Synthetic method for N-phosphonyl methyl imino diacetic acid

A technology of phosphonomethyliminodiacetic acid and iminodiacetonitrile, which is applied in the field of production of N-phosphonomethyliminodiacetic acid, can solve the problems of difficult large-scale production, high production cost, and difficult industrial operation, etc. To achieve the effect of short reaction route and easy purification

Inactive Publication Date: 2007-04-11
重庆三峡英力化工有限公司
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] Prior art such as invention patent US3288846, US5312973, US6118022, US5986128, US6515168 all provide the method that diglyphosate can be prepared industrially with iminodiacetic acid (being called for short IDA) or its salt, phosphorous acid, formaldehyde under strong acid condition, these methods All of them use high-purity substances as raw materials, which are difficult to achieve large-scale production, and the production cost is high, so it is not easy to operate industrially
[0006] Chinese patent application No. 00116540.2 discloses a method for synthesizing diglyphosate with phosphorus trichloride as a raw material, which is characterized in that phosphorus trichloride is hydrolyzed in the system to obtain phosphorous acid and hydrochloric acid simultaneously under vacuum and relatively low temperature conditions. The method is more economical than the traditional method, but because hydrolysis is an exothermic reaction, it is difficult to control, and it is easy to produce by-products, especially the oxidation by-products of phosphorous acid, so this method also has great defects

Method used

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  • Synthetic method for N-phosphonyl methyl imino diacetic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 0.1 mol of iminodiacetonitrile, 0.6 mol of sulfuric acid and 0.4 mol of phosphorous acid into a four-neck flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer, raise the temperature to 150°C, add 0.67 mol of 37% formaldehyde, After the addition was completed, the reaction was carried out at 130° C., and the heating was stopped after the complete conversion of iminodiacetonitrile was detected. The temperature was lowered, crystallization was precipitated, filtered by suction, and dried to obtain 86 grams of bisglyphosate with a content of 98.5%.

Embodiment 2

[0025] Add 0.1 mole of iminodiacetonitrile, 0.9 mole of phosphoric acid and 0.8 mole of phosphorous acid into a four-neck flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer, raise the temperature to 80°C, add 1 mole of 37% formaldehyde, After the addition was completed, the reaction was carried out at 90° C., and the heating was stopped after the complete conversion of iminodiacetonitrile was detected. The temperature was lowered, crystals were precipitated, filtered with suction, and dried to obtain 128 grams of bisglyphosate with a content of 98.5%.

Embodiment 3

[0027] Add 0.1 mol of iminodiacetonitrile, 0.3 mol of phosphoric acid and 0.5 mol of phosphorous acid into a four-neck flask equipped with a stirrer, reflux condenser, dropping funnel and thermometer, raise the temperature to 130°C, add 0.56 mol of 37% formaldehyde, After the addition was completed, the reaction was carried out at 150° C., and the heating was stopped after the complete conversion of iminodiacetonitrile was detected. The temperature was lowered, crystals were precipitated, filtered by suction, and dried to obtain 48 grams of bisglyphosate.

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Abstract

The present invention provides technological process of preparing PMIDA as the intermediate of glyphosate, and features that imino diacetonitrile is used as material in preparing PMIDA (N-phosphonyl methyl imino diaceteic acid).

Description

technical field [0001] The invention relates to a method for producing N-phosphonomethyliminodiacetic acid (bisglyphosate) by using iminodiacetonitrile as a raw material. Background technique [0002] In the industrial production process, bis-glyphosate is mainly used to prepare glyphosate. The chemical name of glyphosate is N-phosphonomethylglycine. It is a highly effective broad-spectrum herbicide. Because of its good systemic conduction performance, it is very effective in the control of a variety of deep-rooted weeds. In recent years, With the gradual promotion of glyphosate-resistant genetically modified crops, its application range has been further expanded, and it has become the largest and fastest-growing herbicide in the world. There are two main production methods for glyphosate acid that are now industrialized: one is the IDA route using hydrocyanic acid or diethanolamine as the starting material used by Monsanto in the United States; The dialkyl phosphite route...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 郭钰来顾爱宏李星田金平尹应武
Owner 重庆三峡英力化工有限公司
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