Purification process of glyphosate mother liquor

A technology for glyphosate mother liquor and treatment process, which is applied in the fields of chemicals for biological control, inorganic chemistry, phosphorus compounds, etc., can solve the problems of high treatment cost, difficulty in reusing waste liquid or waste, and environmental pollution.

Inactive Publication Date: 2019-11-01
刘德亮
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a purification treatment process for glyphosate mother liquor, so as to solve the problem that there are many impurities in the product obtained in the existing glyphosate mother liquor treatment process, resulting in waste liquid or waste that is difficult to reuse, and the treatment cost is high and environmental pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0110] Take 5500g of the acidic mother liquor obtained by the glycine method to produce glyphosate, which is strongly acidic, heat up to 110°C under normal pressure, filter the precipitated triethylamine hydrochloride while heating and concentrating, and return the filtrate to the mother liquor In the process, 1500g of water was distilled off to obtain 2263g of triethylamine hydrochloride and 1737g of glyphosate mother liquor concentrate, and the glyphosate mother liquor concentrate was strongly acidic.

[0111] Cool the glyphosate mother liquor concentrate to 25°C, add 655g of sodium liquid caustic soda, adjust the pH of the solution to 2, then add 595g of triethylamine, adjust the pH of the solution to 5.0, set the temperature to 25°C, and let the solution stand for 2 hours. Divided into two layers, after separation, 1691g of the solution containing triethylamine hydrochloride in the upper layer and 1292g of the sodium salt solution containing organic phosphorus in the lower ...

Embodiment 2

[0116] Take 5500g of the acidic mother liquor obtained by the glycine method to produce glyphosate, its pH=0.2, raise the temperature to 105°C under normal pressure, filter the precipitated triethylamine hydrochloride while heating and concentrating, and return the filtrate to the mother liquor , steamed out 1501g water, obtained 2264g triethylamine hydrochloride and 1735g glyphosate mother liquor concentrate, and the glyphosate mother liquor concentrate pH=0.2.

[0117] Cool the glyphosate mother liquor concentrate to 25°C, add 755g of sodium liquid caustic soda, adjust the pH of the solution to 7.5, then add 105g of triethylamine, adjust the pH of the solution to 14, raise the temperature to 70°C, and let the solution stand for 2 hours. Divided into 3 layers, after separation, 100g triethylamine in the upper layer, 1091g solution containing triethylamine hydrochloride in the middle layer and 1292g sodium salt solution containing organic phosphorus in the lower layer were obta...

Embodiment 3

[0122] Take 5500g of the acidic mother liquor obtained by the glycine method to produce glyphosate, its pH=0.4, raise the temperature to 120°C under normal pressure, filter the precipitated triethylamine hydrochloride while heating and concentrating, and return the filtrate to the mother liquor , 1500g of water was distilled off to obtain 2262g of triethylamine hydrochloride and 1738g of glyphosate mother liquor concentrate, and the pH of the glyphosate mother liquor concentrate was 0.4.

[0123] Cool down the concentrated solution of glyphosate mother liquor to 25°C, add 651g of sodium liquid caustic soda, adjust the pH of the solution to 5.6, then add 100g of triethylamine to adjust the pH of the solution to 7.5, raise the temperature to 30°C, let stand for 2 hours, and divide the solution There are 2 layers, and after separation, 1195g of the solution containing triethylamine hydrochloride in the upper layer and 1293g of the sodium salt solution of organic phosphorus in the ...

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Abstract

The invention provides a purification process of a glyphosate mother liquor. The process includes subjecting the glyphosate mother liquor to concentration and triethylamine hydrochloride precipitation; removing the triethylamine hydrochloride precipitate to obtain a glyphosate mother liquor concentrate A; adding a pH adjusting agent to make the solution layered; extracting triethylamine and hydrochloride from a solution containing the triethylamine hydrochloride; converting the triethylamine hydrochloride into triethylamine; then treating a salt solution containing organophosphorus to obtain acorresponding dibasic biphosphate or an aqueous glyphosate solution. The process is scientific and reasonable, achieves high-efficiency recovery of triethylamine, can obtain a plurality of by-products without waste liquid and solid waste, greatly reduces the treatment cost for the glyphosate mother liquor, and has obvious economic and environmental benefits. The process solves the difficult problem that the glyphosate mother liquor cannot be completely treated, which hinders development of the glyphosate industry, and the process achieves purification of the glyphosate mother liquor and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the recovery and treatment of glyphosate mother liquor, in particular to a purification treatment process for glyphosate mother liquor prepared by a glycine method. Background technique [0002] Glyphosate is a high-efficiency broad-spectrum herbicide that has a broad herbicidal spectrum, low toxicity and no residue. At present, glyphosate is usually prepared by the glycine method in China, that is, paraformaldehyde, glycine and dialkyl phosphite are used as raw materials, triethylamine is used as a catalyst, and glyphosate is obtained after addition, condensation, and acidolysis. This method is relatively simple, the yield is high, the cost is low, and the product quality is good, but because glyphosate has a certain solubility in water, a certain amount of glyphosate mother liquor will inevitably be produced, and the glyphosate mother liquor is an acidic liquid , contains a large amount of triethylamine hydrochloride, hydroc...

Claims

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Application Information

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IPC IPC(8): A01N57/20A01P13/00C07C209/00C07C211/05C01B25/30C01B25/28
CPCA01N57/20C01B25/28C01B25/30C07C209/00C07C211/05
Inventor 刘德亮
Owner 刘德亮
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