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A kind of preparation method of glufosinate-ammonium

A glufosinate-ammonium compound technology, applied in the field of glufosinate-ammonium preparation, can solve the problems of cumbersome purification process, difficult product separation, and three wastes, and achieve high yield and content, meet environmental protection requirements, and simple steps

Active Publication Date: 2018-08-17
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The requirements for safe production are high, and a large amount of mixed salt of ammonium chloride and sodium chloride is produced in the reaction process, which is difficult to separate from the product, and the purification process is cumbersome
CN103965241 utilizes methyl phosphonate and benzylidene glycine ester to synthesize glufosinate-ammonium through addition reaction, and the recovery of diphenyl ketone produced by this process is difficult, and there are many wastes

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 6.25 g of vinyl chloride (0.1 mol) was dissolved in 10 mL of toluene, and then 0.9 g of tert-butanol peroxide (0.01 mol) was added. This mixture was added dropwise to 32.4 g of ethyl methyl hypophosphite (0.3 mol), the reaction temperature was controlled at 50° C., and the dropwise addition was completed in 30 minutes. After the dropwise addition, it was stirred at 25° C. for 15 minutes. The solvent and excess ethyl methyl hypophosphite were distilled off under reduced pressure to obtain the crude compound 3. After rectification, 15.2 g of compound 3 were obtained, with a yield of 82.3% and a purity of 92.3%.

Embodiment 2

[0034] Dissolve 18.5 g of compound 3 (0.1 mol) and 11.3 g of ethyl isocyanoacetate (0.1 mol) in 15 mL of DMF, add 16.56 g of potassium carbonate (0.12 mol), heat to 80°C, and stir for 30 minutes. Add 100mL of ethyl acetate, wash with saturated sodium bicarbonate, saturated brine and water successively, dry over anhydrous sodium sulfate, filter, distill under reduced pressure, and purify by column chromatography to obtain 20.2 g of light yellow liquid compound 6 with a yield of 78.3 %, purity 95.6%.

Embodiment 3

[0036] Add 12.9 grams of compound 6 (0.05 mol) dropwise into 15 mL of 15% dilute hydrochloric acid, the dropping temperature is controlled below 10°C, after the dropwise addition, heat to reflux for 2 hours, dropwise add ammonia water to neutralize, filter and separate Ammonium chloride was removed and recrystallized with methanol to obtain 8.5 g of glufosinate-ammonium ammonium salt with a yield of 91.2% and a purity of 97.1%.

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PUM

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Abstract

The invention relates to a glufosinate ammonium preparation method which includes the steps: (1) taking a compound 3 as a raw material, and performing reaction for the compound 3 and a compound 5 at the temperature ranging from 10 DEG C to 80 DEG C under the actions of alkali; (2) reacting a compound 6 at the temperature ranging from 50 DEG C to 120 DEG C under the actions of acid to obtain a compound 7. The structural formula of the compound 3 is as shown in the specification, the structural formula of the compound 5 is as shown in the specification, the structural formula of the compound 6 is as shown in the specification, the structural formula of the compound 7 is as shown in the specification, wherein R1 is alkyl, the carbon number of the alkyl is 1-5, R2 is alkyl, and the carbon number of the alkyl is 1-3. The preparation method is simple in step, low in cost and suitable for industrial production, cannot generate high-salinity wastewater and more meets environment-friendly requirements, and both the yield and the content of final products are high.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and relates to a preparation method of glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is a contact herbicide with high efficiency, low toxicity, low residue and safety. Its quick-acting property is between paraquat and glyphosate, and it is widely used in agricultural production. [0003] There are many synthetic methods of glufosinate-ammonium, mainly applied by Bayer Company, and its invention has been published in many patents. For example, U.S. Patent Nos. 6,359,162, 4,521,348 and 4,264,532, etc. These patented methods all use dangerous chemicals such as acrolein and sodium cyanide as raw materials, and use the Strecker method to synthesize glufosinate-ammonium. The requirements for safe production are high, and a large amount of mixed salt of ammonium chloride and sodium chloride is produced in the reaction process, which is difficult to separate ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 姜宇华陈佳何永利蔡军义安静
Owner JIANGSU SEVENCONTINENT GREEN CHEM CO LTD