Method for separating and purifying glufosinate-ammonium

A purification method, glufosinate-ammonium technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as complex operation, low concentration, and large consumption of organic solvents, and achieve The effect of high product concentration, high separation and high selectivity

Active Publication Date: 2014-01-01
XIAMEN STARMEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the chemical synthesis method, a large amount of inorganic salts and organic impurities will be produced along with the synthesis process of glufosinate-ammonium, which is difficult to separate by ordinary methods. Generally, the difference in solubility of glufosinate-ammonium and inorganic salts in organic solvents is used to realize the synthesis of synthetic products. Separation, but this method consumes solvent and may cause solvent residues and bring unsafe factors to the operation; "Hebei Chemical Industry" Volume 30 No. 6 "Glufosinate (Basta) Ion Exchange Lipid Purification Technology" mentioned the use of 201× 7 Strongly basic anion exchange resin adsorbs inorganic impurities, then elutes with HCl, and crystallizes with ethanol to obtain a product with a purity of more than 99%, but the yield of this method is low, the loss of glufosinate-ammonium is large, and the production wastewater pollutes the environment; in addition , the Chinese invention patent with the publication number CN102127110A discloses "A Method for Separation and Purification of Glufosinate-ammonium Solution", which discloses a process for the separation and purification of glufosinate-ammonium by using a nanofiltration membrane and an electrodialysis membrane combination process, which can obtain glufosinate-ammonium Ammonium phosphine mass fraction 15-30%, inorganic salt mass fraction 0.05-0.5% glufosinate-ammonium solution and glufosinate-ammonium solution mass fraction 0.01-0.1%, inorganic salt mass fraction 3-7% inorganic salt solution, this method does not It needs acid and alkali, which can protect the environment well, but this method also has the following defects: when the aqueous solution of high-concentration glufosinate-ammonium and inorganic salt circulates in the membrane, its escape rate will increase greatly, and the product purity is about 95%. In the water system, the product concentration cannot be too high in the electrodialysis process, so the recovered by-product inorganic salts, product glufosinate-ammonium and its early crude product have high steam consumption when dissolving, and the industrial operability is poor
In summary, the existing glufosinate-ammonium separation and purification methods have the disadvantages of large consumption of organic solvent, high operating cost, low concentration, complicated operation, and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Using phosphorus trichloride or phosphite as raw material, in the thick liquid of glufosinate-ammonium obtained at the end of the ammoniation reaction, the mass fraction of glufosinate-ammonium is 20%, the mass fraction of sodium chloride is 8%, and the pH of the adjusted solution is 4.3; After filtering with a 20μm filter bag, according to the height-to-diameter ratio of 1:1.5, fill with sodium-type strong acid ion exchange resin, column temperature 0°C, feed volume 0.1bv, constant temperature chromatographic separation, elution with distilled water, control column temperature 0°C for washing The flow rate is 0.5bv.h, and the eluent and residual liquid are collected separately. The purity of glufosinate-ammonium in the eluent is 97.3%, the concentration is 15.2%, and the yield is greater than 98.1%; the purity of sodium chloride in the residual liquid is 98%, and the concentration is 5%. .

Embodiment 2

[0019] After diluting in the glufosinate-ammonium crude solution, the mass fraction of glufosinate-ammonium is 60%, the mass fraction of calcium chloride is 5%, and the pH of the solution is adjusted to 3; Acidic ion exchange resin, column temperature 50°C, feed amount 0.04bv, constant temperature chromatographic separation, elution with distilled water, control column temperature 0°C elution flow rate 0.05bv.h, collect eluent and residual liquid separately, elute The purity of glufosinate-ammonium in the liquid is above 98.7%, the concentration is 55%, and the yield is 99%; the purity of calcium chloride in the residual liquid is 98.3%, and the concentration is 3%.

Embodiment 3

[0021] Glufosinate-ammonium crude liquid is diluted with water, the mass fraction of glufosinate-ammonium is 60%, the mass fraction of sodium chloride is 8%, the pH of the solution is 9, the mass fraction of glufosinate-ammonium is 80%, and the mass fraction of potassium chloride is 3%. The pH is 4.3; after filtering through a 100μm filter bag, the ratio of height to diameter is 1:20, filled with potassium-type strong acid ion exchange resin, the column temperature is 0-100°C, the feed amount is 2bv, separated by variable temperature chromatography, and eluted with distilled water. Control the column temperature at 0-100°C and the elution flow rate is 5bv.h, collect the eluent and residual liquid separately, the purity of glufosinate-ammonium in the eluent is 97.9%, the concentration reaches 75%, and the yield is 98.3%; sodium chloride in the residual liquid Potassium has a purity of 98.6% and a concentration of 2%.

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Abstract

The invention discloses a method for separating and purifying glufosinate-ammonium. The method comprises the steps: 1, diluting glufosinate-ammonium crude liquid into a solution with mass fraction of 10-80% by water; then, carrying out pretreatment on the solution by a 20-100mu m filter bag to remove mechanical impurities which are possibly caused in the glufosinate-ammonium synthesis process; and 2, adjusting the pH of the solution to be within the range of 3-9, and enabling the solution to enter a chromatographic column filled with strong acid type cation exchange resin at the temperature of 0-100 DEG C, with water as an eluting agent, and respectively collecting eluant and residual liquid, wherein the eluant is a glufosinate-ammonium solution, and the residual liquid is an inorganic salt solution. After the technical scheme is adopted, the method for separating and purifying the glufosinate-ammonium has the beneficial effects that the method is high in selectivity, degree of separation, product concentration and purity and simple in technology; the feed of the whole technology comprises raw materials and pure water, and the discharge of the whole technology comprises the glufosinate-ammonium and the inorganic salt, so that other wastes are not produced.

Description

technical field [0001] The invention relates to the field of glufosinate-ammonium production, in particular to a separation and purification method for glufosinate-ammonium. Background technique [0002] Glufosinate ammonium (Glufosinate ammonium) is developed and produced by the German company Hoechst, and its chemical formula is C 5 h 12 NO 4 P, with a formula weight of 181.127, is easily soluble in water, not easily soluble in organic solvents, stable to light, and is an inhibitor of glutamine synthesis. Glufosinate-ammonium is a highly efficient, low-toxic, non-selective (killing) contact organophosphorus herbicide with partial systemic action. Glufosinate-ammonium has the advantages of low toxicity, relatively safe, easy to degrade in soil, safe to crops, small drift, wide herbicidal spectrum, high activity, low dosage, low environmental pressure, rapid weed killing, etc., and can prevent or quickly kill More than 100 annual or perennial dicotyledonous broadleaf or ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/30
Inventor 李振峰孙洪贵卢伯福张松北彭广生虞美辉陈洪景雷细良
Owner XIAMEN STARMEM TECH
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