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A method for separating l-glufosinate-ammonium and gluconic acid with ion-exchange resin

A technology of ion exchange resin and gluconic acid, which is applied in the field of separation of L-glufosinate-ammonium and gluconic acid by ion-exchange resin, can solve the problems such as the separation method of L-glufosinate-ammonium and gluconic acid that have not been reported, and achieve significant industrial application prospects, The effect of high yield and efficient separation

Active Publication Date: 2021-03-05
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In summary, in the existing separation and purification methods about L-glufosinate-ammonium, no matter whether it is to separate and purify the L-glufosinate-ammonium reaction liquid produced by chemical method or biological method, there is no report about L-glufosinate-ammonium Separation method from gluconic acid

Method used

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  • A method for separating l-glufosinate-ammonium and gluconic acid with ion-exchange resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Regulate the pH of the thick solution containing L-glufosinate-ammonium and gluconic acid to 1.5, wherein the concentration of L-glufosinate-ammonium is 63.4g / L, and the concentration of gluconic acid is 68.6g / L. Get 10.0g of pretreated JK006 resin , fill in a 15×300mm exchange column with a height-to-diameter ratio of 4.7:1. At 25°C, pump the crude liquid into the exchange column at a flow rate of 1.0BV / h for chromatographic separation, and collect the effluent containing gluconic acid; After L-glufosinate-ammonium leaks through the end of the ion exchange column, wash the resin with 5BV of deionized water, and desorb L- with 3BV of lye with an ammonia content of 3.2 to 3.5% at a flow rate of 1BV / h after the washing process. Glufosinate-ammonium yields an eluate containing L-glufosinate-ammonium.

[0031] A total of 16.1ml of thick liquid containing L-glufosinate-ammonium and gluconic acid was pumped into the above-mentioned steps, and the concentrations of L-glufosina...

Embodiment 2

[0033] Regulate the pH of the thick solution containing L-glufosinate-ammonium and gluconic acid to 2.3, wherein the concentration of L-glufosinate-ammonium is 63.4g / L, and the concentration of gluconic acid is 68.6g / L. Get 10.0g of pretreated JK006 resin , fill in a 15×300mm exchange column with a height-to-diameter ratio of 4.7:1; at 25°C, pump the crude liquid into the exchange column at a flow rate of 1.0BV / h for chromatographic separation, and collect the effluent containing gluconic acid; After L-glufosinate-ammonium leaks through the end of the ion-exchange column, wash the resin with 5BV of deionized water, and use 3BV of lye with an ammonia content of 3.2-3.5% to desorb L-glufosinate at 1BV / h after the washing process Phosphate yields an eluate containing L-glufosinate-ammonium.

[0034] A total of 21.6ml of thick liquid containing L-glufosinate-ammonium and gluconic acid was pumped into the above steps, and the concentrations of L-glufosinate-ammonium and gluconic ac...

Embodiment 3

[0036] Regulate the pH of the crude solution containing L-glufosinate-ammonium and gluconic acid to 2.3, wherein the concentration of L-glufosinate-ammonium is 63.4g / L, and the concentration of gluconic acid is 68.6g / L. Take 10.0g of pretreated HZ001 Resin, filled in a 15×300mm exchange column with a height-to-diameter ratio of 4.5:1. At 25°C, pump the crude liquid into the exchange column at a flow rate of 1.0BV / h for chromatographic separation, and collect the effluent containing gluconic acid; After L-glufosinate-ammonium leaked from the end of the ion exchange column, wash the resin with 5BV of deionized water, and after the washing process, use 3BV of lye with an ammonia content of 3.2 to 3.5% to desorb L-glufosinate-ammonium to obtain a - the eluate of glufosinate-ammonium.

[0037] A total of 26.3ml of thick liquid containing L-glufosinate-ammonium and gluconic acid was pumped into the above steps, and the concentrations of L-glufosinate-ammonium and gluconic acid in th...

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Abstract

The invention discloses a method for separating L-glufosinate-ammonium and gluconic acid with an ion exchange resin. The method comprises: taking L-glufosinate-ammonium crude liquid containing L-glufosinate-ammonium and gluconic acid, and adjusting the pH of the crude liquid Value to 1~4, obtain feed liquid; Feed liquid is joined in the exchange column that strong acid type cation exchange resin is housed, carry out chromatographic separation, collect the effluent containing gluconic acid; Detect L-grass at the bottom of exchange column When the concentration of ammonium phosphine reaches 5% to 10% of the concentration of L-glufosinate-ammonium in the feed solution, stop adding the feed solution; then, first wash the resin with deionized water, and then use lye as an eluent to desorb L-glufosinate Ammonium phosphine, collect eluent, obtain L-glufosinate-ammonium solution. The invention firstly adjusts the pH value of the L-glufosinate-ammonium crude liquid, and then utilizes a strong acid type cation exchange resin to carry out chromatographic separation, thereby realizing efficient separation of L-glufosinate-ammonium and gluconic acid with high separation efficiency.

Description

technical field [0001] The invention relates to the technical field of L-glufosinate-ammonium production, in particular to a method for separating L-glufosinate-ammonium and gluconic acid with an ion exchange resin. Background technique [0002] Glufosinate refers to the compound 2-amino-4-[hydroxy(methyl)phosphono]-butyric acid. Glufosinate-ammonium is a broad-spectrum contact herbicide developed by Hoechst in the 1980s (later owned by Bayer). It belongs to the phosphonic acid herbicide, and its target is glutamine synthetase, which has activity High, good absorption, wide herbicidal spectrum, low toxicity, good environmental compatibility and other characteristics. [0003] [0004] Glufosinate-ammonium has two optical isomers, namely L-glufosinate-ammonium and D-glufosinate-ammonium. But only the L-form has phytotoxicity, and its herbicidal activity is twice that of the racemic mixture. Therefore, the development of L-glufosinate-ammonium preparation technology has ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30C07C51/47C07C59/105
CPCC07C51/47C07F9/301C07C59/105
Inventor 杨立荣刘亚运尹新坚周海胜张红玉吴坚平
Owner ZHEJIANG UNIV