Preparation method of glufosinate-ammonium acid

A technology of glufosinate ammonium and phosphonic acid, applied in the field of pesticide chemistry, can solve the problems of cumbersome process, low separation yield, time-consuming and labor-intensive, etc.

Active Publication Date: 2018-04-06
NANJING REDSUN BIOCHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although most of the ammonium chloride can be removed by treatment with methanol or ethanol after the neutralization solution is concentrated, it is necessary to continue to use alcohol for recrystallization to obtain glufosinate-ammonium with high purity. The process is cumbersome, time-consuming and labor-intensive , the final separation yield is not high

Method used

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  • Preparation method of glufosinate-ammonium acid
  • Preparation method of glufosinate-ammonium acid
  • Preparation method of glufosinate-ammonium acid

Examples

Experimental program
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Effect test

Embodiment 1

[0029] The preparation of embodiment 1 glufosinate-ammonium intermediate aminonitrile

[0030] At room temperature, add 5.61g of freshly distilled acrolein to 10.21g of acetic anhydride, and at 25-30°C, add the mixture of the two above to 13.61g of diethyl methylphosphonite and 4.6 g in a mixture of absolute ethanol. After stirring at 30°C for 2h, add dropwise at 25-28°C 4.9g of sodium cyanide and 10.7g of ammonium chloride in 50mL of ammonia solution (the mass fraction of ammonia water is 25%), react at 30°C for 2h, and react At the end, use a rotary evaporator to remove excess ammonia water, add 30g of dichloromethane to fully extract three times, after combining the extracts, concentrate and completely remove the dichloromethane to obtain the formula The shown glufosinate-ammonium aminonitrile is 20.2g, the purity is 92%, and the yield is 97.9%.

Embodiment 2

[0032] Get glufosinate-ammonium aminonitrile intermediate 103.5g (purity is 92%, 0.5mol) and place in four-necked flask, add sodium hydroxide solution (mass fraction is 10%) 440.2g, heat up to 80 ℃ for hydrolysis, and draw Slight negative pressure deamination, absorb the released ammonia with water, and the hydrolysis ends after 1 hour; add 69.5g of oxalic acid dihydrate to the hydrolyzate, raise the temperature to 80°C for salt-forming reaction, react for 20min, and concentrate 50% of the volume of the reaction solution % water, then cooled to 0°C, filtered to obtain the filtrate and sodium oxalate solid, rinsed the sodium oxalate solid with an appropriate amount of water, combined the washing liquid with the filtrate, concentrated the combined liquid to 40% of the original volume to obtain a concentrated liquid, and then added concentrated 2 times the volume of methanol, cooled to -5 ° C, fully stirred to precipitate glufosinate-ammonium solid, filtered, dried to obtain 75.5g...

Embodiment 3

[0034] Get glufosinate-ammonium aminonitrile intermediate 207.1g (purity is 92%, 1.0mol) and place in four-necked flask, add sodium hydroxide solution (mass fraction is 10%) 880.5g, heat up to 70 ℃ for hydrolysis, and draw Deamination under slight negative pressure, absorb the released ammonia gas with water, and the hydrolysis ends after 1 hour; add 139.8 g of oxalic acid dihydrate to the hydrolyzate, raise the temperature to 60°C to carry out the salt-forming reaction, and concentrate to account for 60% of the volume of the reaction solution after 20 minutes of reaction water, then cooled to 0°C, filtered to obtain the filtrate and sodium oxalate solid, rinsed the sodium oxalate solid with an appropriate amount of water, combined the washing liquid with the filtrate, concentrated the combined liquid to 45% of the original volume to obtain a concentrated liquid, and then added concentrated 1.8 times the volume of methanol, cooled to -5°C, fully stirred to precipitate glufosina...

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Abstract

The invention discloses a preparation method of glufosinate-ammonium acid. The preparation method comprises the following steps: mixing glufosinate-ammonium amino nitrile with an alkali liquid for hydrolysis, and an absorbing produced ammonia gas with water; and adding oxalic acid into obtained hydrolysate for salt forming reaction; cooling a reaction liquid, filtering to obtain a filtrate and solid oxalate, concentrating the filtrate, adding alcohol into a concentrated liquid so as to separate solid glufosinate-ammonium acid, filtering, washing, and drying, so as to obtain the glufosinate-ammonium acid. According to the preparation method, glufosinate-ammonium amino nitrile is hydrolyzed by virtue of sodium hydroxide or calcium hydroxide and reacts with oxalic acid, ammonia generated through hydrolysis is deaminized through a micro-negative pressure and is absorbed with water so as to generate ammonia water, sodium oxalate or calcium oxalate is directly separated due to small water solubility or insoluble property, ammonium chloride is not generated in the whole preparation process, and the waste water quantity is extremely low. Prepared oxalate can be utilized for preparing oxalic acid again for circular use. The purity of prepared glufosinate-ammonium acid can reach above 96.5%, and the yield of prepared glufosinate-ammonium acid is more than or equal to 80%.

Description

technical field [0001] The invention belongs to the field of pesticide chemistry, and in particular relates to a preparation method of glufosinate-ammonium acid. Background technique [0002] Glufosinate-ammonium is an excellent herbicide, and its structure is shown in Formula I: [0003] [0004] As everyone knows, the traditional method of glufosinate-ammonium is generally the Strecker route (Bayer route), and the specific route is as follows: [0005] [0006] The obtained aminonitrile intermediate is hydrolyzed with hydrochloric acid or sulfuric acid to obtain glufosinate-ammonium hydrochloride shown in structural formula II, and glufosinate-ammonium hydrochloride is added with ethylene oxide or propylene oxide to remove hydrochloric acid to obtain structural formula III The shown glufosinate-ammonium acid is then neutralized with ammonia to obtain glufosinate-ammonium. This method uses flammable and explosive ethylene oxide or propylene oxide, which has potential...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 岳瑞宽陈新春薛谊张兰平蒋剑华王福军
Owner NANJING REDSUN BIOCHEM CO LTD
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