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Comprehensive recovery process for glyphosate mother liquor

A technology of glyphosate mother liquor and recovery method, which is applied in botany equipment and methods, amino compound purification/separation, biocide, etc., and can solve the problem of difficult to reuse waste liquid or waste, incomplete material recovery, and environmental pollution And other issues

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 comprehensive recovery method for glyphosate mother liquor, to solve the incomplete material recovery in the existing glyphosate mother liquor recovery treatment method, produce waste liquid or waste that is difficult to reuse, high processing cost and environmental pollution issues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] Take 5500g of the acidic mother liquor obtained by the production of glyphosate by the glycine method, which is strongly acidic, raise the temperature to 100°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.

[0100] Cool down the glyphosate mother liquor concentrate to 25°C, add 700g of triethylamine, adjust the pH of the solution to 2, then add 420g of ammonium bicarbonate, neutralize to pH=7, obtain 2225g of mother liquor, set the temperature to 25°C, and let stand After 2 hours, the solution was divided into upper and lower layers. After separation, 1107g of the upper layer containing triethylamine hydrochloride solution and 1118g of the lower layer conta...

Embodiment 2

[0105] Take 5500g of the acidic mother liquor obtained by the glycine method to produce glyphosate, its pH=0.1, raise the temperature to 50°C under reduced 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 2265.2g of triethylamine hydrochloride and 1734.8g of glyphosate mother liquor concentrate, and the pH of the glyphosate mother liquor concentrate was 0.1.

[0106] Cool down the glyphosate mother liquor concentrate to 25°C, add 200g of triethylamine, adjust the pH=1 of the solution, then add 380g of ammonium bicarbonate, neutralize to pH=5.0, obtain 2085g of mother liquor, then add 300g of triethylamine, PH = 7.2, heated to 70°C, and after standing for 2 hours, the solution was divided into upper and lower layers. After separation, 1296.8g of a solution containing triethylamine hydrochloride in the upper layer and 1118g of an ammonium salt so...

Embodiment 3

[0111]Take 5500g of the acidic mother liquor obtained by the glycine method to produce glyphosate, its pH=0.2, raise the temperature to 100°C under reduced 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 2265.2g of triethylamine hydrochloride and 1734.8g of glyphosate mother liquor concentrate, and the pH of the glyphosate mother liquor concentrate was 0.2.

[0112] Cool the glyphosate mother liquor concentrate to 25°C, add 350g of triethylamine, adjust the pH of the solution to 2.5, then add 430g of ammonium bicarbonate, neutralize to pH=7.5, obtain 2225g of mother liquor, heat to 89°C, and let stand After 2 hours, the solution was divided into upper and lower layers. After separation, 1117g of a solution containing triethylamine hydrochloride in the upper layer and 1118g of an ammonium salt solution of organic phosphorus in the lower layer w...

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Abstract

The invention provides a comprehensive recovery process for 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 triethylamine and carbonate (or bicarbonate) to layer the solution; extracting triethylamine and hydrochloride from a solution containing the triethylamine hydrochloride; converting the triethylamine hydrochloride into triethylamine; then treating a salt solution containingorganophosphorus to obtain a corresponding 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 comprehensive recovery ofthe 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 comprehensive recovery method 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, hydroch...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/05C07C209/86A01N57/20A01N25/02
CPCC07C209/86A01N57/20A01N25/02C07C211/05
Inventor 刘德亮
Owner 刘德亮
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