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Method for producing glyphosate ammonium salt solid preparation

A glyphosate ammonium salt and solid preparation technology, applied in the field of pesticides, can solve the problems of failure to consider recycling and poor economic benefits, etc.

Active Publication Date: 2010-08-11
HANGZHOU JINFADA CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the existing ammonium salt synthesis, the glyphosate raw drug or wet block reacts with gaseous ammonia, liquid ammonia or ammonia water, and fails to consider recycling the glyphosate in the mother liquor
For example, the invention patent application with publication number CN1260349 discloses the technical scheme of glyphosate and liquid ammonia reaction to form ammonium glyphosate; the invention patent application with publication number CN1340508 discloses the reaction of glyphosate and ammonia in the organic phase to form ammonium glyphosate The technical scheme of salt; the invention patent application with publication number CN1445234 discloses the technical scheme of gas-liquid-solid three-phase reaction and solvent extraction to prepare ammonium glyphosate; the invention patent application with publication number CN1724547 discloses that glyphosate is used as a fixed phase and ammonia water as the mobile phase to synthesize glyphosate ammonium salt, the obtained glyphosate is not suitable to be directly made into glyphosate ammonium salt solid preparation in the same reaction vessel, glyphosate ammonium salt needs to be collected separately After being processed into ammonium salt solid preparations, and the recovery and use of glyphosate in the glyphosate mother liquor has not been considered, the economic benefit is poor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Treat the glyphosate mother liquor with sodium hydroxide to make its pH value 9-11, triethylamine is layered, the lower layer is the alkali mother liquor, and the upper layer triethylamine is separated, and the alkali mother liquor is recovered by rectification. Amine, the recovered triethylamine plus solid sodium hydroxide is dehydrated and returned to the previous process as a catalyst. The obtained mother liquor is a mother liquor with a sodium chloride content greater than 3%. After removing impurities by microfiltration and ultrafiltration, the mother liquor is concentrated by membrane The stage separation treatment method removes sodium, and the membrane concentration and multi-stage separation treatment are divided into concentrated liquid and light liquid, and the concentrated liquid is used as a spare mother liquid. Get its dope 60g, glyphosate former powder 140g, ventilate ammonia under the condition of material kneading, material temperature rises, ...

Embodiment 2

[0027] Embodiment 2: Treat the glyphosate mother liquor with ammonia to recover triethylamine, the obtained mother liquor is a mother liquor with a sodium chloride content less than 3%, and the mother liquor is directly used as a spare mother liquor. Take 110 g of its spare mother liquor, add 150 g of glyphosate raw powder to form a suspension, feed gas ammonia, the reaction temperature is 40-90 ° C, stop the ammonia feeding when the pH value of the reactant reaches 5, and obtain glyphosate ammonium salt, Appropriate water is evaporated, and then the material is sent to the kneader while it is hot, cooled in the kneader and kneaded by adding 24g of polyethylene glycol and fatty alcohol polyoxyethylene ether mixture, and finally granulated and dried to make glyphosate ammonium salt solid Granules.

Embodiment 3

[0028] Embodiment 3: The acquisition of standby mother liquor is the same as in Example 1. Get 100g of standby mother liquor, add glyphosate former medicine 95g, feed gaseous ammonia under stirring, until the solution is transparent, stop feeding ammonia when the pH value is 5, and the temperature of the material rises to 70°C, then cool the material to 30°C, the glyphosate ammonium salt crystallizes out, and the water jet vacuum pump evacuates the solution to filter the solution to obtain 91g of filtrate, 96g of glyphosate ammonium salt filter residue, kneading with glyphosate ammonium salt plus 15g of auxiliary agent, The auxiliary agent is a mixture of alkyl polyglycosides, polyethylene glycol and fatty alcohol polyoxyethylene ether, and finally granulated and dried to make glyphosate ammonium salt solid granules, and the filtrate is recovered and the standby mother liquor in step 3) Mixed use.

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Abstract

The invention provides a method for producing a glyhosate ammonium solid preparation, which belongs to the technical field of pesticide. The method takes glyphosate and a glyphosate mother solution produced by an alkyl ester method as raw materials, and is characterized by comprising the following steps: (1) in a production process of the alkyl ester method, after the acid hydrolysis of the glyphosate is over, the pH value of the mother solution is adjusted to be 0 to 3; the glyphosate is crystallized, separated out, filtered and washed; a filter cake is the glyphosate; and a filtrate is the glyphosate mother solution; (2) triethylamine in the glyphosate mother solution is recovered so as to obtain a standby mother solution; and (3) the standby mother solution is taken as a solvent or a wetting agent, the glyphosate reacts with ammonia so as to generate glyhosate ammonium; the reaction temperature is between 40 and 90 DEG C, and when the pH value of materials is between 4 and 6, gas ammonia or ammonia water supply is stopped; additives are added and well mixed; and glyhosate ammonium solid granules are finally prepared via granulation and drying. The production method has the advantages of simplifying processing steps, along with remarkable economic benefit.

Description

technical field [0001] The invention belongs to the technical field of pesticides, in particular to a production method of glyphosate ammonium salt solid preparation. Background technique [0002] Glyphosate is the systemic herbicide with the largest sales volume and the fastest growth rate in the world, and with the successful development and popularization of glyphosate-transgenic crops and the shortage of energy sources, it has led to the sowing and promotion of biofuel crops. The production of phosphine offers new opportunities. [0003] Glyphosate (glyphosate), the chemical name is N-(phosphine carboxymethyl) glycine, the pure product is a non-volatile white solid, the specific gravity is 0.5, it melts at about 230 ° C, and it is accompanied by decomposition. The solubility in water at room temperature Only 1.2 grams, insoluble in general organic solvents, its isopropylamine salt is completely soluble in water, non-flammable, non-explosive, stable in normal temperature...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): A01N57/20A01P13/00
Inventor 孔鑫明俞叶明刘劭农刘开孟
Owner HANGZHOU JINFADA CHEM IND