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Continuous production method of glyphosate crystallization

A production method and technology of glyphosate, which are applied in the field of continuous production of glyphosate crystallization, can solve the problems of long residence time, no classification, and no recovery, so as to improve yield and quality, reduce energy consumption and cost, and reduce The effect of drying energy consumption

Active Publication Date: 2015-09-16
HANGZHOU JINFADA CHEM IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the limitation of equipment materials and other factors, most of them adopt batch method, which seriously restricts the enlargement and optimization of production equipment. Factors such as low production efficiency, high labor intensity of workers, high investment in production equipment and large area occupied by batch crystallization process exist. And other issues
There are not many reports on the process of continuous production of glyphosate. Although CN1944445A also relates to the continuous crystallization process of glyphosate, there are still long average residence times, large crystallization tanks due to lack of classification, and high temperature crystal heat. Problems such as high glyphosate content in

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1) A synthetic solution prepared from methanol, triethylamine, paraformaldehyde, glycine, and dimethyl phosphite (the molar ratio of methanol: triethylamine: paraformaldehyde: glycine: phosphorous acid is 9:0.8:1.8:1 :1.2), that is, the synthetic liquid obtained by the alkyl ester method and 30% hydrochloric acid (the molar ratio of synthetic liquid to hydrochloric acid is 1:3.2) hydrolyzed glyphosate hydrolysate is passed into the neutralization tank and the concentration of hydrogen is 32% Liquid caustic soda such as sodium oxide or potassium hydroxide is circulated and neutralized to a pH of 1.5, and the residence time of the neutralized liquid in the neutralization tank is controlled to be 2 hours;

[0023] 2) The neutralization liquid obtained in step 1) is controlled by the liquid level to enter the first-stage heat exchanger at a flow rate of 1 ton / hour to cool to 60°C, and then pass into the first-stage crystallization kettle at a flow rate of 1 ton / hour for circula...

Embodiment 2

[0030] 1) Prepared from methanol, triethylamine, paraformaldehyde, glycine, dimethyl ester (methanol: triethylamine: paraformaldehyde: glycine: dimethyl ester molar ratio is 10:1.1:1.9:1:1.3) The synthetic solution and the glyphosate hydrolysate obtained by hydrolysis with 30% hydrochloric acid are passed into the neutralization tank and the concentration of 32% sodium hydroxide or potassium hydroxide and other liquid caustic soda is circulated and neutralized to pH 0, and the neutralization solution is controlled The residence time in the neutralization kettle is 0.5 hours;

[0031] 2) The neutralized liquid obtained in step 1) is passed into the first-stage heat exchanger at a flow rate of 0.5 ton / hour through liquid level control to cool to 40°C, and then passed into the first-stage crystallization kettle at a flow rate of 0.5 ton / hour for circulation 1 hour;

[0032] 3) The first-grade crystal water obtained in step 2) is discharged through liquid level control and then enters...

Embodiment 3

[0038] 1) Prepared from methanol, triethylamine, paraformaldehyde, glycine, dimethyl ester (methanol: triethylamine: paraformaldehyde: glycine: dimethyl ester molar ratio 11:1.2:1.8:1:1.4) The synthesis solution and the glyphosate hydrolysate obtained by hydrolysis with 30% hydrochloric acid are passed into the neutralization kettle and the concentration of 32% sodium hydroxide or potassium hydroxide and other liquid caustic soda is circulated and neutralized to pH 3, and the neutralization solution is controlled The residence time in the neutralization kettle is 3 hours;

[0039] 2) The neutralization liquid obtained in step 1) is controlled by the liquid level to enter the first-stage heat exchanger at a flow rate of 6 tons / hour to cool to 80°C, and then pass into the first-stage crystallization kettle at a flow rate of 6 tons / hour to circulate 3 hours;

[0040] 3) The first-grade crystal water obtained in step 2) is discharged through liquid level control and then enters a cont...

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Abstract

The invention discloses a continuous production method of a glyphosate crystal, which belongs to the technical field of post-treatment and processing of glyphosate. The method comprises the following steps of: introducing a synthetic liquid prepared from methanol, triethylamine, paraformaldehyde, glycine and dimethyl ester, and a glyphosate hydrolyzate obtained by hydrolyzing hydrochloric acid into a neutralizing kettle for circularly neutralizing with a caustic soda liquid; feeding a neutralizing liquid discharged under liquid level control into a first-stage heat exchanger for cooling, and introducing into a first-stage crystalizing kettle for circulating; feeding first-stage crystal slurry discharged under liquid level control into a continuous automatic separator for separating to obtain hot wet powder and a hot mother solution; feeding the hot mother solution discharged under liquid level control into a second-stage heat exchanger for cooling, and introducing into a second-stage crystalizing kettle for circulating; feeding second-stage crystal slurry discharged under liquid level control into a continuous automatic separator for separating to obtain original powder and a cold mother solution; and directly adding water into the original powder to obtain a glyphosate water aqua, and recovering a cold mother solution. Due to the adoption of the continuous production method, the production efficiency of the glyphosate can be effectively increased.

Description

Technical field [0001] The invention belongs to the technical field of glyphosate post-treatment processing, and specifically relates to a continuous production method of glyphosate crystallization. Background technique [0002] Glyphosate is a herbicide commercialized by Monsanto in the United States in 1974. Due to its high efficiency, low toxicity, low residue, broad spectrum, and good environmental compatibility, glyphosate has become the world's most used herbicide. A wide range of herbicides. The production of glyphosate in my country started in the 1980s, and most of it uses an alkyl ester synthesis process with glycine, dimethyl phosphite, and paraformaldehyde as the main raw materials. This method has stable process and high yield, so it develops very rapidly. The method includes a multi-step reaction process of synthesis, hydrolysis and crystallization. Due to the limitation of equipment materials and other factors, the batch method is mostly adopted, which seriously...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38A01N57/20A01P13/00
Inventor 孔鑫明周海杨刘劭农邓青松周锦枫程晨杰汤晓娟李竞熊齐春孙晓昂
Owner HANGZHOU JINFADA CHEM IND