, turn on the quartz reactor and heat it with a resistance furnace;

[0035] B. After the temperature of the quartz reactor rises to 110°C, then respectively feed methane and phosphorus trichloride (methane flow rate: 610L / h, phosphorus trichloride flow rate: 0.3L / h; the molar ratio of methane to phosphorus trichloride is 8:1), methane undergoes CH 4 The preheater is preheated to 90°C, and phosphorus trichloride is passed through PCl 3 The vaporizer is heated to gasification, mixed by the mixer, and then enters the quartz reactor to stay and react for 10s;

[0036] C. Condensate the mixed material obtained through the reaction in step B through the pri...

Embodiment 2

[0040] like figure 1 Shown, a kind of method for synthesizing methyl phosphine dichloride comprises the following steps:

[0041] A. Replace the quartz glass reactor (volume 2.45L, length 40cm) with nitrogen to fill the whole reactor with nitrogen, then turn on the ultraviolet lamp, the wavelength of ultraviolet light is 280nm, turn on the quartz reactor and heat it with a resistance furnace;

[0042] B. After the temperature of the quartz reactor rises to 90°C, then respectively feed methane and phosphorus trichloride (methane flow rate: 318L / h, phosphorus trichloride flow rate: 0.311L / h; the molar ratio of methane to phosphorus trichloride is 4:1), methane undergoes CH 4 The preheater is preheated to 80°C, and phosphorus trichloride is passed through PCl 3 The vaporizer is heated to gasification, mixed by a mixer, and then enters a quartz reactor to stay and react for 16s;

[0043] C. Condensate the mixed material obtained through the reaction in step B through the primar...

Embodiment 3

[0047] likefigure 1 Shown, a kind of method for synthesizing methyl phosphine dichloride comprises the following steps:

[0048] A. Replace the quartz reactor (volume 2.45L, length 80cm) with nitrogen to fill the whole reactor with nitrogen, then turn on the ultraviolet lamp, the wavelength of ultraviolet light is 185nm, turn on the quartz reactor and heat it with a resistance furnace;

[0049] B. When the temperature of the quartz reactor rises to 300°C, then respectively feed methane and phosphorus trichloride (methane flow rate: 1042L / h, phosphorus trichloride flow rate: 0.41L / h; the molar ratio of methane to phosphorus trichloride is 10:1), methane undergoes CH 4 The preheater is preheated to 150°C, and phosphorus trichloride is passed through PCl 3 The vaporizer is heated to gasification, mixed by the mixer, and then enters the quartz reactor to stay and react for 4s;

[0050] C. Condensate the mixed material obtained through the reaction in step B through the primary c...

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Abstract

The invention mainly aims at the problems of high reaction temperature, certain reaction pressure, easy generation of solid impurities, low continuous production capacity, high cost, high environmental pressure and the like in the existing process of synthesizing methyl phosphine dichloride by a high-temperature method, and provides a method for synthesizing methyl phosphine dichloride by using methane and phosphorus trichloride as raw materials. According to the synthetic method, the reaction selectivity and yield are maintained. Meanwhile, no toxic initiator is added, the pressure, temperature and other conditions required by the reaction are reduced, the problem that the reaction conversion rate is reduced due to the fact that the surface of the solid catalyst is covered and inactivatedis solved, the continuous degree is higher, and the yield is higher. According to the method, a product with the content of methyl phosphine dichloride being greater than 17wt% can be synthesized, and after the product is rectified, a methyl phosphine dichloride product with the content being greater than 99wt% and phosphorus trichloride with the content being greater than 98.5 wt% can be obtained.

Description

technical field [0001] The invention relates to the technical field of synthesis of organophosphorus compound intermediates, in particular to a method for synthesizing methylphosphine dichloride. Background technique [0002] Methylphosphine dichloride CH 3 PCl 2 , colorless transparent liquid, boiling point 80~82℃, density 1.3g / cm 3 , extremely active in nature, flammable and explosive in contact with water, easily oxidized in air, difficult to store and transport. Methylphosphine dichloride is an important intermediate in the synthesis of organophosphorus compounds and is widely used. Hundreds of organophosphorus compounds can be directly or indirectly synthesized from it, and the reaction using it as a starting material has a very high conversion rate, and most reactions are almost carried out quantitatively. If the production capacity of methyl phosphine dichloride can be increased and its production cost can be reduced, it will bring huge economic value. [0003] A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/52
CPCC07F9/52C07F9/5072
Inventor 朱槽王长江卢刚高杉
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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