A kind of crystallization process of glyphosate production

A technology of glyphosate and glyphosate acid, which is applied in the direction of chemicals, biocides, and biocides for biological control, can solve the problem of high content of glyphosate and sodium chloride, reduce the content of impurities, Improvement of yield and quality

Active Publication Date: 2016-05-25
SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention aims to solve the problem that the sodium chloride content of glyphosate is too high in the glycine method. Aiming at this problem, a process research is carried out, and a crystallization process for glyphosate production by the glycine method is provided, which can effectively control the original glyphosate Sodium chloride content in

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of crystallization technique that glyphosate is produced, carries out as follows:

[0025] A. In the process of preparing glyphosate acid by the dimethyl phosphite method, the triethylamine salt condensation solution of the dimethyl glyphosate obtained after the condensation reaction was hydrolyzed with hydrochloric acid to obtain 2100 kg of hydrolyzate;

[0026] B. Add 350 kg of dilution water to the hydrolyzed solution after hydrolysis, cool down to 68°C, add 680 kg of triethylamine to neutralize excess hydrochloric acid, stir for 27 minutes, and the pH value is 1.29

[0027] C. Continue to cool down to below 35°C, separate, wash and dry to obtain 2526.5 kg of glyphosate technical.

[0028] The content of glyphosate in the original medicine is 95.5%, and the content of sodium chloride is 55PPM.

[0029] The amount of glycine is 1450 kg, the content is 98.5%, and the yield of glyphosate calculated by glycine is 75%.

Embodiment 2

[0031] This embodiment is basically the same as Embodiment 1, on this basis:

[0032] The hydrolyzate in step B is 1900 kg, add 475 kg of dilution water, cool down to 60°C, slowly add 680 kg of triethylamine under the hydrolyzate to neutralize excess hydrochloric acid, stir for 25 minutes, and measure the pH value to be 1.5 .

[0033] Cool to 28°C and centrifuge, wash, and dry 2,570 kg of glyphosate.

[0034] The content of glyphosate in the original medicine is 95.2%, and the content of sodium chloride is 45PPM.

[0035] The amount of glycine used is 1450 kg, the content is 98.5%, and the yield of glyphosate calculated by glycine is 76%.

Embodiment 3

[0037] This embodiment is basically the same as Embodiment 1, on this basis:

[0038] The hydrolyzate in step B is 2300 kg, add 365 kg of dilution water, cool down to 62°C, slowly add 680 kg of triethylamine from the hydrolyzate, stir for 30 minutes, and measure the pH value to be 0.5.

[0039] Cool to 24°C and centrifuge, wash, and dry 2545.9 kg of glyphosate.

[0040] The content of glyphosate in the original medicine is 95.1%, and the content of sodium chloride is 58PPM.

[0041] The amount of glycine used is 1450 kg, the content is 98.5%, and the yield of glyphosate calculated by glycine is 75.2%.

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Abstract

The invention provides a crystallization process for producing glyphosate through a glycine method in order to solve the problem that the glyphosate salt content is extremely high in the glycine method. The crystallization process comprises the following steps of: A) adding hydrochloric acid to hydrolyze a triethylamine salt condensation solution of dimethyl glyphosate obtained through the condensation reaction so as to obtain a hydrolysis liquid in the process of preparing glyphosate acid through a dimethyl phosphite method; B) adding water to dilute in the hydrolysis liquid in which the hydrolysis is completed, reducing the temperature to be 70 DEG C or below with stirring, adding triethylamine to neutralize excessive hydrochloric acid, uniformly stirring, and measuring the pH value; and C) continuously reducing the temperature to be 35 DEG C or below, and separating, washing and drying to obtain the original glyphosate. According to the process, the sodium chloride content in the original glyphosate can be effectively controlled to be 300PPM or below.

Description

technical field [0001] The invention relates to the field of glyphosate production, more specifically, the invention relates to a crystallization process for glyphosate production. Background technique [0002] Glyphosate (glyphosate), scientific name N-(phosphonomethyl) glycine, N-(phosphonomethyl) glycine, is an organophosphorus herbicide. The herbicidal properties of glyphosate were discovered by D.D. Baird in the United States in 1971, and developed and produced by Monsanto. By the 1980s, it had become an important variety of herbicides in the world. Glyphosate is a systemic chronic broad-spectrum herbicide that mainly inhibits enolacetonyl shikimelin phosphate synthase in the body, thereby inhibiting the conversion of shikime to phenylalanine, tyrosine and tryptophan. Transformation, which interferes with protein synthesis leading to plant death. Glyphosate is absorbed by the stems and leaves and then transmitted to various parts of the plant. It can control more than...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38A01N57/20A01P13/00
Inventor 姜永红罗仲明高才李之文罗蓉田姚
Owner SICHUAN LESHAN FUHUA TONGDA AGRO-CHEM TECH CO LTD
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