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Method for synthesizing (3-amino-3-cyano) propyl methyl butyl phosphite based on micro-channel reactor

A technology of propyl methyl butyl phosphite and micro-channel reactor is applied in the field of glufosinate-ammonium intermediate synthesis, which can solve the problems of increased consumption of raw materials, low production efficiency, increased waste water and waste salt and the like

Inactive Publication Date: 2020-11-27
SICHUAN FOURSTAR BIOTECH RANDD CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The present invention mainly aims at the problems that the existing synthetic method of (3-amino-3-cyano)propylmethyl butyl phosphite leads to increased consumption of raw materials in subsequent sections, increased waste water and waste salt, huge production equipment, complex control, and low production efficiency. , providing a method for synthesizing (3-amino-3-cyano)propylmethyl butyl phosphite based on a microchannel reactor

Method used

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  • Method for synthesizing (3-amino-3-cyano) propyl methyl butyl phosphite based on micro-channel reactor
  • Method for synthesizing (3-amino-3-cyano) propyl methyl butyl phosphite based on micro-channel reactor
  • Method for synthesizing (3-amino-3-cyano) propyl methyl butyl phosphite based on micro-channel reactor

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Effect test

Embodiment 1

[0030] A method for synthesizing (3-amino-3-cyano) propylmethyl phosphite butyl based on a microchannel reactor, comprising the following steps:

[0031] A, open the heating system of microchannel reactor, make system warm up to reaction temperature 30 ℃;

[0032] B. Metering 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate, water and ammonia gas into the microchannel reactor (wherein, 3-(butoxymethylphosphoryl)- 1-cyanopropyl acetate 0.3mol / min, ammonia gas 0.6mol / min, water 1.5mol / min), the reaction pressure is normal pressure;

[0033] C. The three materials introduced in step B stay and react in the microchannel reactor for 1min, and after the ammonia gas is recovered by flash evaporation, the dilute ammonia solution of (3-amino-3-cyano)propylmethyl butyl phosphite is collected Product 1142.3g, as NH 3 The calculated ammonia content is 0.08%, and the external standard quantitative detection of high performance liquid chromatography shows that the content of (3-amino-3-cy...

Embodiment 2

[0035] A method for synthesizing (3-amino-3-cyano) propylmethyl phosphite butyl based on a microchannel reactor, comprising the following steps:

[0036] A, open the heating system of microchannel reactor, make system warm up to reaction temperature 70 ℃;

[0037] B. Metering 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate, water and ammonia gas into the microchannel reactor (wherein, 3-(butoxymethylphosphoryl)- 1-cyanopropyl acetate 0.3mol / min, ammonia gas 3mol / min, water 6mol / min), the reaction pressure is 1.8MPa;

[0038] C. The three materials introduced in step B stay and react in the microchannel reactor for 10 minutes. After the ammonia gas is recovered by flash evaporation, the dilute ammonia solution of (3-amino-3-cyano)propylmethyl phosphite butyl is collected Product 1991.6g, in NH 3 The calculated ammonia content was 0.86%, and the external standard quantitative detection of high-performance liquid chromatography was carried out. The content of (3-amino-3-cyano)...

Embodiment 3

[0040] A method for synthesizing (3-amino-3-cyano) propylmethyl phosphite butyl based on a microchannel reactor, comprising the following steps:

[0041] A, open the heating system of microchannel reactor, make system warm up to reaction temperature 50 ℃;

[0042] B. Metering 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate, water and ammonia gas into the microchannel reactor (wherein, 3-(butoxymethylphosphoryl)- 1-cyanopropyl acetate 0.3mol / min, ammonia gas 0.6mol / min, water 6mol / min), the reaction pressure is 1MPa;

[0043] C. The three materials introduced in step B stay and react in the microchannel reactor for 3 minutes, and after the ammonia gas is recovered by flash evaporation, the dilute ammonia solution of (3-amino-3-cyano)propylmethyl butyl phosphite is collected Product 1972.1g, in NH 3 The calculated ammonia content is 0.02%, and the external standard quantitative detection of high performance liquid chromatography shows that the content of (3-amino-3-cyano) pro...

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Abstract

The invention relates to the technical field of glufosinate-ammonium intermediate synthesis, and particularly discloses a method for synthesizing (3-amino-3-cyano) propyl methyl butyl phosphite basedon a micro-channel reactor. The invention mainly aims at solving the problems of the increase of the raw material consumption of a subsequent work section, wastewater and waste salt increase, huge production equipment, complex control and low production efficiency and the like of an existing (3-amino-3-cyano) propyl methyl butyl phosphite synthesis method. According to the method, 3-(butoxy methylphosphoryl)-1-cyanopropyl acetate, water and ammonia gas are adopted as raw materials; the micro-channel reactor is adopted, and flash evaporation degassing is used in combination to recover excess ammonia gas; the yield of the obtained (3-amino-3-cyano) propyl methyl butyl phosphite can reach 95% or above at most, the types of materials are reduced, the water amount of the system is reduced, continuous reaction is realized, the reaction period is greatly shortened, energy consumption is reduced, and the production cost is greatly reduced.

Description

technical field [0001] The invention relates to the technical field of synthesis of glufosinate-ammonium intermediates, in particular to a method for synthesizing (3-amino-3-cyano)propylmethyl butyl phosphite based on a microchannel reactor. Background technique [0002] (3-Amino-3-cyano) butyl methyl phosphite is an intermediate in the synthesis of glufosinate-ammonium, molecular formula C 9 h 19 N 2 o 2 P, the structural formula is as follows: [0003] [0004] In the synthesis of glufosinate-ammonium, (3-amino-3-cyano)propylmethyl butyl phosphite is generally composed of 3-(butoxymethylphosphoryl)-1-cyanopropyl acetate and dissolved The ammonia solution of ammonium chloride is obtained by reacting at a certain temperature, and its synthesis reaction is as follows: [0005] [0006] In order to ensure that the reaction is carried out smoothly, this method needs to use more ammoniacal liquor to dissolve ammonium chloride, to ensure that the reaction is a homogene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/32B01J19/00
CPCC07F9/3211C07F9/3264B01J19/0093
Inventor 王长江李舟卢刚王文
Owner SICHUAN FOURSTAR BIOTECH RANDD CORP
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