A method for the purification of glufosinate-ammonium
A technology of glufosinate-ammonium and glufosinate-ammonium hydrochloride is applied in chemical instruments and methods, organic chemistry, compounds of Group 5/15 elements of the periodic table, etc., and can solve problems such as being expensive and difficult to meet industrialized production applications, etc. To achieve the effect of simple operation, satisfying industrialized large-scale production, and good application prospects
Active Publication Date: 2019-04-09
GUANGAN LIER CHEM CO LTD
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Problems solved by technology
[0007] The purpose of the present invention is to provide a glufosinate-ammonium purification method for the problem that the existing glufosinate-ammonium purification method needs to use highly toxic and explosive ethylene oxide, or needs to use expensive organic amines, which is difficult to meet the industrial production application. Methods
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Embodiment 1
[0035] The separation and purification process is as follows.
[0036] Using phosphonite and phosphorus trichloride as raw materials, after cyanidation reaction, the intermediate cyanamide solution of glufosinate-ammonium is obtained; then hydrochloric acid is added to it for hydrolysis to obtain glufosinate-ammonium hydrochloride aqueous solution, and then evaporated and concentrated Until the water content of the material is below 10%, the concentrated mother liquor is obtained. The concentrated mother liquor is subjected to an esterification reaction with methanol or ethanol under acid catalysis (see Table 1 for screening of reaction conditions). After controlling the esterification rate to be higher than 95% in reflux, the temperature is lowered to 10° C., and the solid inorganic salt is removed by filtration to obtain filtrate. After recovering the alcohol from the filtrate, add hydrochloric acid to stir and reflux, the esterification product in the middle control is les...
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The invention discloses a glufosinate-ammonium purifying method and aims to solve the problem that existing glufosinate-ammonium purifying methods need to adopt high-toxicity explosive ethylene oxide, or need to adopt expensive organic amine and are hard to satisfy industrial production application. In allusion to the problem of separating glufosinate-ammonium and inorganic salt, the invention provides a safe and simple method suitable for industrial production. The invention has the following beneficial effects: reagents used in the invention are cheap and easily available; purification cost is low; production period is short; and the method can meet requirements of industrial large-scale production. In addition, recycling of mother liquor also can be realized, solid waste discharge is effectively reduced, and purification yield is raised. The method of the invention has a good application prospect.
Description
technical field [0001] The invention relates to the field of chemical engineering, especially the field of purification, and specifically relates to a method for purifying glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium, also known as glufosinate-ammonium phosphate, is an excellent herbicide with high efficiency, low toxicity and non-selectivity. In recent years, with the expansion of the planting area of genetically modified crops and the development of resistant weeds, the market demand for glufosinate has been increasing. [0003] At present, glufosinate-ammonium is mainly produced by the following method: using methyl phosphite diester as raw material, reacting rearrangement with acrolein, then undergoing Strecker reaction to obtain cyanamide derivatives, and finally undergoing hydrolysis to obtain glufosinate-ammonium. This method can produce a large amount of inorganic salts (sodium chloride and ammonium chloride) in the hydrolysis process; ...
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IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 吴锋程柯
Owner GUANGAN LIER CHEM CO LTD