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Method for producing N-(phosphonomethyl)iminodiacetic acid and recycling mother solution by hydrogen chloride desalinization

A cyclic application, hydrogen chloride technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problems of uneconomical process, high energy consumption, and large consumption of vapor to concentrate mother liquor, etc. To achieve the effect of simple and easy method, avoid high energy consumption and avoid cumbersome process

Inactive Publication Date: 2014-02-05
CHONGQING UNISPLENDOUR CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

No matter which treatment method is used, it needs to consume a large amount of steam to concentrate the mother liquor, which has high energy consumption, and only part of the sodium chloride can be taken out, and a large amount of saline wastewater still needs to be treated.
On the other hand, excessive phosphorous acid and formaldehyde are used in the reaction, and part of the diglyphosate is still dissolved in the mother liquor of diglyphosate. If the waste water is directly treated and discharged, phosphorous acid, formaldehyde and diglyphosate will be wasted, and the process is extremely unsatisfactory. economy

Method used

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  • Method for producing N-(phosphonomethyl)iminodiacetic acid and recycling mother solution by hydrogen chloride desalinization
  • Method for producing N-(phosphonomethyl)iminodiacetic acid and recycling mother solution by hydrogen chloride desalinization

Examples

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Effect test

Embodiment 1

[0024] 1) Add 420g (4.2mol) of 20% sodium hydroxide solution to a stirring four-necked round bottom flask with a thermometer, and then add 200g (95% , 2.0mol), after the addition, keep warm for 1 hour, iminodiacetonitrile is hydrolyzed to obtain iminodiacetic acid disodium salt, and then heated to 90°C to distill water to remove ammonia;

[0025] 2) Add 730g (31%, 6.2mol) of hydrochloric acid to the disodium salt of iminodiacetic acid obtained in step 1) to acidify to obtain a mixture of iminodiacetic acid and sodium chloride;

[0026] 3) Add 192.5g (98%, 2.3mol) of phosphorous acid to the mixture obtained in step 2), heat, distill water (510g of water has been distilled twice), and add 211g of formaldehyde dropwise between 115 and 120°C (content 37%, 2.6mol), heat preservation reaction for 2 hours after the addition, to synthesize diglyphosate;

[0027] 4) Cool the reaction product obtained in step 3) to 10°C, keep it crystallized for 2 hours, filter, wash the filter cake wi...

Embodiment 2

[0030] 1) Prepare a batch of iminodiacetic acid disodium salt under the same conditions as in Example 1;

[0031] 2) Add the separated sodium chloride obtained in step 5) of Example 1 to the disodium salt of iminodiacetic acid and acidify the mother liquor containing hydrogen chloride to obtain a mixture of iminodiacetic acid and sodium chloride;

[0032] 3) Add 171.5g (98%, 2.05mol) of phosphorous acid to the mixture obtained in step 2), heat, distill 180.2g of water, and add dropwise 180.0g of formaldehyde (content 37%, 2.22mol) between 115 and 120°C ), heat preservation reaction for 2 hours after adding, and synthesize diglyphosate;

[0033] 4) Cool the reaction product obtained in step 3) to 10°C, keep it crystallized for 2 hours, filter, wash the filter cake with 30mL of water, and dry to obtain 431.9g of white bisglyphosate product, with a content of 98.3% and a yield of 93.5%; a mother liquor of 523.6 g;

[0034] 5) Concentrate and distill 73g of water from the mother...

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Abstract

The invention discloses a method for producing N-(phosphonomethyl)iminodiacetic acid and recycling a mother solution by hydrogen chloride desalinization, which comprises the following steps: 1) hydrolyzing iminodiacetonitrile with a sodium hydroxide solution to obtain disodium iminodiacetate; 2) adding hydrogen chloride to acidify the disodium iminodiacetate; 3) adding phosphorous acid and formaldehyde, heating to react to synthesize the N-(phosphonomethyl)iminodiacetic acid; 4) cooling, crystallizing, separating the solid, and drying to obtain the N-(phosphonomethyl)iminodiacetic acid product; 5) adding hydrogen chloride into the mother solution subjected to N-(phosphonomethyl)iminodiacetic acid separation until the concentration of the hydrogen chloride is 15-30% so as to precipitate sodium chloride, and separating and taking the sodium chloride out; and 6) returning the hydrogen-chloride-containing mother solution subjected to sodium chloride separation to the step 2) to acidify the disodium iminodiacetate. The method is simple and easy to implement, can avoid the problems of complex process and high energy consumption in the original desalinization technique for concentrating the mother solution, and can recycle excessive phosphorous acid, formaldehyde and dissolved N-(phosphonomethyl)iminodiacetic acid in the mother solution, thereby reducing the raw material consumption and enhancing the yield.

Description

technical field [0001] The invention relates to a production of diglyphosate and a method for treating mother liquor, and relates to a method for production of bisglyphosate and a method for recycling hydrogen chloride desalination of mother liquor. Background technique [0002] N-phosphoromethylglycine (glyphosate) is an important broad-spectrum herbicide, and a common precursor for its synthesis is N-phosphoromethyliminodiacetic acid (diglyphosate). One of the common synthetic methods is to use iminodiacetonitrile as a raw material, hydrolyze with sodium hydroxide, acidify with hydrochloric acid, and then react with phosphorous acid and formaldehyde to obtain bisglyphosate. The synthetic reaction equation is as follows: [0003] [0004] A large amount of sodium chloride is produced in the reaction process, and the usual treatment method is to take it out in the synthesis of iminodiacetic acid, or to take out the diglyphosate after the diglyphosate reaction is finished,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38C01D3/14
Inventor 丁永良刘佳游欢李静朱丽利郑道敏姚如杰
Owner CHONGQING UNISPLENDOUR CHEM
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