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Preparation method of N-(phosphonomethyl) iminodiacetic acid

A technology of bisphosphonate and preset temperature, applied in the field of preparing bisphosphonate, can solve the problems of intractability, incomplete absorption of ammonia gas and high cost

Inactive Publication Date: 2018-11-30
泰兴市飞天化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this process is that the amount of 32% NaOH is large, the cost is high, and the ammonia gas generated in the production cannot be completely absorbed, forming disorganized gas in the air
[0009] The shortcoming of prior art comprises: 1. alkaline hydrolysis reaction has used expensive liquid caustic soda (32% ionic membrane caustic, promptly adopts the sodium hydroxide that ion-exchange membrane method electrolyzes salt water and makes) as raw material; 2. alkaline hydrolysis reaction 3. The by-product of the alkaline hydrolysis reaction, ammonia gas, is a hazardous chemical, and the safety level of the workshop is Class B; 4. After the alkaline hydrolysis reaction, there will be no economic value 5. The material condensation of iminodiacetic acid after the alkali hydrolysis reaction contains a large amount of chlorine impurities in the obtained diglyphosate, which needs a large amount of water to wash, and will produce a large amount of phosphorus water, which is difficult to handle

Method used

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  • Preparation method of N-(phosphonomethyl) iminodiacetic acid
  • Preparation method of N-(phosphonomethyl) iminodiacetic acid
  • Preparation method of N-(phosphonomethyl) iminodiacetic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0208] Embodiment 1: Acid hydrolysis reaction small test 1 (iminodiacetonitrile: the first one Hydrochloric acid molar ratio = 1:4.5)

[0209] will be 32.2% No. Put one hydrochloric acid into the acidolysis kettle and heat up to 80°C, dissolve 92% iminodiacetonitrile with 16% of the second hydrochloric acid and heat to 55°C, slowly add the iminodiacetonitrile solution into the kettle, the feeding time is 45min, the temperature of the whole feeding process is 105°C, keep warm for 2 hours after feeding. The iminodiacetic acid content was 19.4% and the conversion rate was 91.3% at the end of the heat preservation.

Embodiment 2

[0210] Embodiment 2: Acid hydrolysis reaction small test 2 (iminodiacetonitrile: the first one Hydrochloric acid molar ratio = 1:5.0)

[0211] will be 32.5% No. Put one hydrochloric acid into the acidolysis kettle and raise the temperature to 83°C, dissolve the iminodiacetonitrile with 16% second hydrochloric acid and heat it to 60°C, slowly add the iminodiacetonitrile solution into the kettle, the feeding time is 55min, and the temperature of the whole feeding process is 106°C , Insulation 2h after feeding. At the end of the heat preservation, the iminodiacetic acid content was 19.3% and the conversion rate was 95.1%.

Embodiment 3

[0212] Embodiment 3: Acid hydrolysis reaction small test 3 (iminodiacetonitrile: the first one Hydrochloric acid molar ratio = 1:5.5)

[0213] will be 31.3% No. Put one hydrochloric acid into the acidolysis kettle and raise the temperature to 82°C, dissolve the iminodiacetonitrile with 18.1% second hydrochloric acid and heat it to 65°C, slowly add the iminodiacetonitrile solution into the kettle, the feeding time is 42min, and the temperature of the whole feeding process is 101°C , Insulation 2h after feeding. The iminodiacetic acid content was 17.5% and the conversion rate was 96.9% at the end of the heat preservation.

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Abstract

The present application discloses a preparation method of N-(phosphonomethyl) iminodiacetic acid by the following steps: acidolysis of iminodiacetonitrile to form an iminodiacetic acid raw material for the preparation of the N-(phosphonomethyl) iminodiacetic acid; and formation of the N-(phosphonomethyl) iminodiacetic acid by use of the iminodiacetic acid, hydrochloric acid, phosphorous acid and formaldehyde.

Description

technical field [0001] The application relates to a method for preparing diglyphosate. Specifically, the application relates to a method of acid-decomposing iminodiacetonitrile to generate diglyphosate as the main raw material iminodiacetic acid, and then using iminodiacetic acid to generate diglyphosate. Background technique [0002] Diglyphosate, namely N-phosphine carboxymethyliminodiacetic acid, is white or light yellow crystal or powder, slightly soluble in water and easily soluble in alkali. Diglyphosate is mainly used in the production of herbicides, and is also an important intermediate widely used in the rubber, pharmaceutical, and dye industries. The main intermediate product in the preparation of bisglyphosate is iminodiacetic acid. [0003] Iminodiacetic acid, NH(CH 2 COOH) 2 , Molecular formula is C 4 h 7 NO 4 . It is white powder or orthorhombic crystal. Iminodiacetic acid has a wide range of uses, mainly used in the manufacture of glyphosate and othe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
CPCC07F9/3808
Inventor 杜连才叶三红曾垚
Owner 泰兴市飞天化工有限公司