Synthesis method of glufosinate-ammonium

A synthesis method and technology of glufosinate-ammonium, applied in the field of pesticides, can solve the problems of high resin price, low-value inorganic waste salt, difficult separation, etc., and achieve the effects of serious loss, large amount of three wastes, and high cost

Active Publication Date: 2021-06-29
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of synthetic method is accompanied by the generation of inorganic salts in the preparation process, such as sodium sulfate, sodium chloride, ammonium chloride, ammonium sulfate, etc., because the solubility of glufosinate-ammonium and inorganic salts in water is very large, it is difficult to adopt conventional methods. Separation, generally adding water-miscible organic solvents such as methanol, ethanol, etc., using the different solubility of glufosinate-ammonium and inorganic salts in organic solvents for separation, but the post-salt removal method is not only complicated, but also consumes a lot of solvents, while producing a large amount of low-value inorganic waste salt
[0006] In order to solve the above technical problems, the prior art adopts the method of ion exchange resin to separate the inorganic salt in the glufosinate-ammonium solution, although the final glufosinate-ammonium product can reach Very high purity, but the resin used in this method is expensive, complicated to operate, the yield is only below 80%, and the loss of glufosinate-ammonium is serious
This makes it difficult to promote the industrial production of glufosinate-ammonium

Method used

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  • Synthesis method of glufosinate-ammonium

Examples

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Effect test

Embodiment 1

[0039] The present embodiment provides a kind of preparation method of glufosinate-ammonium, comprising the steps:

[0040] In the 2L autoclave, add 5-[2 (hydroxyl (methyl) phosphono) ethyl] hydantoin 210g (1mol), 20wt% ammoniacal liquor 85g (1mol), water 900g (50mol), catalyst MTBD7.6g ( 0.05mol), heated to 160°C and controlled the pressure at 2.0MPa to react for 2h. After the reaction finished, the reaction solution was concentrated under reduced pressure to reclaim ammonia and catalyst, and the resulting concentrated solution was added with 350g methanol to reflux for 2h, then naturally dropped to room temperature, filtered and dried to obtain glufosinate-ammonium 195.3g after crystallization, detected by HPLC, its content was 97.1%, the yield is 95.8%.

Embodiment 2

[0042] The present embodiment provides a kind of preparation method of glufosinate-ammonium, comprises the steps:

[0043] In the 2L autoclave, add 5-[2 (hydroxyl (methyl) phosphono) ethyl] hydantoin 210g (1mol), 25wt% ammoniacal liquor 136g (2mol), water 900g (50mol), catalyst MTBD3.1g ( 0.02mol), heated to 160°C and controlled the pressure at 2.5MPa to react for 2h. After the reaction was finished, the reaction solution was concentrated under reduced pressure to recover ammonia water and catalyst. The resulting concentrated solution was added with 350 g of methanol and refluxed for 2 hours, then naturally lowered to room temperature, filtered and dried to obtain 197.1 g of glufosinate-ammonium, which was detected by HPLC with a content of 97.0%. , yield 96.6%.

Embodiment 3

[0045] The present embodiment provides a kind of preparation method of glufosinate-ammonium, comprises the steps:

[0046]In the 2L autoclave, add 5-[2 (hydroxyl (methyl) phosphono) ethyl] hydantoin 210g (1mol), 20wt% ammoniacal liquor 170g (2mol), water 900g (50mol), catalyst MTBD1.5g ( 0.01mol), heated to 160°C and controlled the pressure at 1.0MPa for 3h. After the reaction was finished, the reaction solution was concentrated under reduced pressure to recover ammonia water and the catalyst. The resulting concentrated solution was added with 350 g of methanol and refluxed for 2 hours, then naturally lowered to room temperature, filtered and dried to obtain 192.7 g of glufosinate-ammonium, which was detected by HPLC with a content of 96.9%. , yield 94.3%.

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Abstract

The invention relates to the field of pesticides, in particular to a synthesis method of glufosinate-ammonium. The synthesis method of glufosinate-ammonium comprises the following steps: reacting a mixed aqueous solution of a hydantoin derivative, volatile alkali and a catalyst under 1.0-2.5 MPa, and after the reaction is finished, carrying out post-treatment to obtain glufosinate-ammonium, wherein the catalyst is a guanidine compound. The synthesis method of glufosinate-ammonium provided by the invention jumps out of the thought of separating glufosinate-ammonium from inorganic salt in the prior art, creatively adopts the mutual cooperation of volatile alkali and the catalyst (guanidine compound), and hydrolyzes the hydantoin derivative under the specific pressure of 1.0-2.5 MPa, so that the hydantoin compound is thoroughly hydrolyzed, the yield of glufosinate-ammonium is improved, meanwhile, the reaction time is shortened, acid-base neutralization is not needed after the reaction is finished, inorganic salt is not generated, generation of the inorganic salt in the glufosinate-ammonium preparation process is fundamentally eradicated, three wastes are not generated, the yield of glufosinate-ammonium is high, and industrial popularization is easy.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a synthesis method of glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium (Glufosinafe) is a broad-spectrum contact-killing herbicide, which has the characteristics of wide herbicidal spectrum, low toxicity, high activity and good environmental compatibility. The structural formula is as follows: [0003] [0004] Since the drug effect of glufosinate-ammonium is only transmitted in the leaves and does not transfer to other places, it will not act on the roots of unearthed plants, so its phytotoxicity is relatively small; and the soil treated with glufosinate is subsequently sown All kinds of plants, their growth will not be affected. As an excellent herbicide, glufosinate-ammonium has the characteristics of high efficiency, low toxicity and non-selectivity. It is currently the second largest genetically modified crop-tolerant herbicide in the world after glyphos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
CPCC07F9/30Y02P20/584
Inventor 范立攀史秀肖高倩贾成国
Owner HEBEI VEYONG BIO CHEM
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