Glufosinate-ammonium separating and purifying method

A technology for separation and purification of glufosinate-ammonium, applied in the field of separation and purification of glufosinate-ammonium, can solve the problems of violating the basic chemical principle of strong base to weak base, difficult process, low recovery rate, etc., and achieve novel process route and simplified purification Craft, Recycle Simple Effects

Active Publication Date: 2016-02-10
SHANDONG WEIFANG RAINBOW CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses the alcohol R 1 When OH is hot filtered to remove inorganic salts and mechanical impurities, the alcohol R 1 OH will partially esterify with glufosinate-ammonium hydrochloride resulting in low recovery
The patent uses a base weaker than the organic base R 2 R 3 R 4 The ammonia gas of N converts the R in glufosinate-ammonium free base 2 R 3 R 4 The replacement of N violates the basic chemical principle of strong base to weak base, so the process is difficult and difficult to realize

Method used

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  • Glufosinate-ammonium separating and purifying method
  • Glufosinate-ammonium separating and purifying method
  • Glufosinate-ammonium separating and purifying method

Examples

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Effect test

Embodiment 1

[0048] Weigh 500g of glufosinate-ammonium acid hydrolysis solution (equivalent to 13.98% glufosinate-ammonium content) into a 1000ml four-neck flask, add 182.8g of 18% ammonia water to it dropwise to pH=6.07, and obtain 682.7g of ammonium solution, and ammonium The solution was spray-dried to obtain glufosinate-ammonium crude product A185.3g (moisture content 0.7%). Transfer the crude product A of glufosinate-ammonium into a 500ml four-necked bottle, add 185.3g of n-butanol, then raise the temperature to 100°C under stirring, keep it warm for 1 hour, and filter it while it is hot, and dry the filtered cake to obtain crude product B165.1g of glufosinate-ammonium . Transfer crude product B of glufosinate-ammonium into a 1000ml four-necked bottle, add 330.2g of trimethyl phosphate and then heat up to 80°C under stirring, keep warm for 1h and filter at this temperature and wash the filter cake with 165.1g of trimethyl phosphate to obtain Glufosinate-ammonium crude product C (ie f...

Embodiment 2

[0050] Weigh 500g of glufosinate-ammonium acid hydrolysis solution (equivalent to 13.98% glufosinate-ammonium content) into a 1000ml four-neck flask, add 205.4g of 18% ammonia water to it dropwise to pH = 8.13, and obtain 705.4g of ammonium solution, and ammonium The solution was spray-dried to obtain glufosinate-ammonium crude product A185.2g (moisture content 0.6%). Transfer the crude product A of glufosinate-ammonium into a 3000ml four-necked bottle, add 1852g of propanol, then raise the temperature to 40°C under stirring, keep it warm for 1 hour, then filter it while it is hot, and dry the filtered cake to obtain crude product B164.7g of glufosinate-ammonium. Transfer crude product B of glufosinate-ammonium into a 2000ml four-necked bottle, add 1154.3g tributyl phosphate and then heat up to 50°C under stirring, filter at this temperature after insulated for 1h and wash the filter cake with 164.7g tributyl phosphate to obtain Glufosinate-ammonium crude product C (i.e. filtr...

Embodiment 3

[0052] Weigh 500g of glufosinate-ammonium acid hydrolysis solution (equivalent to 13.98% glufosinate-ammonium content) into a 1000ml four-neck flask, add 193.8g of 18% ammonia water to it dropwise to pH = 7.01, and obtain 693.8g of ammonium solution. The solution was spray-dried to obtain glufosinate-ammonium crude product A185.4g (moisture content 0.3%). Transfer the crude product A of glufosinate-ammonium into a 2000ml four-neck bottle, add 741.6g of isopropanol, then raise the temperature to 60°C under stirring, keep it warm for 1 hour, then filter it while it is hot, and dry the filtered cake to obtain crude product B164.9g of glufosinate-ammonium . Transfer crude product B of glufosinate-ammonium into a 500ml four-necked bottle, add 164.9g of trioctyl phosphate and then heat up to 100°C under stirring, keep it warm for 1h, filter at this temperature and wash the filter cake with 164.9g of trioctyl phosphate to obtain Glufosinate-ammonium crude product C (ie filtrate and ...

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Abstract

The invention discloses a glufosinate-ammonium separating and purifying method. The method includes the steps of conducting ammoniation on a glufosinate-ammonium acidolysis solution or solid glufosinate-ammonium hydrochloride, conducting drying to obtain a glufosinate-ammonium crude product A, adding the glufosinate-ammonium crude product A to alcohol, conducting filtering to obtain a glufosinate-ammonium crude product B, adding the glufosinate-ammonium crude product B to phosphate ester, conducting filtering to obtain filtrate, washing a filter cake through phosphate ester, combining filtrate with washing liquid to obtain a glufosinate-ammonium crude product C, adding the glufosinate-ammonium crude product C to water to be extracted, and taking a water layer which can be directly used as a glufosinate-ammonium aqueous solution or obtaining high-purity glufosinate-ammonium active compounds after the water layer is spray-dried. The method is simple in step, the content of chloride impurities in the obtained glufosinate-ammonium aqueous solution or glufosinate-ammonium active compounds is extremely low, basically no organic impurities exist, the purity of the separated glufosinate-ammonium active compounds can reach 98% or higher, and the recovery rate of glufosinate-ammonium reaches up to 98% or higher. Compared with the traditional process, the method has the higher advantages of cost, safety, environmental friendliness and quality and has extremely-high social value and economic value.

Description

technical field [0001] The invention relates to a separation and purification method of glufosinate-ammonium. technical background [0002] Glufosinate-ammonium is also known as glufosinate-ammonium. We usually refer to glufosinate-ammonium ammonium salt. The chemical formula of glufosinate ammonium salt is: C 5 h 15 N 2 o 4 P, the structural formula is: . Glufosinate-ammonium was first developed in 1978 by Hoechst AG of Germany (now owned by Bayer AG of Germany). Since the development of glufosinate-ammonium, research related to glufosinate-ammonium has never stopped in the world. At present, there are many research patents related to the preparation of glufosinate-ammonium disclosed at home and abroad, such as US6359162B1, EP0009022A1, CN102399239A, CN102372738A, CN101747367A, CN103374030A, CN103588812A, etc., among which the most representative ones are US6359162B1 and EP0009022A. At present, the main synthesis techniques of glufosinate-ammonium are: Stryker-Zelin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 孙国庆侯永生张利国迟志龙
Owner SHANDONG WEIFANG RAINBOW CHEM
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