Method for preparing high-purity glufosinate-ammonium by adopting organic alkali deacidification method
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A technology for organic base and glufosinate-ammonium, which is applied in the field of preparing high-purity glufosinate-ammonium by deacidification of organic bases, can solve the problems of increasing production cost and three-waste treatment cost, unable to recover and dissolve in high yield, difficult to recover, etc. Efficient and simple recycling, easy operation, less by-products
Inactive Publication Date: 2014-09-24
ZHEJIANG UNIV OF TECH +2
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Although these methods greatly reduce the ash in the subsequent glufosinate-ammonium preparation because they do not produce a large amount of inorganic salts and ammonium chloride, and have good industrial application value, they also generate 2-chloroethanol, 3-chloropropanol, etc. Chlorine-containing high-boiling by-products that are not easy to recover, and additionally increase production costs and waste treatment costs, and the mother liquor containing chloroethanol and chloropropanol cannot recover the glufosinate-ammonium dissolved in it at a high yield, resulting in losses
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Embodiment 1-5
[0030] according to Table 1 Reaction conditions and process parameters shown, adding glufosinate-ammonium hydrochloride to alcohol R 1 OH, reflux to dissolve, filter to remove inorganic salts and mechanical impurities, concentrate and recover 50% of the total volume of R 1 OH solvent, the evaporated solvent can be used directly. Then add the organic base R 2 R 3 R 4 N neutralize 7 The hydrochloric acid in the solution is nearly neutral, cooled to 0-5°C, the glufosinate-ammonium free base is precipitated, and the free base is obtained by filtration, which can be directly used in the next step of ammonia reaction without purification. Purity was measured by liquid phase normalization method.
[0032] Table 1 Neutralization reaction conditions of glufosinate-...
Embodiment 6-10
[0036] according to Table 2 The reaction conditions, the free base that embodiment 1-5 gained is added to corresponding alcoholic solvent R respectively 1 OH, and then pass ammonia gas at a certain temperature. After the reaction is complete, cool to 0-5°C, filter, and dry under reduced pressure to obtain glufosinate-ammonium. Purity was measured by liquid phase normalization method. The structure of glufosinate-ammonium 1 Confirmed by H-NMR and ESI-MS, it is consistent with the literature value. 1 H-NMR (400MHz, D 2 O, TMS): δ, 3.80 (1H, t), 2.11 (2H, t), 1,56-1.75 (2H, m), 1.28 (3H,d), ESIMS: 182[M+1], 198[ M+NH 3 ].
[0037] Table 2 Amination reaction conditions and results
[0038]
[0039] As can be seen from the above table, the reaction received more than 78%, the total reaction yield reached more than 64%, and the purity reached 97%.
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Abstract
The invention discloses a method for preparing high-purity glufosinate-ammonium by adopting an organic alkali deacidification method, belonging to the technical field of preparation of the glufosinate-ammonium. The method comprises the following steps: by taking glufosinate-ammonium hydrochloride as a raw material, dissolving the glufosinate-ammonium hydrochloride into alcohol R1OH, and thermally filtering out inorganic salt and mechanical impurities; partially concentrating the filtrate, adding organic alkali R2R3R4N for a deacidification reaction, cooling and filtering out glufosinate-ammonium free alkali; adding a crude glufosinate-ammonium free alkali product into the alcohol R1OH, introducing ammonia gas, cooling and filtering to obtain a glufosinate-ammonium product; and recycling an alcohol solvent from crystallization mother liquor of the free alkali, subsequently adding into an inorganic alkaline water solution for neutralization, separating out the organic alkali in the upper layer and directly using the organic alkali in the deacidification reaction. The method disclosed by the invention can be used for effectively removing a small amount of inorganic matters including ammonium chloride, sodium chloride, the mechanical impurities, hydrogen chloride and the like from the glufosinate-ammonium hydrochloride, also can be used for simply and conveniently preparing a high-purity glufosinate-ammonium product without introducing new impurities and organic byproducts and has good industrial application prospects.
Description
technical field [0001] The invention belongs to the technical field of glufosinate-ammonium preparation, and in particular relates to a method for preparing high-purity glufosinate-ammonium by an organic alkali deacidification method. Background technique [0002] Glufosinate-ammonium (glufosinate-ammonium) is an organophosphorus herbicide developed in the 1970s by the German company Hoechst. Glufosinate-ammonium is the second most herbicide-tolerant genetically modified crop in the world. It has low toxicity, is safe for crops, has a wide herbicidal spectrum, high activity, less dosage, and can quickly kill more than 100 species of grasses and broadleaves. For weeds, water can be used as a base agent, which is safe and convenient to use. The above characteristics make it popular in domestic and foreign markets. [0003] Most of the synthetic methods of glufosinate-ammonium use phosphorus trichloride or phosphonite as the starting material, through a certain reaction proces...
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