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Method for preparing N-phosphonomethyliminodiacetic acid

A dipping technology of diglyphosate, which is applied in the new process field of preparing diglyphosate, achieves the effects of improving the reaction yield, overcoming a large amount of salty wastewater, and being environmentally friendly

Active Publication Date: 2011-11-30
HUBEI HUIDA HIGH TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the environmental protection issues of this route have not fundamentally changed.

Method used

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  • Method for preparing N-phosphonomethyliminodiacetic acid
  • Method for preparing N-phosphonomethyliminodiacetic acid
  • Method for preparing N-phosphonomethyliminodiacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Step 1: Preparation of iminodiacetic acid

[0022] Enter 30% ammoniacal liquor 56.7g (1.0mol) and 2.0g ammonium bicarbonate salt in reaction flask, then enter 0.5g catalyst CoCl After stirring, at room temperature, drop the 150ml aqueous solution of 197.0g (2.1mol) chloroacetic acid, After the addition, continue to stir at room temperature for 7 hours, then raise the temperature to above 100°C to distill the distillate, and keep it at this temperature for 5 hours. Sampling and analysis of chloroacetic acid content is less than 1.0% and free chlorine content is less than 1.0%, and the reaction solution is directly processed without treatment. One step reaction. The yield of this step is 90.5%.

[0023] (2) Step 2: Preparation of Diglyphosate (PMIDA)

[0024] Add 82.0g (1.0mol) of phosphorous acid and 156.5g (1.5mol) of hydrochloric acid (35%) to the reaction solution of the previous step, stir evenly and then raise the temperature to above 100°C and start adding 75...

Embodiment 2

[0026] (1) Step 1: Preparation of iminodiacetic acid

[0027] Enter 30% ammoniacal liquor 56.7g (1.0mol) and 2.0g bicarbonate ammonium salt in reaction flask, then enter 0.5g catalyst ZnCl After stirring, add dropwise the 150ml aqueous solution of 197.0g (2.1mol) chloroacetic acid at room temperature, After the addition, continue to stir at room temperature for 7 hours, then raise the temperature to above 100°C to distill the distillate, and keep it at this temperature for 5 hours. Sampling and analysis of chloroacetic acid content is less than 0.5% and free chlorine content is less than 1.0%, and the reaction solution is directly carried out without treatment. One step reaction. The yield of this step is 88.0%.

[0028] (2) Step 2: Preparation of Diglyphosate (PMIDA)

[0029] Add 82.0g (1.0mol) of phosphorous acid and 156.5g (1.5mol) of hydrochloric acid (35%) to the reaction solution of the previous step, stir evenly and then raise the temperature to above 100°C and start ...

Embodiment 3

[0031] (1) Step 1: Preparation of iminodiacetic acid

[0032] Enter 30% ammoniacal liquor 56.7g (1.0mol) and 2.0g ammonium carbonate in reaction flask, then enter 0.8g catalyzer ZnCl After stirring uniformly, add dropwise the 150ml aqueous solution of 197.0g (2.1mol) chloroacetic acid at room temperature, add After finishing, continue to stir at room temperature for 7 hours, then raise the temperature to above 100°C to distill the distillate, and keep at this temperature for 5 hours, take a sample and analyze the content of chloroacetic acid and free chlorine to be less than 1.0%, and proceed to the next step without any treatment reaction. The yield of this step is 85.6%.

[0033] (2) Step 2: Preparation of Diglyphosate (PMIDA)

[0034] Add 82.0g (1.0mol) of phosphorous acid and 156.5g (1.5mol) of hydrochloric acid (35%) to the reaction solution of the previous step, stir evenly and then raise the temperature to above 100°C and start adding 75.0g (1.0mol) of formaldehyde (4...

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Abstract

The invention relates to a novel preparation process of N-phosphonomethyliminodiacetic acid (PMIDA), which is a process method for preparing the PMIDA by using chloroacetic acid, ammonia water, a catalyst, phosphorous acid and formaldehyde in the presence of an inorganic acid. The method comprises the following steps: (1) reacting chloroacetic acid and ammonia water in the presence of ammonium bicarbonate (ammonium carbonate and urea) and a catalyst to prepare iminodiacetic acid; and (2) instead of separating the reaction solution obtained by the previous step, directly adding phosphorous acid and the inorganic acid, adding 40 percent aqueous solution of formaldehyde dropwise at the temperature of above 100 DEG C, cooling to room temperature after the reaction is finished, adjusting the pH value till the isoelectric point of the N-phosphonomethyliminodiacetic acid, cooling, crystallizing, filtering, washing and drying to obtain a N-phosphonomethyliminodiacetic acid product of which the content is over 98 percent. The preparation method starts from a basic chemical raw material; the drawbacks of the generation of large amount of sodium chloride and ammonia and large acid consumption of the production by the conventional iminodiacetonitrile process are overcome; severe conditions are avoided; the operation is simple; environmental protection is realized; and industrial production is easy.

Description

field of invention [0001] The present invention relates to a new preparation process of bisglyphosate (N-phosphonomethyl diacetic acid (PMIDA)), in particular to a method for preparing bisglyphosate in the presence of chloroacetic acid, ammonia water, catalyst, phosphorous acid, formaldehyde and inorganic acids. A new process for phosphine (PMIDA). The preparation method adopts the following steps: (1) chloroacetic acid and ammonia water are prepared in the presence of ammonium bicarbonate (ammonium carbonate, urea) and a catalyst to obtain iminodiacetic acid; (2) the reaction solution in the previous step does not need to be separated, and phosphorous acid is directly added and inorganic acid, drop 40% formaldehyde aqueous solution at a temperature above 100°C, drop to room temperature after the reaction is completed, adjust the pH value to the isoelectric point of diglyphosate, cool and crystallize and filter, wash and dry to obtain the diglyphosate product, the product cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38
Inventor 凌云李永芳陈文王先文
Owner HUBEI HUIDA HIGH TECH CO LTD
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