Synthesis method of N-(Phosphonomethyl) iminodiacetic acid

A synthesis method, the technology of diglyphosate, applied in the field of synthesis of diglyphosate, can solve the problems of increasing the filtration process, affecting the operating environment, complicated process operation, etc., and achieve the effect of improving hydrolysis efficiency, reducing side reactions, and good appearance

Active Publication Date: 2013-04-03
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, iminodiacetonitrile is mainly synthesized by alkaline hydrolysis to synthesize iminodiacetic acid sodium salt. During this period, deamination, dehydration, decolorization, and then adding acid to neutralize iminodiacetic acid sodium salt can be used for the synthesis of diglyphosate. The operation of this process is cumbersome, unnecessary liquid caustic soda is wasted, and a huge ammonia absorption device needs to be built, and there is still amine waste gas in the production process, which affects the environment
[0005] Described in the patent CN101580517 the various advantages of acid hydrolysis iminodiacetonitrile, but the patent introduction will add some solid catalysts (manganese dioxide, potassium permanganate) in the acid hydrolysis process, and the catalyst will be filtered and removed after the reaction. The addition of the catalyst may cause poor appearance of the material and increase the trouble of the filtration process. At the same time, acid gas will inevitably be generated during the acidolysis process, which will affect the operating environment.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 100 g of water, 273 g of hydrochloric acid with a mass fraction of 30%, and 55 g of concentrated sulfuric acid with a mass fraction of 98% were successively put into a 1L kettle, and then 100 g of iminodiacetonitrile with a mass fraction of 95% was slowly added. Then flush nitrogen to 0.2Mpa to replace the gas in the kettle, and then empty it. The reaction kettle was closed and the temperature was raised to 160°C. Nitrogen was flushed into the kettle to a pressure of 1Mpa. Afterwards, keep warm for 6 hours, and start to lower the temperature after the heat preservation is over. When the temperature drops to 80°C, release the pressure, transfer the material to a 1000ml four-neck flask, weigh, and detect. The weight is 502.1g, and the IDA content is 25.81%.

[0030] 94.5 g of solid phosphorous acid was added to the flask, and then the temperature was raised to reflux. 104 g of formaldehyde solution with a mass fraction of 36.5% was added dropwise for 2 hours. After th...

Embodiment 2

[0032] 100 g of water, 273.3 g of hydrochloric acid with a mass fraction of 30%, 110 g of concentrated sulfuric acid with a mass fraction of 98% were successively put into a 1L kettle, and then 100 g of iminodiacetonitrile with a mass fraction of 95% was slowly added. Then flush nitrogen to 0.2Mpa to replace the gas in the kettle, and then empty it. The reaction kettle was closed and the temperature was raised to 160°C. Nitrogen was flushed into the kettle to a pressure of 2Mpa. Afterwards, keep warm for 6 hours, and start to cool down after the heat preservation ends. When the temperature drops to 80°C, release the pressure, transfer the material to a 1000ml four-necked flask, add 94.5g of solid phosphorous acid in the flask, and then heat up to reflux. 104 g of formaldehyde solution with a mass fraction of 36.5% was added dropwise for 2 hours. After the dropwise addition, keep the temperature for 1 hour, then lower the temperature, add 100g of water, add 80g of liquid caus...

Embodiment 3

[0034] Into a 1L autoclave, 427.7 g of hydrochloric acid with a mass fraction of 30%, 95 g of phosphorous acid with a mass fraction of 99%, and 100 g of iminodiacetonitrile with a mass fraction of 95% were slowly added. Then flush nitrogen to 0.2Mpa to replace the gas in the kettle, and then empty it. The reaction kettle was closed and the temperature was raised to 140°C. Nitrogen was flushed into the kettle to a pressure of 0.6Mpa. Afterwards, keep warm for 4 hours, and start to lower the temperature after the heat preservation ends. When the temperature drops to 90°C, the pressure is released, and the material is transferred out, with a weight of 570.4g.

[0035] The above-mentioned material was transferred to a 1000ml four-neck flask, and then the temperature was raised to reflux. Add 104g of formaldehyde solution with a mass fraction of 36.5% dropwise within two hours, and then keep warm for 1.5 hours. After the keep warm, add 100g of water and continue to cool down to 5...

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Abstract

The invention discloses a synthesis method of N-(Phosphonomethyl) iminodiacetic acid (PMIDA) using iminodiacetonitrile as the raw material. The method comprises the following steps: using mixed acid as a hydrolytic reagent, hydrolyzing the iminodiacetonitrile in the mixed acid water solution to obtain acid salt of the iminodiacetic acid, and then performing the condensation reaction of the hydrolyzation solution with phosphorous acid and formaldehyde at the presence of hydrochloric acid to obtain the N-(Phosphonomethyl) iminodiacetic acid, wherein the mixed acid is hydrochloric acid and sulfuric acid, or hydrochloric acid and orthophosphorous acid. According to the invention, the mixed acid is used as a hydrolytic reagent; meanwhile, high temperature and high pressure are adopted to enable the hydrolyzation to be more thorough; at the same time, no waste gas is emitted; and the periodic time of the whole synthesis process is short, the operation is simple, the utilization ratio of the raw materials is high, the side product is few, energy consumption is low and the three wastes are less.

Description

technical field [0001] The invention relates to a synthesis method of diglyphosate, in particular to a synthesis method of diglyphosate, which uses iminodiacetonitrile as a raw material, has short production cycle, simple operation and good product quality. Background technique [0002] Diglyphosate is an important intermediate for the synthesis of glyphosate, and glyphosate has a broad spectrum and high efficiency. With the advantages of low toxicity and other advantages, with the promotion of glyphosate-resistant transgenic crops, its usage is increasing, and it is currently the largest herbicide product in the world. [0003] Diglyphosate is obtained by condensation of iminodiacetic acid, phosphorous acid and formaldehyde under acidic conditions. According to the different preparation methods of iminodiacetic acid, it can be divided into iminodiacetonitrile method and diethanolamine method. At present, in China, iminodiacetonitrile is mainly used as raw material to prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/38
Inventor 孙国庆侯永生陈桂元李志清张杰
Owner SHANDONG WEIFANG RAINBOW CHEM
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