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Preparation method of N-(phosphonomethyl)iminodiacetic acid

A technology of bisglyphosate and ammonium chloride, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, ammonium halide, etc., can solve problems such as cost, safety, environmental protection and high energy consumption, and save equipment investment , Realize the utilization of resources and solve the effect of environmental protection treatment problems

Active Publication Date: 2011-06-22
捷马化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As mentioned above, in the prior art of preparing bisglyphosate, there are problems in various aspects such as cost, safety, environmental protection, high energy consumption, etc.

Method used

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  • Preparation method of N-(phosphonomethyl)iminodiacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Put 100g (1mol) of iminodiacetonitrile and 180g of water into a reaction flask with stirring, raise the temperature to 40°C, and evenly add 138.9g (1mol) of phosphorus trichloride dropwise for acidolysis reaction. After the dropwise addition, raise the temperature to 80°C, keep warm for 4 hours. Add 81.1g mass fraction of 37% formaldehyde (1mol) at 90°C and keep it warm for 5 hours to generate diglyphosate, cool down to 10°C, crystallize, separate solid and liquid, wash with water, and dry to obtain a mass fraction of 98.1% bisglyphosate The product is 199g, the yield is 86%; the reaction mother liquor is 702g, and the mass fraction of bisglyphosate is 2.2%.

[0016] Introduce 18g of ammonia gas into 702g of reaction mother liquor, PH=3, heat up and evaporate and dehydrate 270g, ammonium chloride is supersaturated and precipitated, cool and crystallize, and separate solid and liquid to obtain 110g of ammonium chloride, mass fraction 99.3%; concentrate mother liquor 285g...

Embodiment 2

[0018] Put 100g (1mol) of iminodiacetonitrile, 720g of water and 285g of the concentrated mother liquor in Example 1 into a stirred reaction flask, raise the temperature to 70°C, and evenly drop 277.8g (2mol) of phosphorus trichloride to carry out the acidolysis reaction , after the dropwise addition was completed, the temperature was raised to 130° C., and the temperature was kept for 1 hour. Add 162.2g of 37% formaldehyde (2mol) at 120°C and keep it warm for 2 hours to generate diglyphosate, cool down to 10°C, crystallize, and separate the solid and liquid to obtain 208.1g of diglyphosate with a mass fraction of 98.2%. The yield is 90%; the reaction mother liquor is 1298g, and the mass fraction of bis-glyphosate is 3.9%.

[0019] Introduce 105g of ammonia gas into 1298g of reaction mother liquor, PH=7, heat up to evaporate and dehydrate 700g, cool and crystallize, and separate solid and liquid to obtain 300g of ammonium chloride, with a mass fraction of 99.0%; 360g of concen...

Embodiment 3

[0021] Put 100g (1mol) of iminodiacetonitrile and 540g of water into a reaction flask with stirring, raise the temperature to 50°C, and evenly add 187.5g (1.35mol) of phosphorus trichloride dropwise for acidolysis reaction. After the dropwise addition, raise the temperature to 100°C for 2 hours. Add 121.6g mass fraction of 37% formaldehyde (1.5mol) at 100°C, keep warm for 3 hours to generate bisglyphosate, deacidify water 300g, add water 300g, cool down to 15°C, crystallize, solid-liquid separation to obtain a mass fraction of 98.5 207.5g of bis-glyphosate product, the yield is 90%; the reaction mother liquor is 742g, and the mass fraction of bis-glyphosate is 2.6%.

[0022] Introduce 29g of ammonia gas into 742g of reaction mother liquor, pH=5.5, heat up to evaporate and dehydrate 378g, cool and crystallize, and separate solid and liquid to obtain 123g of ammonium chloride, with a mass fraction of 99.2%; 252g of concentrated mother liquor will be used until the next batch of ...

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Abstract

The invention discloses a preparation method of N-(phosphonomethyl)iminodiacetic acid, which comprises the following steps: (1) putting iminodiacetonitrile into water, dropwisely adding phosphorus trichloride while controlling the temperature at 40-70 DEG C and stirring, heating to 80-130 DEG C after the dropwise adding process is finished, keeping the temperature for 1-4 hours to generate a mixed solution containing iminodiacetic acid hydrochloride, phosphorous acid, ammonium chloride and hydrochloric acid, adding formaldehyde into the mixed solution to carry out condensation reaction at 90-120 DEG C, cooling to crystallize, and carrying out solid-liquid separation to obtain an N-(phosphonomethyl)iminodiacetic acid product and a reaction mother solution containing ammonium chloride; and (2) adding ammonia into the reaction mother solution, regulating the pH value to 3-7, dehydrating by evaporation to concentrate until the ammonium chloride is oversaturated to precipitate, cooling to crystallize, carrying out solid-liquid separation to obtain ammonium chloride and a concentrated mother solution, and concentrating the mother solution for cyclic use. The invention fundamentally avoids the generation of a great deal of waste liquor containing sodium chloride, saves the investment into ammonia recovery equipment, simplifies the technique, increases the equipment utilization rate, and meanwhile recycles the byproduct ammonium chloride and the mother solution successfully.

Description

technical field [0001] The present invention relates to a preparation method of diglyphosate, more specifically a method for preparing diglyphosate with iminodiacetonitrile, phosphorus trichloride and formaldehyde as raw materials, and the recovery of by-product ammonium chloride and mother liquor Approach. Background technique [0002] Diglyphosate (PMIDA) is the main chemical intermediate for the production of the broad-spectrum herbicide glyphosate, and has a broad market prospect. The production method of bisglyphosate is mainly formed by the condensation reaction of iminodiacetic acid or its alkali metal salt with phosphorous acid and formaldehyde. According to the different raw materials and processes for preparing iminodiacetic acid (IDA), the production methods are as follows : [0003] 1. The diethanolamine method, as disclosed in Chinese patents such as CN1563021A, CN101696225A, and CN1484647, uses diethanolamine and sodium hydroxide as raw materials to prepare i...

Claims

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Application Information

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IPC IPC(8): C07F9/38C01C1/16
Inventor 王文周良徐国明刘小华刘景伟翁建新冯琼蕾邹有英
Owner 捷马化工股份有限公司
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