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A kind of purification process of glufosinate-ammonium

A technology for glufosinate-ammonium and glufosinate-ammonium hydrochloride, which is applied in the fields of compounds of Group 5/15 elements of the periodic table, organic chemistry, chemical instruments and methods, etc., can solve the problem that it is difficult to prepare and separate high-purity glufosinate phosphine and other problems, to achieve the effect of low inorganic salt content, simple process steps and high industrialization prospects

Active Publication Date: 2011-12-07
YONGNONG BIOSCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] According to the simple recrystallization method of ethanol or methanol reported in the above-mentioned patent literature, it is difficult to achieve the purpose of preparing and separating high-purity glufosinate-ammonium

Method used

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  • A kind of purification process of glufosinate-ammonium
  • A kind of purification process of glufosinate-ammonium
  • A kind of purification process of glufosinate-ammonium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0021] According to the feed ratio of Table 1, glufosinate-ammonium hydrochloride (I) is added to alcohol R 1 OH, carry out esterification reaction, after the reaction is complete, cool to below 15°C, filter to remove insoluble matter in the system (the white solid is NH 4 Cl and a small amount of sodium chloride), the filtrate decompresses and removes the solvent to obtain the esterification product (II) of glufosinate-ammonium hydrochloride, and the alcohol solvent that evaporates can be recycled and used mechanically;

[0022] Table 1 Feed ratio and reaction conditions of esterification reaction

[0023]

[0024] According to the proportioning and reaction conditions of table 2, the esterification product (II) of the glufosinate-ammonium hydrochloride prepared by embodiment 1-4 1 )-(II 4 ) were added to hydrochloric acid aqueous solution to carry out hydrolysis reaction. After the reaction was complete, the acid water was removed, and 350g of ethanol was added and stir...

Embodiment 5-8

[0028] According to the feed ratio of Table 3, the glufosinate-ammonium hydrochloride (III) finally obtained in Examples 1 to 4 is added to alcohol R 2 OH, then pass through ethylene oxide, after the reaction is complete, cool to 0-5°C and filter to obtain the wet product white crystalline glufosinate-ammonium acid, and dry to obtain glufosinate-ammonium acid (IV);

[0029] table 3

[0030]

[0031]

Embodiment 9-12

[0033] According to the feed ratio of Table 4, the glufosinate-ammonium acid (IV) obtained in Examples 5-8 is added to R 3 In OH, feed ammonia gas at 30-40°C, the reaction is complete, cool to 0°C and filter to obtain a wet product, and dry to obtain glufosinate-ammonium;

[0034] Table 4

[0035]

[0036] Among them, the final structure detection data of glufosinate-ammonium obtained is:

[0037] 1 H-NMR (400MHz, D 2 O, TMS): δ=3.785 (1H, t), 2.065 (2H, t), 1.542-1.727 (2H, m), 1.253 (3H, d);

[0038] 13 C-NMR (400MHz, D 2 O, TMS): δ=176.51(s), 57.57(d), 29.41(d), 26.56(s), 17.32(d);

[0039] 31 P-NMR (400MHz, D 2 O, TMS): δ = 43.846 (s).

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Abstract

The invention discloses a process for purifying glufosinate-ammonium, which comprises: (1) adding glufosinate-ammonium hydrochloride into an alcohol R1OH to perform an esterification reaction, and after the reaction is accomplished, cooling, filtering, removing solvent from filtrate and obtaining ester product of glufosinate-ammonium; (2) adding the ester product of glufosinate-ammonium, which isobtained by step (1), into water solution of hydrochloric acid to perform a hydrolysis reaction, and obtaining glufosinate-ammonium hydrochloride by post treatment; (3) adding the glufosinate-ammonium hydrochloride obtained by the step (2) into an alcohol R2OH, introducing epoxy ethane and obtaining glufosinate-ammonium acid; and (4) adding the glufosinate-ammonium acid obtained by the step (3) into an alcohol R3OH, introducing ammonia gas, and obtaining glufosinate-ammonium after the reaction is finished. In the invention, the process for purifying glufosinate-ammonium comprises simple steps, the inorganic salt content in the obtained glufosinate-ammonium is low, and the purity of the obtained glufosinate-ammonium is high; the process for separating glufosinate-ammonium hydrochloride from HCl by epoxy ethane is more economic than the conventional process which adopts epoxypropane and epoxy chloropropane; and the method is very safe and has a very bright industrialization prospect.

Description

technical field [0001] The invention belongs to chemical purification methods, in particular to a high-purity glufosinate-ammonium purification process. Background technique [0002] Glufosinate-ammonium (generally referred to as glufosinate-ammonium) is a herbicide developed by the former German company Hoechst.AG in 1978. Its invention has multiple patent publications. U.S. patents are represented by: U.S.4168983 (1979), U.S.4264532 (1981), U.S.4499027 (1985), U.S.4599207 (1986), U.S.6539162B1 (2002), etc. In the above-mentioned patent documents, none of the separation of glufosinate-ammonium and the generated NH 4 Cl (or other inorganic salts such as NaCl etc.) method report, and in most synthetic methods, all generate NH when synthesizing glufosinate-ammonium 4 By-products such as Cl or NaCl, such as: [0003] [0004] It can be seen from the formula that no matter in the process of preparing glufosinate-ammonium hydrochloride or in the process of preparing glufos...

Claims

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Application Information

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IPC IPC(8): C07F9/30
Inventor 诸锡云滕忠华汪正宏张旭华孙青吴克孟
Owner YONGNONG BIOSCI
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