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Method of oxidizing N-phosphonometyl to prepare glyphosate

A technology for glyphosate and glyphosate, which is applied to the field of preparing glyphosate by a suspension method, can solve the problems of high cost, pollution and low selectivity of hydrogen peroxide, and achieve the effects of improving atom utilization and low cost.

Active Publication Date: 2008-01-16
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Some of the existing technical solutions use air or oxygen as the oxidant, but activated carbon loaded with heavy metals is required as the catalyst, and there is a certain degree of pollution problem; there are also hydrogen peroxide as the oxidant, but the cost of hydrogen peroxide is much higher than that of oxygen or air. Many, or there are problems such as low selectivity
[0010] In a word, although the existing technology can realize the conversion of diglyphosate to glyphosate, and can realize industrialized production, there are still quite a lot of defects and deficiencies

Method used

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  • Method of oxidizing N-phosphonometyl to prepare glyphosate
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  • Method of oxidizing N-phosphonometyl to prepare glyphosate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take 92.6g (98%) of bisglyphosate, 100g of water, and 0.6g of sodium tungstate into a pressure-resistant reaction vessel with a stirring device, dissolve 120g of 2-ethylhydroanthraquinone in 120g of trioctyl phosphate and stir evenly Then add it into the reaction vessel, stir, continuously feed air into the reaction vessel and raise the temperature, control the pressure in the reaction vessel to 0.2Mpa, keep it warm for 50 minutes when the temperature reaches 70°C, and then reduce the reaction temperature to 50°C after the heat preservation is over. Insulate for 40 minutes; after the end of the insulation, stop feeding the air, cool, let stand for stratification, and separate the upper organic phase and the lower aqueous phase with a separatory funnel. 15g of 10% ferrous sulfate solution was added dropwise to the water phase, cooled to form a large amount of white precipitate, which was separated by filtration, washed twice with water, dried, and sampled for analysis. T...

Embodiment 2

[0039] The reaction solution (I) that obtains with embodiment 1 replaces 2-ethylhydroanthraquinone and trioctyl phosphate in embodiment 1, repeat embodiment 1, the glyphosate content that makes is 95.7%, and yield is 76.3% %.

Embodiment 3

[0041] Take 79.4g (98%) of bisglyphosate, 85.8g of water, and 0.38 g of sodium tungstate and add them into a pressure-resistant reaction vessel with a stirring device, mix 80 g of 2-ethylhydroanthraquinone and 40 g of 2-ethyltetrahydroanthraquinone Mix and dissolve 120g of trioctyl phosphate and trimethylbenzene in a mixed solvent with a weight ratio of 1:1 and stir evenly, then add it into the reaction vessel, stir, continuously feed air into the reaction vessel and raise the temperature, and control the pressure in the reaction vessel at 0.3 Between MPa, when the temperature reaches 65°C, keep it warm for 100 minutes. After the heat preservation is over, reduce the reaction temperature to 40°C and keep it warm for 35 minutes. After cooling, a large amount of white precipitate was formed, which was separated by filtration. The precipitate was washed twice with water, dried, and sampled for analysis. The glyphosate content in the precipitate was 97.1%, and the yield was 79.6%....

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Abstract

This invention relates prepn. of glyphosate by using diglyphosphine as raw material. The prepn. steps are: (1) diglyphosphine-water system is added with alkyl hydroanthraquinone (or hydroanthraquinone) dissolved in organic solvent, in the presence of tungstate as catalyst, and pumping-in oxygen-contained gas to proceed oxidation, (2). The reaction liquid from step (1) is added with ferrous sulfate (or sodium sulfite) as catalyst to proceed decarboxylation, after separation, to obtain the crystal glyphosate. Advantages are: alkyl hydroanthraquinone or hydroanthraquinone can be reused, so there is less loss in prodn; and air or oxygen is used for oxidatio, so heavy metal carried by carbon is not needed; the by-product-hydrogen is useful.

Description

(1) Technical field [0001] The invention relates to a method for preparing glyphosate (PMG) by oxidation of diglyphosate (PMIDA), in particular to a method for preparing glyphosate (PMG) by a suspension method. (2) Background technology [0002] The chemical name of glyphosate is N-phosphonomethylglycine (PMG), and its molecular formula is: [0003] [0004] It is a high-efficiency broad-spectrum herbicide. Because of its good systemic conductivity, it is very effective in the control of a variety of deep-rooted weeds. In recent years, the sales volume has gradually increased. With the glyphosate-resistant transgenic With the gradual promotion of crops, its application range has been further expanded. Now it has become the herbicide with the largest sales volume and the fastest growth rate in the world. The sales volume in 2003 reached 4.7 billion US dollars, accounting for 16% of the entire pesticide market. [0005] At present, there are many technological routes for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 王伟任不凡周曙光邵振威秦龙李丽娟郑红朝
Owner ZHEJIANG XINAN CHEM INDAL GROUP