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Method for recycling glyphosate from glyphosate mother liquor of IDA method

A technology of glyphosate mother liquor and glyphosate, which is applied in the field of glyphosate recovery, can solve problems such as transformation or upgrading, and achieve the effects of improving recovery rate, reducing energy consumption costs, and strengthening economic value

Active Publication Date: 2011-08-24
SHANDONG WEIFANG RAINBOW CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This means that the current mother liquor treatment process of glyphosate enterprises can no longer meet the current requirements and must be changed or upgraded

Method used

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  • Method for recycling glyphosate from glyphosate mother liquor of IDA method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Get glyphosate content and be 1.0% IDA method glyphosate mother liquor waste water 5kg, add NH 3 Adjust the pH to 2.5, then filter to remove solid impurities. The filtered mother liquor was loaded into a membrane concentration device to obtain 0.82 kg of a membrane dope with a glyphosate content of 6.0%. Ammonia water was added to the membrane dope to adjust the pH to 5, and the temperature was 50° C. and the vacuum degree was 0.09 MPa to distill and dehydrate under reduced pressure to obtain 0.25 kg of a secondary concentrated solution with a glyphosate content of 19.1%. Add hydrochloric acid to the secondary concentrated solution to adjust the pH to 1.0, slowly cool down to room temperature for crystallization, filter and wash with water after crystallization to obtain 53g of a solid with a glyphosate content of 75%, and finally recrystallize to obtain a glyphosate content of 95.5% The solid 38g. During the whole process, the recovery rate of glyphosate reached 72.6...

Embodiment 2

[0023] Take 5 kg of IDA method glyphosate mother liquor wastewater with a glyphosate content of 1.0%, add NaOH to pH 4, and then filter to remove solid impurities. The filtered mother liquor is packed into a membrane concentration device to obtain 0.62 kg of a membrane dope with a glyphosate content of 7.9%. Add ammonia to the membrane dope to adjust the pH to 6. At a temperature of 60° C. and a vacuum of 0.095 MPa, the Press distillation dehydration, obtain the secondary concentrated solution 0.22kg of glyphosate content 22%. Add hydrochloric acid to the secondary concentrate to adjust the pH to 1.2, slowly lower to normal temperature for crystallization, filter and wash with water after crystallization to obtain 59g of a solid with a glyphosate content of 71%, and finally recrystallize to obtain a glyphosate content of 95.0% Solid 37.5 g. During the whole process, the recovery rate of glyphosate reached 71.2%.

Embodiment 3

[0025] Take 5 kg of IDA method glyphosate mother liquor wastewater with a glyphosate content of 1.0%, add KOH to adjust the pH to 5, and then filter to remove solid impurities. The filtered mother liquor was loaded into a membrane concentration device to obtain 0.62 kg of a membrane dope with a glyphosate content of 8.6%. KOH was added to the membrane solution to adjust the pH to 6, and the temperature was 80° C. and the vacuum degree was 0.095 MPa for vacuum distillation and dehydration to obtain 0.22 kg of a concentrated solution with a glyphosate content of 22%. Add hydrochloric acid to the secondary concentrate to adjust the pH to 1.5, slowly drop to normal temperature for crystallization, filter and wash with water after crystallization to obtain 59 g of solids with a glyphosate content of 71%, according to the glyphosate described in claim 1 or 2 The recovery method is characterized in that: the alkali regulator is finally recrystallized to obtain 37.5 g of a solid with ...

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Abstract

The invention discloses a method for recycling glyphosate from glyphosate mother liquor of IDA method. The method adopts the following steps: entering the glyphosate mother liquor of IDA method into a membrane concentration device after pre-treatment to obtain primary glyphosate concentrated liquor; adding alkali conditioning agent in the primary glyphosate concentrated liquor, and carrying out distillation, concentration and dehydration in an evaporator to obtain secondary glyphosate concentrated liquor; adding acid in the secondary glyphosate concentrated liquor for conditioning, crystallizing at normal temperature, filtering and washing with water to obtain glyphosate solid, and re-crystallizing the glyphosate solid to obtain glyphosate bulk drug. The method combines membrane method and evaporating concentration, so that the yield of glyphosate is high, rectificating is unnecessary, the production cost is lowered, energy consumption is saved, environment protection pressure is reduced, and higher economic value is obtained.

Description

technical field [0001] The invention relates to a method for recovering glyphosate in an aqueous solution, in particular to a new method for recovering glyphosate from glyphosate mother liquor produced by an IDA method. Background technique [0002] As a high-efficiency, broad-spectrum, low-toxicity herbicide, glyphosate has become the herbicide with the fastest sales and growth rate in the world. At present, the preparation of glyphosate in China mostly uses the alkyl ester method and iminodiacetic acid Law. [0003] During the production of glyphosate by the iminodiacetic acid (IDA) method, a large amount of mother liquor with a glyphosate content of about 1% is produced. The existing technology is to evaporate and dehydrate the mother liquor with steam or use a membrane method to concentrate it to obtain a glyphosate content of 10%. % water agent. With the gradual improvement of the country's environmental protection requirements, the Ministry of Agriculture, the Minist...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 刘月栋孙国庆陈琦侯永生李志清路宁亚
Owner SHANDONG WEIFANG RAINBOW CHEM
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