Novel process for recycling mother solution of glyphosate prepared by glycin method

A technology of glycine method and glyphosate, which is applied in the fields of chemicals for biological control, organic chemistry, herbicides and algicides, etc., can solve the problems of complex composition of mother liquor, high material consumption, quality degradation, etc., and achieve economical savings. The effect of input of raw materials and equipment, reduction of energy consumption and improvement of production capacity

Active Publication Date: 2009-12-02
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The existing synthetic route has high material consumption, a large amount of formaldehyde is produced during acidolysis, and formaldehyde (6-10%) is prone to condensation reaction with glyphosate under high temperature and acidic conditions when concentrated, resulting in reduced yield and quality. complex

Method used

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  • Novel process for recycling mother solution of glyphosate prepared by glycin method
  • Novel process for recycling mother solution of glyphosate prepared by glycin method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Adopt the method for comparative example 1 to prepare glyphosate crystallization mother liquor 75.5g, this mother liquor adds alkali and reclaims triethylamine to obtain mother liquor to be treated (hereinafter referred to as mother liquor to be treated), then passes into hydrogen chloride gas in this mother liquor to be treated, finally 143.9 g of solid-liquid mixture was obtained, and 50.6 g of crude sodium chloride was obtained after suction filtration, and 83.3 g of acid precipitation and desalination mother liquor. After chemical composition analysis, the hydrochloric acid content in the acid precipitation and desalination mother liquor is 26.69%, the chlorine content in the sodium chloride solid is 58.50%, and the acid precipitation desalination and sodium chloride removal rate is 92.28%. The acid precipitation and desalination mother liquor is reserved for the next batch Instead of hydrochloric acid, and according to the comparative example 1 acidification and hyd...

Embodiment 2

[0020] The method of Example 1 was used to treat the glyphosate crystallization mother liquor. Hydrogen chloride gas was introduced into the mother liquor to be treated, and finally 144.3 g of a solid-liquid mixture was obtained. After suction filtration, 51.5 g of crude sodium chloride was obtained, and 85.2 g of the mother liquor for acid precipitation and desalination. After chemical composition analysis, the hydrochloric acid content in the acid precipitation and desalination mother liquor is 27.23%, the chlorine content in the sodium chloride solid is 58.69%, and the acid precipitation desalination and sodium chloride removal rate is 92.34%. The acid precipitation and desalination mother liquor is reserved for the next batch Instead of hydrochloric acid, and according to the comparative example 1 acidification and hydrolysis part recycling.

Embodiment 3

[0022] Adopt the method for contrasting example 1 to prepare glyphosate, replace the hydrochloric acid acidification process esterification product with the acid precipitation desalting mother liquor of embodiment 1 gained during acidification, after deacidification, add water, cooling and crystallization, get glyphosate former powder 42.92g (content 95.5%), former powder yield 78%, total yield 81.3%, get glyphosate mother liquor 78.6g, after this mother liquor adds alkali and reclaims triethylamine, obtains mother liquor to be treated (hereinafter referred to as mother liquor to be treated), then to the mother liquor to be treated Hydrogen chloride gas was passed through the mother liquor to obtain 147.1 g of a solid-liquid mixture, 54.23 g of crude sodium chloride was obtained after suction filtration, and 86.8 g of the mother liquor for acid precipitation and desalination. After chemical composition analysis, the hydrochloric acid content in the acid precipitation and desali...

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Abstract

The invention relates to a novel process for recycling waste liquid produced by preparation of weedicide glyphosate (N-phosphono-methyl glycine) by taking alkyl phosphate as a raw material. The process overcomes the disadvantages of mass energy consumption of desalting by hot condensation, large equipment investment, low content of the glyphosate after being heated, low content of the glyphosate in a condensate, large product loss and the like, can well reclaim byproduct salt and can farthest obtain the solid glyphosate. The novel process for recycling mother solution recycles the waste liquid, meets the clean production requirement of energy conservation and emission-reduction and has good economic and social benefits.

Description

field of invention [0001] The present invention relates to a kind of novel method of recycling the waste liquid produced by the herbicide glyphosate (N-phosphonomethylglycine) using alkyl phosphite as raw material. Specifically, the method of the present invention comprises the following steps: Glyphosate is synthesized and crystallized by the glycine method, glyphosate is separated, and triethylamine is recovered. The mother liquor absorbs hydrogen chloride gas, acid precipitation and desalination, and the acid precipitation and desalination mother liquor replaces hydrochloric acid to the acid hydrolysis process, and is recycled for desalination. This process overcomes the disadvantages of thermal concentration and desalination, such as large energy consumption, large investment in equipment, reduced heating content of glyphosate, low glyphosate content in the concentrate, and large product loss. It can not only recover by-product salt well, but also can Get the most out of s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38C02F1/58A01P13/00
Inventor 查正炯尹应武易飞
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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