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Method for producing glyphosate by adopting PMIDA as raw material

A technology of glyphosate and diglyphosate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as not easy to operate, decomposition and consumption of hydrogen peroxide, and achieve easy Operation and control, process mild effect

Inactive Publication Date: 2015-08-12
ANHUI YINONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese patent CN102382136A discloses a new hydrogen peroxide oxidation process of glyphosate, and discloses that the reaction temperature reaches 66±1°C, and the hydrogen peroxide is added dropwise for 40-45 minutes, which directly leads to the decomposition and consumption of hydrogen peroxide
However, in theory, alkali will promote the decomposition of hydrogen peroxide, so it is not easy to adjust by adding alkali

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] A kind of method adopting diglyphosate as raw material to produce glyphosate comprises the following steps:

[0017] (1) Using hydrogen peroxide as the oxidant and activated carbon as the catalyst, the oxidation reaction is carried out under acidic conditions at a temperature of 50±2°C; the mass ratio of diglyphosate to activated carbon is 1:0.05, and the molar ratio of diglyphosate to hydrogen peroxide It is 1:1.0-1.1, and the time of adding hydrogen peroxide in the oxidation reaction: 4 hours / 8 thousand moles of bisglyphosate;

[0018] (2) Continue to keep warm for 2 hours after the oxidation reaction is over. After the heat preservation is over, cool down to 8°C, filter, dissolve the catalyst-containing glyphosate filter cake with hot water at 80-90°C, and then filter to separate the catalyst;

[0019] (3) The concentrated glyphosate solution obtained by filtration and separation is cooled to crystallize, centrifuged and dried, and the original glyphosate powder is o...

Embodiment 2

[0021] A kind of method adopting diglyphosate as raw material to produce glyphosate comprises the following steps:

[0022] (1) Using hydrogen peroxide as the oxidant and activated carbon as the catalyst, the oxidation reaction is carried out under acidic conditions at a temperature of 50±2°C; the mass ratio of diglyphosate to activated carbon is 1:0.1, and the molar ratio of diglyphosate to hydrogen peroxide The ratio is 1:1.0-1.1, the time for adding hydrogen peroxide in the oxidation reaction: 5 hours / 8 thousand moles of diglyphosate;

[0023] (2) Continue to keep warm for 3 hours after the oxidation reaction is over. After the heat preservation is over, cool down to 10°C, filter, dissolve the catalyst-containing glyphosate filter cake with hot water at 80-90°C, and then filter to separate the catalyst;

[0024] (3) The concentrated glyphosate solution obtained by filtration and separation is cooled to crystallize, centrifuged and dried, and the original glyphosate powder i...

Embodiment 3

[0026] A kind of method adopting diglyphosate as raw material to produce glyphosate comprises the following steps:

[0027] (1) Using hydrogen peroxide as the oxidant and activated carbon as the catalyst, the oxidation reaction is carried out under acidic conditions at a temperature of 50±2°C; the mass ratio of diglyphosate to activated carbon is 1:0.20, and the molar ratio of diglyphosate to hydrogen peroxide The ratio is 1:1.0-1.1, the time for adding hydrogen peroxide in the oxidation reaction: 5 hours / 8 thousand moles of diglyphosate;

[0028] (2) Continue to keep warm for 5 hours after the oxidation reaction is over. After the heat preservation is over, cool down to 12°C, filter, dissolve the catalyst-containing glyphosate filter cake with hot water at 80-90°C, and then filter to separate the catalyst;

[0029] (3) The concentrated glyphosate solution obtained by filtration and separation is cooled to crystallize, centrifuged and dried, and the original glyphosate powder ...

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Abstract

The present invention relates to a method for producing glyphosate by adopting PMIDA as a raw material. The method comprises: carrying out an oxidation reaction at a temperature of 50+ / -2 DEG C under an acid condition by adopting hydrogen peroxide as an oxidation agent and by adopting active carbon as a catalyst, continuously maintaining the temperature for a plurality of hours after completing the oxidation reaction, carrying out cooling filtration, dissolving the glyphosate filter cake containing the catalyst with hot water, carrying out filtration separation on the catalyst, carrying out cooling crystallization on the obtained glyphosate solution, and carrying out centrifugal drying and drying to obtain the glyphosate raw powder. According to the present invention, the original process for producing the glyphosate through PMIDA oxidation with hydrogen peroxide is importantly improved, the total glyphosate yield can achieve 96%, the raw powder yield achieves 89%, and the process is mild and is easy to operate and control.

Description

technical field [0001] The invention relates to a method for producing glyphosate by using diglyphosate as a raw material. Background technique [0002] The existing techniques for producing glyphosate by oxidation of diglyphosate include air oxidation and hydrogen peroxide oxidation. The former uses cheap air as an oxidant, but because it is a gas-liquid-solid heterogeneous oxidation reaction, it must be pressurized to have sufficient reaction speed, and the equipment investment is large, and the cost of air pressurization is also high. The latter uses hydrogen peroxide as the oxidant, operates under normal pressure, and requires less investment in equipment. For a long time, when using hydrogen peroxide to oxidize diglyphosate to produce glyphosate, sodium tungstate is used as a catalyst, and ferrous sulfate and sodium sulfite are used as reducing agents after oxidation. The reaction steps are long, and the system components are complex after the reaction. Important The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 徐益峰方润
Owner ANHUI YINONG CHEM
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