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A kind of preparation method of new glufosinate-ammonium

A technology of glufosinate-ammonium and methylphosphinate, which is applied in the field of pesticide chemistry, can solve the problems of large amount of waste water, increase the difficulty of separation of subsequent products, increase the difficulty of post-processing of by-products, etc., and achieve high product purity and good industrialization prospects and economy, the effect of reducing difficulty

Active Publication Date: 2022-05-24
NANJING REDSUN BIOCHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, a large amount of ammonium chloride, ammonium acetate, etc. are produced, and the amount of waste water is also large: (3-cyano-3-acetoxypropyl) methyl phosphinate reacts with ammonia water to prepare the ammoniated product process Ammonium acetate in the same amount of substances will be produced, which will be decomposed into acetic acid and ammonium chloride in the acid hydrolysis process, which increases the difficulty of separating subsequent products, and the by-products are not single salts, but ammonium chloride and ammonium chloride. The mixture of salts such as sodium chloride also increases the difficulty of post-processing of by-products

Method used

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  • A kind of preparation method of new glufosinate-ammonium
  • A kind of preparation method of new glufosinate-ammonium
  • A kind of preparation method of new glufosinate-ammonium

Examples

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Effect test

Embodiment 1

[0036] At normal temperature, 172.6g (3-aldehyde propyl) methyl phosphinate (95%) was added dropwise to a four-necked bottle containing 624.2g aqueous sodium bisulfite solution (20%), and the dropwise addition was completed within 30min. , after the dropwise addition was completed, the reaction was continued to be fully stirred for 1 h at a temperature of 28-30 °C. The temperature was raised to 50°C, 196.2g of sodium cyanide solution (30%) was added to the reaction solution, the dropwise addition was completed within 30min, the stirring was continued for 30min after the dropwise addition, and then cooled to 40°C, and 200mL of ammonia water (20%) was added. , fully reacted, concentrated to a thick slurry; add 500g of hydrochloric acid (35%), fully hydrolyzed and desolubilized by heating under reflux, adjusted the pH value to 9 with ammonia water (20%), and removed ammonium chloride by alcohol precipitation with 300g of methanol, etc. Inorganic salt, the solution was concentrate...

Embodiment 2

[0038] Under normal temperature, 260.0g (3-aldehyde propyl) methyl phosphinate (95%) was added dropwise to a four-necked bottle containing 945.1g of sodium bisulfite aqueous solution (20%), and the dropwise addition was completed within 30min. , after the dropwise addition, continue to fully stir the reaction at 28 ~ 30 ℃ for 1h. The temperature was raised to 50°C, 300.1g of sodium cyanide solution (30%) was added to the reaction solution, the addition was completed within 30min, and the stirring was continued for 30min after the dropwise addition, and then cooled to 40°C, and 300mL of ammonia water (20%) was added. , fully reacted, concentrated to a thick slurry, added 755g hydrochloric acid (35%), fully hydrolyzed and desolubilized by heating under reflux, adjusted the pH value to 9 with ammonia water (20%), and removed ammonium chloride by alcohol precipitation with 450g methanol, etc. Inorganic salt, the solution was concentrated to obtain the crude glufosinate-ammonium, a...

Embodiment 3

[0040] Under normal temperature, 86.3g (95%) of (3-aldehyde propyl) methyl phosphinate was added dropwise to a four-necked flask containing 312.2g of sodium bisulfite aqueous solution (20%), and the dropwise addition was completed within 20min. , after the dropwise addition, continue to fully stir the reaction at 28 ~ 30 ℃ for 1h. The temperature was raised to 50°C, 98.3g of sodium cyanide solution (30%) was added to the reaction solution, the dropwise addition was completed within 20min, and the stirring was continued for 30min after the dropwise addition, and then cooled to 40°C, and 100 mL of ammonia water (20%) was added. , fully reacted, concentrated to a thick slurry, added 250g hydrochloric acid (35%), fully hydrolyzed and desolvated by heating under reflux, adjusted the pH value to 9 with ammonia water (20%), and removed ammonium chloride by alcohol precipitation with 150g methanol, etc. Inorganic salt, the solution was concentrated to obtain the crude glufosinate-ammo...

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Abstract

The invention discloses a new preparation method of glufosinate-ammonium, which comprises the following steps: reacting a glufosinate-ammonium intermediate (3-aldehyde propyl) methyl phosphinate with sodium bisulfite, and then reacting with sodium cyanide to obtain ( 3-cyano-3-hydroxypropyl) methyl phosphinate, and then sequentially undergoes an ammoniation reaction, a hydrolysis reaction, and a salt-forming reaction to obtain glufosinate-ammonium. The present invention uses (3-aldehyde propyl) methyl phosphinate as a raw material, utilizes the good affinity of sodium bisulfite to aldehyde groups to realize the preparation of glufosinate-ammonium, and avoids the use of acetic anhydride in the traditional process. Simple, not only reduces the cost, but also reduces the difficulty of separating by-products, the obtained by-product salt is less than the traditional process, the purification process is simple, the product purity is high, and it has good industrialization prospects and economy.

Description

technical field [0001] The invention belongs to the field of pesticide chemistry, and in particular relates to a novel preparation method of glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is an excellent herbicide, and its structure is shown in formula III: [0003] [0004] As we all know, the traditional production method of glufosinate-ammonium is generally the Strecker route (Bayer route), and the specific route is as follows: [0005] [0006] Methylphosphine dichloride reacts with n-butanol (or isobutanol) to prepare monobutyl methylphosphite, and then reacts with 1-cyano-2-propenyl acetate under the action of a catalyst. The product (3-cyano-3-acetoxypropyl) methyl phosphinate (formula IV) is then subjected to ammoniation reaction with ammonia to obtain the amino nitrile intermediate, which is hydrolyzed with hydrochloric acid to obtain glufosinate-ammonium salt Add ammonia water to neutralize glufosinate-ammonium hydrochloride to glu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 王福军岳瑞宽薛谊陈新春蒋剑华陈洪龙
Owner NANJING REDSUN BIOCHEM CO LTD