Process for purifying 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 purity

Active Publication Date: 2013-09-11
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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  • Process for purifying glufosinate-ammonium
  • Process for purifying glufosinate-ammonium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0021] Add glufosinate-ammonium hydrochloride (I) to alcohol R according to the feeding ratio in Table 1. 1 OH, carry out the 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 is decompressed to remove the solvent to obtain the esterified product (II) of glufosinate-ammonium hydrochloride, and the evaporated alcohol solvent can be recycled and reused;

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

[0023]

[0024] According to the ratio and reaction conditions in Table 2, the esterified product of glufosinate-ammonium hydrochloride prepared in Examples 1-4 (II 1 )-(II 4 ) Were added to the hydrochloric acid aqueous solution to carry out the hydrolysis reaction. After the reaction was completed, the acid water was removed, 350g of ethanol was added and stirred at 50°C for 3 hours to gradually dis...

Embodiment 5-8

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

[0029] table 3

[0030]

[0031]

Embodiment 9-12

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

[0034] Table 4

[0035]

[0036] Among them, the final structure detection data of glufosinate-ammonium 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 a chemical purification method, and specifically relates to a purification process of high-purity glufosinate-ammonium. Background technique [0002] Glufosinate-ammonia (generally referred to as glufosinate-ammonia) is a herbicide developed by Hoechst AG in 1978. Many patents have been published for its invention. Representatives of U.S. patents include: U.S. 4168983 (1979), U.S. 4,264,532 (1981), U.S. 4,490,027 (1985), U.S. 4599207 (1986), U.S. 6539162B1 (2002), etc. In the above-mentioned patent documents, there is no publication on the separation of glufosinate-ammonium and the generated NH 4 Cl (or other inorganic salts such as NaCl, etc.) methods are reported, and in most synthetic methods, NH is generated during the synthesis of glufosinate-ammonium 4 By-products such as Cl or NaCl, such as: [0003] [0004] It can be seen from the formula that both in the process of preparing glufosinate-ammonium hydrochloride, or in the pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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