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Method for preparing glyphosate

A technology of glyphosate and glyphosate mother liquor, applied in botany equipment and methods, chemical instruments and methods, chemicals for biological control, etc., can solve high production costs, no description of treatment methods, and high pressure on environmental protection and other issues, to achieve the effect of reducing environmental protection treatment costs, improving atomic economy, and reducing production costs

Active Publication Date: 2009-09-16
捷马化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

By adding alcohols or urea compounds to the reaction mother liquor to react with the by-product formaldehyde to remove it, but the description and examples of this method have no data on the results, and the waste generated is difficult to deal with, and the pressure on environmental protection is great.
[0007] CN101045735A, CN101337979A disclose taking active carbon as catalyzer, utilize oxygen-enriched gas to oxidize PMIDA to prepare the method for glyphosate, have improved the reaction concentration of PMIDA, have solved the problem of high energy consumption brought by reaction with PMIDA saturated solution, but these Methods For the reaction mother liquor containing harmful impurities such as formaldehyde, the treatment method and related result data are not described in the instructions and examples, so a large amount of reaction mother liquor is accumulated. Under the environment, the pressure of environmental protection is huge and the production cost is high
Because it contains harmful impurities such as formaldehyde, the reaction mother liquor cannot be directly recycled into the oxidation reaction system, which will cause a large amount of waste water formed by the reaction mother liquor to accumulate
And because part of the glyphosate is dissolved in the reaction mother liquor, the yield of solid glyphosate is limited
Therefore develop a low-cost method for preparing glyphosate by catalytic oxidation of high-concentration diglyphosate that can recycle glyphosate reaction mother liquor, to improve solid glyphosate yield, and overcome the environmental protection problem that by-product formaldehyde brings, of great value

Method used

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  • Method for preparing glyphosate

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Put 100g of bisglyphosate with a mass fraction of 98.6%, 5g of activated carbon catalyst and 400g of water into a reactor with agitation, air inlet and air outlet, and under the condition of 0.5Mpa pressure and 55°C, feed oxygen to catalyze Oxidation reaction, after the reaction, solid-liquid separation, to obtain 396g reaction mother liquor, wherein the mass fraction of glyphosate is 1.2%, and the mass fraction of formaldehyde is 2.5%. Add the filter cake containing glyphosate crystals and activated carbon into 800g glyphosate saturated solution, raise the temperature to dissolve the glyphosate crystals, separate the activated carbon and glyphosate solution within 30 minutes through the solid-liquid separation device, and collect the activated carbon The catalyst is returned to the catalytic oxidation reaction system for recycling.

[0023] Freeze the glyphosate solution to 5°C to fully crystallize the glyphosate, separate and obtain 65.6g of glyphosate solid, the mass...

Embodiment 2

[0026] 100g mass fraction is 98.6% bisglyphosate, 10g active carbon catalyst and 200g glyphosate solution (reaction mother liquor after membrane separation removes formaldehyde in embodiment 1) drop into the reactor that has stirring, air inlet and gas outlet Inside, under the conditions of 0.8Mpa pressure and 80°C, oxygen was introduced to carry out catalytic oxidation reaction. After the reaction, solid-liquid separation was carried out to obtain 204g reaction mother liquor, wherein the mass fraction of glyphosate was 1.4%, and the mass fraction of formaldehyde was 3.8%. Add the filter cake containing glyphosate crystals and activated carbon into 1200g glyphosate saturated solution, raise the temperature to dissolve the glyphosate crystals, separate the activated carbon and glyphosate solution through the solid-liquid separation device, collect the activated carbon catalyst and return to the catalytic It can be recycled in the oxidation reaction system.

[0027] Freezing gly...

Embodiment 3

[0030] Put 100g of bisglyphosate with a mass fraction of 98.6%, 20g of activated carbon catalyst and 100g of water into a reactor with stirring, air inlet and air outlet, and under the conditions of 1.2Mpa pressure and 110°C, feed oxygen to catalyze Oxidation reaction. After the reaction, solid-liquid separation was carried out to obtain 102 g of reaction mother liquor, wherein the mass fraction of glyphosate was 1.8%. The filter cake containing glyphosate crystals and activated carbon is joined in 1300g glyphosate saturated solution and 200g glyphosate solution (reaction mother liquor that 2 membrane separations remove formaldehyde in the embodiment), temperature rises and dissolves glyphosate crystal, through solidification The liquid separation device separates the activated carbon and the glyphosate solution, collects the activated carbon catalyst and returns it to the catalytic oxidation reaction system for recycling.

[0031] Freeze the glyphosate solution to below 5°C t...

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Abstract

The invention discloses a method for preparing glyphosate. N- (Phosphonomethyl) iminodiacetic acid is in the oxygenation reaction with oxygen in the water medium in the presence of catalyzer such as activated carbon, the solid-liquid separation is performed after the reaction to obtain the crystal with glyphosate and the filter cake with activated carbon, the reaction mother liquor is in the later process; the filter cake is added in the glyphosate saturated solution, after heating and dissolving the activated carbon is separated from the glyphosate solution, the glyphosate solution is cooled and crystallized, after separation the solid glyphosate product and the filter solution are obtained, the filter cake is made into the glyphosate saturated solution; the reaction mother liquor passes through a barrier separation device, the glyphosate in the mother liquor is separated from the by-product such as formaldehyde, the glyphosate mother liquor is recycled in the oxygenation reaction, or used as the glyphosate saturated solution. The invention provides the low-cost method for preparing glyphosate by the catalytic oxidation of high-concentration N- (Phosphonomethyl) iminodiacetic acid by the cyclic utilization of the reaction mother liquor, improving the yield of solid glyphosate and solving the environmental protection problem caused by the byproduct such as formaldehyde.

Description

technical field [0001] The invention relates to a method for preparing glyphosate, more specifically a method for preparing glyphosate by catalytic oxidation of high-concentration diglyphosate by recycling the reaction mother liquor. Background technique [0002] Glyphosate (glyphosate, N-phosphonomethylglycine) is a high-efficiency broad-spectrum herbicide that is widely used in agriculture, forestry, animal husbandry, and horticulture, and has become the world's largest-selling herbicide. [0003] There are many methods for preparing glyphosate, mainly glycine route and iminodiacetic acid (IDA) route etc. Wherein the IDA route is to carry out condensation reaction of IDA and formaldehyde, phosphorous acid source etc. to prepare bisglyphosate (PMIDA, N-phosphonomethyliminodiacetic acid), and then oxidize PMIDA to prepare glyphosate. In the prior art, there are many methods for preparing glyphosate by oxidizing PMIDA, mainly oxygen-enriched gas oxidation method, hydrogen pe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38B01J21/18A01N57/20A01P13/00
CPCY02P20/584
Inventor 王文徐国明周良刘小华刘景伟冯琼蕾
Owner 捷马化工股份有限公司
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