CN101570547A - Method for processing glyphosate mother liquor - Google Patents

Abstract

A method for processing glyphosate mother liquor, comprising the following steps: (1) adding triethylamine as extractant to glyphosate acid mother liquor, mixing evenly, regulating the PH value of the obtained solution to 8-10 by adding alkali for standing and layering, separating the solution to obtain triethylamine salt solution on the upper layer and glyphosate concentrated mother liquor on the lower layer which has 6%-8% of glyphosate; (2) regulating the PH value of glyphosate concentrated mother liquor obtained in step (1) to about 11 by adding alkali, distilling the solution and obtaining a small quantity of triethylamine and a residual mother liquor which can be used to prepare 30% glyphosate ammonium water solution. The invention has the advantages that the operation of the invention is simple and the cost is low, the content of the obtained glyphosate mother liquor reaches 6-8% and sodium chloride in the concentrated mother liquor is few which can be used to prepare 30% glyphosate ammonium water solution.

Description

The treatment process of glyphosate mother solution

Technical field

The present invention relates to a kind of treatment process of glyphosate mother solution, relate in particular to a kind of treatment process of glyphosate by using glycine mother liquor.

Background technology

Glyphosate is a most popular weedicide on the world market, has characteristics such as efficient, low toxicity and noresidue, and China is the production base of glyphosate maximum at present.Glyphosate production mainly contains two kinds of methods, and the one, the IDA method, offshore company generally adopts this method, another kind of glycine method, domestic big multiple enterprises adopts this method, and production capacity is above 300,000 tons/year.Can produce a large amount of Cl that contains during preparing glyphosate by glycin method ^-Acid mother liquid, the main method of domestic most glyphosate production business processes mother liquors is: add 30% sodium hydroxide solution in acid mother liquor, regulate pH value 10-12, standing demix, reclaim the upper strata catalyst of triethylamine, the residue alkali liquor is after concentrate, removing part sodium-chlor, get the concentrated mother liquor that glyphosate content is about 2-3%, be used to prepare 10% sodium glyphosate aqua.Because contain a large amount of sodium-chlor in the 10% sodium glyphosate aqua, weeding ratio is low in the use, environmental pollution is serious, and usage quantity reduces year by year, and will eliminate out weedicide market behind 1-2.

Summary of the invention

The object of the invention is to provide a kind of production cost low, the mother liquor processing method that the glyphosate utility value is high, and this method reaction conditions gentleness, glyphosate mother solution pollutes little after treatment, glyphosate content height in the recovery.

The present invention is achieved in that and it is characterized in that processing step is:

(1) press extraction agent triethylamine and glyphosphonic acid aqueous mother liquor weight ratio 1: 2-5 mixes, under temperature 30-60 ℃, in mother liquor, add triethylamine, after stirring, add alkali and regulate PH to 8-10, standing demix separates the upper strata, back and gets triethylamine salt solution, lower floor gets the dense mother liquor of glyphosate, and its glyphosate content is 6%-8%;

(2) add alkali behind the dense mother liquor of glyphosate that step (1) is obtained, transfer pH to 11-12, distill out triethylamine, the residue mother liquor is used to prepare 30% ammonium glyphosate aqua;

(3) with the triethylamine salt solution that obtains in the step (1), add alkali and transfer pH value 10-12, standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of glyphosate, and a small amount of triethylamine is told in lower floor's rectifying, enters Sewage treatment systems.

Alkali of the present invention is sodium hydroxide, and its concentration is 30%-99%.

Advantage of the present invention is: 1, use this method simple to operate, cost is low; The catalyzer of using in extraction agent that uses in the process and the reaction all is a triethylamine, reclaims easy.2, the glyphosate mother solution content that obtains reaches 6-8%, and sodium-chlor is few in the dense mother liquor, can be used for preparing 30% ammonium glyphosate aqua.

Embodiment

Embodiment one

Get adding triethylamine 100g in the 400g glyphosphonic acid mother liquor, after stirring, add 98% sodium hydroxide 25g, regulate PH to 9.0, standing demix, upper strata triethylamine salt solution weight 418.5g, the heavy 106.5g of the dense mother liquor of lower floor's glyphosate, glyphosate content is 7.25%;

Triethylamine salt solution adds 30% sodium hydroxide accent pH to 12, and standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of glyphosate, and a small amount of triethylamine is told in lower floor's rectifying, enters Sewage treatment systems.

The dense mother liquor of glyphosate adds 98% sodium hydroxide accent pH to 11, and rectifying goes out a spot of triethylamine, the heavy 108.0g of residue mother liquor, and glyphosate content 7.15% is used to prepare 30% ammonium glyphosate aqua.

Embodiment two

Get adding triethylamine 100g in the 400g glyphosphonic acid mother liquor, after stirring, add 30% sodium hydroxide 90g, regulate PH to 9.3, standing demix, upper strata triethylamine salt solution weight 474.5g, the heavy 115.5g of the dense mother liquor of lower floor's glyphosate, glyphosate content is 6.65%;

Upper strata triethylamine salt solution adds 30% sodium hydroxide accent pH to 12, and standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of glyphosate, and a small amount of triethylamine is told in lower floor's rectifying, enters Sewage treatment systems.

The dense mother liquor of glyphosate adds 30% sodium hydroxide accent pH to 11, and rectifying goes out a spot of triethylamine, the heavy 126.5g of residue mother liquor, and glyphosate content 6.08% is used to prepare 30% ammonium glyphosate aqua.

Claims (2)

1, a kind of treatment process of glyphosate mother solution is characterized in that process method step is:

(1) press extraction agent triethylamine and glyphosphonic acid aqueous mother liquor weight ratio 1: 2-5 mixes, under temperature 30-60 ℃, in mother liquor, add triethylamine, after stirring, add alkali and regulate PH to 8-10, standing demix separates the upper strata, back and gets triethylamine salt solution, lower floor gets the dense mother liquor of glyphosate, and its glyphosate content is 6%-8%;

(2) add alkali behind the dense mother liquor of glyphosate that step (1) is obtained, transfer pH to 11-12, distill out triethylamine, the residue mother liquor is used to prepare 30% ammonium glyphosate aqua;

(3) with the triethylamine salt solution that obtains in the step (1), add alkali and transfer pH value 10-12, standing demix reclaims the upper strata triethylamine and is re-used in the synthetic production of glyphosate, and a small amount of triethylamine is told in lower floor's rectifying, enters Sewage treatment systems.

2, the treatment process of glyphosate mother solution according to claim 1 is characterized in that alkali is sodium hydroxide, and its concentration is 30%-99%.