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Preparation method of glufosinate-ammonium

A technology of glufosinate-ammonium and hydantoin, applied in the field of pesticides, can solve the problems of high energy consumption and complicated post-treatment of inorganic waste salt

Active Publication Date: 2021-07-06
HEBEI VEYONG BIO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] A large amount of inorganic waste salts will be produced in the process of preparing glufosinate-ammonium in the above-mentioned prior art, resulting in complicated post-processing; or the use of toxic raw material barium hydroxide; or the problems of high energy consumption in the recycling of a large amount of inorganic waste salts obtained, The invention provides a preparation method of glufosinate-ammonium, which does not need to use toxic raw materials and does not produce inorganic salts in the preparation process

Method used

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Examples

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Embodiment 1

[0043] The present embodiment provides a kind of preparation method of glufosinate-ammonium, comprising the steps:

[0044] Add 210g (1mol) of 5-[2-(hydroxy(methyl)phosphono)ethyl]hydantoin and 210g of water into a 1L autoclave, then fill it with carbon dioxide to a pressure of 1MPa, and raise the temperature to 120°C (system pressure is 1.4MPa ) to react for 15h. After the completion of the reaction, release carbon dioxide and water vapor (compress and recover while releasing), then concentrate under reduced pressure to 215g, then add 215g methanol, heat and reflux for 2h, crystals are precipitated, filter after cooling, and dry to obtain glufosinate-ammonium 175g, after HPLC Its content is detected to be 96.5%.

[0045] 1 H-NMR (400MHz, D 2 O) δ: 3.64 (t, 1H), 1.90-1.94 (m, 2H), 1.40-1.52 (m, 2H), 1.09 (d, 3H).

[0046] 13 C-NMR (100MHz, D 2 O) δ: 14.46 (d, j=93), 24.16 (d, j=2), 26.51 (d, j=91), 55.05 (d, j=15), 174.13.

Embodiment 2

[0048] The present embodiment provides a kind of preparation method of glufosinate-ammonium, comprising the steps:

[0049] Add 105g (0.5mol) of 5-[2-(hydroxy(methyl)phosphono)ethyl]hydantoin and 1050g water into a 2L autoclave, then fill it with carbon dioxide to a pressure of 4MPa, and raise the temperature to 180°C (the system pressure is 5.5MPa) for 4 hours. After the reaction was completed, carbon dioxide and water vapor were released (compressed and recovered while releasing), then concentrated under reduced pressure to 179g, then added 895g of methanol, and heated to reflux for 2h to have crystallization, filtered after cooling, and dried to obtain glufosinate-ammonium 93.1g. Its content was detected by HPLC to be 98.9%.

Embodiment 3

[0051]The present embodiment provides a kind of preparation method of glufosinate-ammonium, comprising the steps:

[0052] Add 210g (1mol) of 5-[2-(hydroxy(methyl)phosphono)ethyl]hydantoin and 420g of water into a 1L autoclave, then fill it with carbon dioxide to a pressure of 2MPa, and raise the temperature to 140°C (system pressure is 2.8MPa ) to react for 10h. After the reaction was completed, carbon dioxide and water vapor were released (compressed and recovered while releasing), then concentrated under reduced pressure to 263g, then added 526g of methanol, heated to reflux for 2h, crystals were separated out, filtered after cooling, and dried to obtain 192g of glufosinate-ammonium. Its content was detected by HPLC to be 98.7%.

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Abstract

The invention relates to the field of pesticides, and in particular relates to a preparation method of glufosinate-ammonium. The preparation method of the glufosinate-ammonium comprises the following steps: introducing carbon dioxide into an aqueous solution of hydantoin derivatives until the system pressure is 1 to 4MPa, then heating to 120-180 DEG C for reaction, and after the reaction is finished, carrying out post-treatment to obtain the glufosinate-ammonium. Carbon dioxide is filled into an aqueous solution of the hydantoin derivatives until the system reaches specific pressure, so that more carbon dioxide is dissolved in water, that is, the hydantoin derivatives are in a weak acid environment, hydrolysis of the hydantoin derivatives is promoted by combining specific heating temperature, and meanwhile, generation of impurities is reduced. Inorganic salt is not generated in the whole preparation process, and subsequent desalting operation is not needed; a large amount of waste liquid is not generated, and the prepared glufosinate-ammonium is high in yield and good in purity; in addition, the whole glufosinate-ammonium preparation process is simple and convenient, low in cost and easy to industrialize.

Description

technical field [0001] The invention relates to the field of pesticides, in particular to a preparation method of glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is an organic phosphine herbicide, which has the advantages of good safety, long-lasting effect and wide herbicidal spectrum. Widely used in orchards, vineyards, non-cultivated land, potato fields and other environments to control annual and perennial dicotyledonous and gramineous weeds, perennial grassy weeds and sedges, with good results. [0003] At present, the relatively mature industrialized process for preparing glufosinate-ammonium is the Strecker reaction method: diethyl methylphosphite is reacted with acrolein, and then the aminonitrile compound is obtained through the Strecker reaction, and the aminonitrile compound is hydrolyzed with hydrochloric acid to obtain glufosinate-ammonium. Its process route is as follows: [0004] [0005] The above process of glufosinate-ammonium ...

Claims

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Application Information

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IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 史秀肖范立攀贾成国
Owner HEBEI VEYONG BIO CHEM
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