Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of clean preparation method of glufosinate-ammonium

A technology of glufosinate-ammonium and glufosinate-ammonium sodium salt is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Serious corrosion of equipment and other problems, to achieve the effect of more appearance and color, high atomic utilization, and not easy to absorb moisture

Active Publication Date: 2020-01-14
LIER CHEM CO LTD
View PDF14 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to provide a solution for the problems of severe corrosion of equipment, large amount of three wastes, low yield of existing product purification means or high cost of complex operation in the existing method when aminonitrile acid is hydrolyzed. A kind of clean preparation method of glufosinate-ammonium

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of clean preparation method of glufosinate-ammonium
  • A kind of clean preparation method of glufosinate-ammonium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Take 230 g of aminobutyronitrile aqueous solution, add 128 g (1.6 mol) of 50% sodium hydroxide therein, raise the temperature to 85° C. and react for 2 h, during which ammonia gas is continuously released, and the ammonia gas is absorbed and recovered with water. After the reaction is complete, an aqueous solution of glufosinate-ammonium sodium salt is obtained; the aqueous solution of glufosinate-ammonium sodium salt is cooled to 0°C, and then CO 2 To supersaturation, then raise the temperature to 30°C and feed ammonia gas to make the solution pH=8-9, continue to pass ammonia gas for 1 h, then stir for 3 h, a large amount of inorganic salt sodium bicarbonate is precipitated, filter the inorganic salt, and concentrate the filtrate to obtain 50% glufosinate-ammonium solution 150g, yield 92.6%.

Embodiment 2

[0036] Take 230 g of aminobutyronitrile aqueous solution, add 128 g (1.6 mol) of 50% sodium hydroxide therein, raise the temperature to 85° C. and react for 2 h, during which ammonia gas is continuously released, and the ammonia gas is absorbed and recovered with water. After the reaction was complete, an aqueous solution of glufosinate-ammonium sodium salt was obtained; the aqueous solution of glufosinate-ammonium sodium salt was cooled to 30°C, and 164g NH 4 HCO 3, then stirred for 5h, a large amount of inorganic salts were precipitated, the inorganic salts were filtered, the filtrate was concentrated, 200g of methanol was added to freeze crystallization, a large amount of white crystals were precipitated, the white crystals were filtered, and after drying, 73.5g of glufosinate-ammonium was obtained with a purity of 98%. 90.9%.

Embodiment 3

[0038] Take 1150 g of aminobutyronitrile aqueous solution, add 640 g (8 mol) of 50% sodium hydroxide therein, raise the temperature to 85° C. and react for 2 h, during which ammonia gas is continuously released, and the ammonia gas is absorbed and recovered with water. After the reaction is complete, an aqueous solution of glufosinate-ammonium sodium salt is obtained; the aqueous solution of glufosinate-ammonium sodium salt is cooled to 0°C, and CO 2 To supersaturation, then raise the temperature to 25°C, feed ammonia gas to make the pH = 8-9, continue to pass ammonia gas for 1 h, then stir for 3 h, a large amount of inorganic salt sodium bicarbonate is precipitated, filter the inorganic salt, concentrate the filtrate, and pass through A large amount of white crystals were precipitated by freezing, filtered, and dried to obtain 372 g of glufosinate-ammonium with a purity of 97% and a yield of 91.1%.

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a clean preparation method of glufosinate-ammonium, and aims to solve the problems that in the prior art, through hydrolysis of aminonitrile acid, equipment corrosion is serious, the amount of three wastes (waste gas, waste water and industrial residue) is large, and the existing product purification method has too low yield, complicated operation or high cost. The method comprises the following steps: preparing glufosinate sodium salt by adopting basic hydrolysis of aminonitrile, introducing carbon dioxide and ammonia gas, or directly adding NH4HCO3 into an aqueous solution of the glyphosate sodium salt, carrying out filtering separation on NaHCO3, and concentrating the filtrate to obtain an aqueous solution of glufosinate-ammonium or carrying out further concentrating and crystallization to obtain the glufosinate-ammonium; while by-product sodium bicarbonate can be further processed into sodium bicarbonate or sodium carbonate. With the preparation method provided by the invention, the problem of serious equipment corrosion during the hydrolysis of aminonitrile can be effectively solved, and the preparation method accords with cleaning production, has low production cost and wide application prospect, and has important progressive significance for the preparation of the glufosinate-ammonium.

Description

technical field [0001] The invention relates to the field of glufosinate-ammonium production, in particular to a clean preparation method for glufosinate-ammonium. The invention provides a clean separation and purification method for glufosinate-ammonium, which can effectively reduce the three wastes in the purification process of glufosinate-ammonium, prolong the service life of the equipment, simplify the purification operation, improve the purity of the product, and reduce the purification cost, and has good application prospect. Background technique [0002] The structural formula of glufosinate-ammonium is: It was successfully developed by Hoechst Company (later owned by Bayer Company), and belongs to organophosphorus herbicides, glutamine synthesis inhibitors, and non-selective contact herbicides. At present, glufosinate-ammonium can be used in orchards, vineyards, non-cultivated land, potato fields and other environments to control annual and perennial dicotyledono...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/30
CPCC07F9/301
Inventor 曾柏清蔡隆昌程柯范谦
Owner LIER CHEM CO LTD