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Method for post-processing N-(phosphonomethyl)iminodiacetic acid oxidation reaction liquid

A technology of oxidation reaction and bisglyphosate, applied in chemical instruments and methods, ammonium halide, organic chemistry, etc., can solve problems such as glyphosate decomposition, achieve the effects of reducing corrosion, reducing treatment and sewage treatment costs, and saving costs

Inactive Publication Date: 2014-08-13
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this process produces a large amount of wastewater containing ammonium chloride, and in the process of concentrating and recovering ammonium chloride, it causes the decomposition of glyphosate in the wastewater

Method used

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  • Method for post-processing N-(phosphonomethyl)iminodiacetic acid oxidation reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The glyphosate solution obtained from the oxidation of diglyphosate is cooled to 30°C to crystallize, and the filtrate obtained by filtration and separation contains about 0.9 wt% of glyphosate, and is directly discharged after simple treatment, and the glyphosate and activated carbon after filtration and separation The solid mixture is mixed in the circulating mother liquor, and at a temperature of 40°C, ammonia gas is slowly introduced, and the reaction is stirred until the pH of the solution is 4.20, and the activated carbon is separated by filtration to obtain a glyphosate ammonium salt solution, and the activated carbon is recovered and recycled after treatment . Glyphosate ammonium salt solution is acidified with hydrogen chloride solution at 20°C, stirred until the pH of the solution is 1.53, filtered and separated to obtain glyphosate crystals, and the filtrate is divided into two parts according to 1:1, one part of the filtrate is used as the circulating mother ...

Embodiment 2

[0022] The glyphosate solution obtained from the oxidation of diglyphosate is cooled to 10°C to crystallize, and the filtrate obtained by filtration and separation contains about 0.8 wt% of glyphosate, and is directly discharged after simple treatment, and the glyphosate and activated carbon after filtration and separation The solid mixture is mixed in the circulating mother liquor, and at a temperature of 20°C, ammonia gas is slowly introduced, and the reaction is stirred until the pH of the solution is 4.20, and the activated carbon is separated by filtration to obtain a glyphosate ammonium salt solution, and the activated carbon is recovered and recycled after treatment . Glyphosate ammonium salt solution is acidified with hydrogen chloride solution at 20°C, stirred and reacted until the pH of the solution is 1.53, filtered and separated to obtain glyphosate crystals, and the filtrate is divided into two parts at a ratio of 1.5:1, and the larger part of the filtrate is used ...

Embodiment 3

[0024] The glyphosate solution obtained from the oxidation of diglyphosate is cooled to 0°C to crystallize, and the filtrate obtained by filtration and separation contains about 0.7wt% glyphosate in mass fraction. After simple treatment, it is directly discharged, and the glyphosate and activated carbon after filtration and separation The solid mixture is mixed in the circulating mother liquor, and at a temperature of 20°C, ammonia gas is slowly introduced, and the reaction is stirred until the pH of the solution is 4.20, and the activated carbon is separated by filtration to obtain a glyphosate ammonium salt solution, and the activated carbon is recovered and recycled after treatment . Ammonium glyphosate solution was acidified with hydrogen chloride solution at 10°C, stirred until the pH of the solution was 1.53, filtered and separated to obtain glyphosate crystals, and the filtrate was divided into two parts at a ratio of 1:0.5, and most of the filtrate was used as a circula...

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Abstract

The invention discloses a method for post-processing a N-(phosphonomethyl)iminodiacetic acid (PMIDA) oxidation reaction liquid. The method comprises the following steps: cooling the PMIDA oxidation reaction liquid and crystallizing, carrying out filtering separation to obtain a solid mixture of glyphosate and activated carbon; adding the solid mixture and a circulating mother liquor together to an ammoniation kettle, introducing ammonia gas and reacting, after the reaction is completed, carrying out filtering separation to obtain the activated carbon; acidifying the filtrate I obtained by filtration with a hydrogen chloride solution and crystallizing, and then carrying out filtering separation to obtain glyphosate crystals and a filtrate II; dividing the filtrate II into two parts, wherein one part of the filtrate II is used as a circulating mother liquor; introducing gas containing hydrogen chloride into the other part of the filtrate II so as to carry out salting out and crystallizing, and carrying out filtering separation to obtain ammonium chloride crystals and a hydrogen chloride solution used for acidifying filtrate I. By virtue of the method, the yield of glyphosate can be improved, and ammonium chloride serving as a byproduct is produced; the process conditions are mild, the emission of wastewater is reduced, the by-product and earnings are increased and the method is of great economic value.

Description

technical field [0001] The invention relates to a post-treatment method of diglyphosate oxidation reaction liquid, and belongs to the field of glyphosate preparation process improvement. Background technique [0002] Glyphosate (PMG), scientific name N-(phosphonomethyl) glycine, also known as Zhencaoning, Roundup, Nongwang, is a highly efficient, low toxicity, low residue, broad-spectrum, environmentally friendly biocidal Systemic herbicides are the most widely produced and used pesticides in the world. At present, an important production route of the industrial production method for preparing glyphosate is to use iminodiacetic acid as a raw material, undergo alkaline hydrolysis and condensation to obtain diglyphosate, and use activated carbon as a catalyst to obtain glyphosate through air oxidation of diglyphosate. In order to separate glyphosate from the catalyst, the existing method is to feed ammonia to convert glyphosate into glyphosate ammonium salt, then use concentr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38C01C1/16
Inventor 艾秋红罗和安何常青游奎一刘平乐王良芥
Owner XIANGTAN UNIV