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Synthetic method of methyl hypophosphite

A technology of methyl hypophosphite and synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve problems such as low production efficiency, long reaction time, and complicated post-processing, etc. question

Active Publication Date: 2020-10-20
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Methyl hypophosphite in the prior art is prepared by a reaction tower, such as CN106674275B, but the preparation by the reaction tower has long reaction time, low production efficiency, easy disproportionation reaction, toxic substances, and complicated post-treatment shortcoming

Method used

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  • Synthetic method of methyl hypophosphite
  • Synthetic method of methyl hypophosphite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1 (as figure 1 shown), the continuous flow reactor 1 includes a first preheating part 12 with a first inlet, a second preheating part 13 with a second inlet, and the first preheating part 12 and the second preheating part 13 A plurality of reaction parts 11 that are connected and serially connected in sequence.

Embodiment 2

[0039] Embodiment 2 (as figure 2 As shown), the continuous flow reactor 1 includes a plurality of reaction parts 11 connected in series in sequence, the first inlet is arranged on the second reaction part 11, and the second inlet is arranged on the first reaction part 11.

[0040] The structure of the reaction section and the preheating section in the present invention are the same, and only the names are different.

[0041] When using this equipment for production, methyl phosphine dichloride enters from the first inlet according to a certain flow rate, alcohol enters from the second inlet according to a certain flow rate and after preheating, methyl phosphine dichloride and alcohol enter in the continuous flow reactor 1, and the residence time of the reactants in the continuous flow reactor 1 can be controlled by controlling the number of reaction parts 11 in series; the reaction liquid coming out of the continuous flow reactor 1 enters the In the evaporator 3, by-products...

Embodiment 3

[0050] Synthesis of n-Butyl Methylphosphinate

[0051] Butanol alcohol is preheated to 75°C through the first plate at a flow rate of 15g / min, and methylphosphine dichloride is mixed with ethanol on the second plate at a flow rate of 5g / min. After a residence time of 2 minutes, enter Vaporization chamber, the temperature of the vaporization chamber is 75°C, the negative pressure is -0.095MPa, and chlorobutane, butanol and hydrogen chloride are collected for 5 minutes, and 29.7g of the product is emitted from the bottom of the vaporization chamber, with a purity of 96% and a yield of 99%.

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Abstract

The invention relates to a method for synthesizing methyl hypophosphite, which is prepared by reacting methyl phosphine dichloride and alcohol serving as raw materials in a continuous flow reactor. The method is simple in technological process, few in side reaction, capable of reducing generation of toxic substances, low in after treatment cost, high in production efficiency, high in yield and purity, good in safety and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, in particular to a method for synthesizing methyl hypophosphite. Background technique [0002] Methyl hypophosphite in the prior art is prepared by a reaction tower, such as CN106674275B, but the preparation by the reaction tower has long reaction time, low production efficiency, easy disproportionation reaction, toxic substances, and complicated post-treatment shortcoming. Contents of the invention [0003] The purpose of the present invention is to provide a kind of synthesis method and production equipment of methyl hypophosphite with high production efficiency and simple aftertreatment. [0004] In order to achieve the above object, the present invention adopts following technical scheme: [0005] One aspect of the present invention provides a method for synthesizing methyl phosphinate, which is prepared by reacting methyl phosphine dichloride and alcohol as raw materials, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32
CPCC07F9/3264
Inventor 姜宇华周炜陈佳纪雷夏易能
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD