New technique for preparing glyphosate by oxidizing N-Phosphonomethyl iminodiacetic acid in air

A technology of diglyphosate and air, which is applied in the new process field of preparing glyphosate by air oxidation of diglyphosate, which can solve the problems of catalyst recovery difficulty, increased difficulty of product separation and purification, and failure to fundamentally eliminate the use of hydrogen peroxide.

Active Publication Date: 2007-12-26
BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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  • Abstract
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  • Application Information

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Problems solved by technology

The disadvantages of these methods include several aspects: 1) the use of expensive noble metal catalysts makes it difficult to recover the catalysts, and the catalysts are easily lost; 2) the preparation methods of organic ligands are complicated, which increases the difficulty of product separation and purification
3) The catalyst needs to be replaced regularly; 4) There are patent restrictions
Although this method reduces the amount of hydrogen peroxide used, it does not eliminate the use of hydrogen peroxide at all
The disadvantage of this method is that diglyphosate needs to react with oxygen or air under a certain pressure to partially react

Method used

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  • New technique for preparing glyphosate by oxidizing N-Phosphonomethyl iminodiacetic acid in air

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] The ultrasonic generator used in this experiment has a frequency of 25KHz and a power of 100W.

[0028] Add 2.5 grams of gac (charcoal is prepared as a raw material) in the there-necked flask, 50 milliliters of water, 10 grams of PMIDA, heat and stir, feed air into reaction solution, open ultrasonic generator, temperature rises to 40 ℃, detects that diglycophosphine is completely Reaction, the reaction time is 15 hours, the glyphosate reaction selectivity is 89.1%, and finally 6.49g of glyphosate raw powder is obtained, with a content of 99%.

Embodiment 2

[0030] The reclaimed gac in embodiment 1, 100 milliliters of water, 10 grams of PMIDA, heat and stir, feed into air to reaction solution, open ultrasonic generator, temperature rises to 80 ℃, detects that diglyphosate disappears, and reaction stops, and reaction time 12 hours, the glyphosate reaction selectivity was 90.68%, and finally 6.53g of glyphosate powder was obtained, with a content of 99.5%.

Embodiment 3

[0032] The reclaimed gac in embodiment 2, 100 milliliters of water, 10 grams of PMIDA, heat and stir, feed into air to reaction solution, open ultrasonic generator, temperature rises to 90 ℃, detects that diglyphosate disappears, and reaction stops, and reaction time 12 hours, the glyphosate reaction selectivity was 88.4%, and finally 6.24g of glyphosate powder was obtained, with a content of 99.4%.

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Abstract

This invention discloses a method for oxidizing N-(carboxymethyl)-N-(phosphonomethyl)-glycine into glyphosate with air or oxygen as the oxidant under the catalysis of activated carbon or carbon nanotubes and ultrasonic wave. The method has such advantages as high yield, high reaction selectivity, high product purity, no need for expensive catalyst or reductant, and no need for H2O2.

Description

technical field [0001] The invention relates to a new process for synthesizing glyphosate, an important pesticide-herbicide, by catalytic oxidation of diglyphosate. Background technique [0002] Glyphosate (glyphosate, N-(phosphonomethyl)-glycine) is a herbicide screened and synthesized by Monsanto Chemical Company in the United States in the 1960s, which belongs to amino acid derivatives. The good biological activity of glyphosate makes it a widely used high-efficiency, low-toxicity, post-emergent herbicide, and its current annual sales rank first among pesticide products. [0003] The synthesis methods of glyphosate mainly include glycine method and iminodiacetic acid method. The glycine method mainly uses glycine as a raw material to obtain glyphosate through reaction. Due to the low yield and high cost of the method, and because a large amount of alkali is consumed when recovering the solvent and the catalyst, equipment, energy consumption and workload are increased. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 郭钰来尹应武田金平阎慧娟冯倩
Owner BEIJING ZIGUANG YINGLI CHEM TECH CO LTD
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