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A purification method and glufosinate-ammonium technology are applied in the purification field of chemicals, which can solve the problems of high cost, large solvent and energy consumption, long process route and the like, and achieve the effects of simple steps, high safety and high purity
Active Publication Date: 2016-05-04
JIANGSU SEVENCONTINENT GREEN CHEM CO LTD
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The purification method has a long process route, large co
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[0044] An embodiment, as attached figure 1 Shown:
[0045] Step (1), heating the acid-hydrolyzed glufosinate-ammonium hydrochloride reaction solution to remove low-boiling point organic solvents and a part of water, and filtering to remove part of ammonium chloride and other insoluble impurities;
[0046] Step (2), add alkali to the filtrate obtained in step (1), adjust the pH to 5~14 for reaction, then heat and distill part of the water, filter to remove ammonium chloride and other insoluble impurities, then add acid, adjust the pH to 1 to 5 are reacted, and then filtered, washed, and dried to obtain the glufosinate-ammonium acid; the filtrate obtained in step (2) is combined with the glufosinate-ammonium hydrochloride reaction solution in step (1);
[0047] Step (3), dissolving the glufosinate-ammonium acid obtained in step (2) in a solvent, and then introducing ammonia gas to carry out a salt-forming reaction, to precipitate glufosinate-ammonium solids, and then filter, wa...
Embodiment 1
[0058] The reaction solution of glufosinate-ammonium hydrochloride (1000 grams, including 300 grams of glufosinate-ammonium hydrochloride) obtained by acid hydrolysis was heated to 110°C, low-boiling point organic matter and part of water (100g) were distilled off, cooled to 30°C, and dripped Add a mixed solution of 5 grams of glycine and 30 grams of ammonia water, adjust the pH=1, react for 1 hour, crystallize, filter, wash with methanol, and dry to obtain 30 grams of off-white glufosinate-ammonium acid with a yield of 12% and a purity of 95%. The filtrates were combined for the next step.
Embodiment 2
[0062] Add a certain amount of ammonia water dropwise to the filtrate (865 g) obtained in Example 1, adjust pH = 10, heat to 110°C, distill off part of the water (350g), cool to 30°C, filter to remove insoluble ammonium chloride, etc. Add a certain amount of hydrochloric acid dropwise to the remaining filtrate, adjust the pH=1, crystallize, filter, wash with methanol, and dry to obtain 215 grams of off-white glufosinate-ammonium acid, with a yield of 97% and a purity of 95%.
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Abstract
The invention relates to a purification method for glufosinate-ammonium. The method comprises the following steps that an acidolysis glufosinate-ammonium hydrochloride reaction solution is heated and distilled to remove low-boiling-point organic solvent and some water, and filtering is performed to remove some ammonium chloride and other insoluble impurities; the pH value of the filtrate is adjusted to be 1-5, and then filtering, washing and drying are performed to obtain glufosinate-ammonium acid; the glufosinate-ammonium acid is dissolved into the solvent, then, ammonia gas is introduced to be subjected to a salt forming reaction, glufosinate-ammonium solid is separated out, and then filtering, washing and drying are performed to obtain high-purity glufosinate-ammonium; the filtrate and glufosinate-ammonium hydrochloride reaction solution are combined. According to the purification technology, fatty amine hard to remove and high-risk ethylene oxide and epoxypropane are prevented from being used, the steps are simple, the obtained glufosinate-ammonium is low in inorganic salt content and high in purity, yield and safety, water or alcohol is used as the solvent in the technological process, ammonium hydroxide and inorganic base are used for being subjected to a neutral reaction, the glufosinate-ammonium conforms to the environment-friendly and economical principle, and the good industrial prospect is achieved.
Description
technical field [0001] The invention belongs to a purification method of chemicals, in particular to a purification method of glufosinate-ammonium. Background technique [0002] Glufosinate-ammonium is a contact-killing herbicide with the characteristics of high efficiency, low toxicity, low residue and safety. Its quick-acting property is between that of paraquat and glyphosate. It is widely used in agricultural production. The structural formula of glufosinate-ammonium is as follows : [0003] . [0004] The crude product of glufosinate-ammonium hydrochloride contains a large amount of inorganic salt by-products such as ammonium chloride and produces viscous organic impurities. There are also relevant reports on the purification process of glufosinate-ammonium hydrochloride in China. For example, patent CN103819503 mentions that glufosinate-ammonium Phosphine hydrochloride is ammonified into salt, and then mixed with carbon dioxide to obtain glufosinate-ammonium acid...
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