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
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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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