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Method for treating glyphosate mother solution

A technology of glyphosate mother liquor and treatment method, which is applied in the field of glyphosate mother liquor treatment, can solve the problems of high cost, difficult recycling of glyphosate ammonium salt solution, low recovery rate of triethylamine, etc., and achieve improved recovery rate , Great environmental protection and economic benefits, outstanding environmental protection and economic benefits

Active Publication Date: 2013-07-03
SHANDONG WEIFANG RAINBOW CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patents 200410099086.4 and 200610154907.9 propose to feed ammonia into the glyphosate mother liquor to recover triethylamine, then distill and dehydrate to remove ammonium chloride to obtain concentrated glyphosate ammonium salt, but the recovery rate of triethylamine is low, and the obtained concentrated grass Glyphosate ammonium salt solution is also not easy to recycle, and the cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 1000.0g of glyphosate crystallization mother liquor containing 19.8% of triethylamine, add 800.0g of aqueous solution of calcium hydroxide with a concentration of 10%, fully stir and mix evenly, the pH of the mixed solution is 10.5, and inject it into normal pressure (absolute pressure is 1.0atm) Distillation is carried out in the distillation device, and the fraction at 70-100°C is collected.

[0030] The distilled distillate was colorless and transparent triethylamine, which was dehydrated with caustic soda to obtain 198.0 g of 98.5% triethylamine, with a water content of 0.4%, and a recovery rate of triethylamine of 98.5%.

[0031] Add hydrochloric acid to the tower bottom residue after distillation to adjust to neutral filtration and separation to obtain a calcium chloride solution with a concentration of about 15%.

Embodiment 2

[0033] Get the calcium chloride solution that obtains among the embodiment 1 and add calcium oxide to be made into 20% aqueous solution, for subsequent use.

[0034] Take 1000.0 g of the glyphosate crystallization mother liquor containing 19.8% of triethylamine, add 420.0 g of an aqueous solution of calcium hydroxide with a concentration of 20% and fully stir and mix evenly. The pH of the mixed solution is 11.0. Distillation is carried out in the distillation device, and the fraction at 45-70°C is collected.

[0035] The distilled distillate was colorless and transparent triethylamine, which was dehydrated with calcium oxide to obtain 199.1 g of 98.5% triethylamine with a water content of 0.5% and a recovery rate of triethylamine of 99.0%.

[0036] Add hydrochloric acid to the tower bottom residue after distillation to adjust to neutral filtration and separation to obtain a calcium chloride solution with a concentration of about 25%.

Embodiment 3

[0038] Get the calcium chloride solution that obtains among the embodiment 1 and add calcium oxide to be made into 25% aqueous solution, for subsequent use.

[0039] Take 1000.0 g of glyphosate crystallization mother liquor containing 19.8% of triethylamine, add 350.0 g of an aqueous solution of calcium hydroxide with a concentration of 25% and stir and mix evenly, the pH of the mixed solution is 11.8, and inject it under reduced pressure (absolute pressure is 0.1 atm) Distillation is carried out in the distillation device, and the fraction at 40-60°C is collected.

[0040] The distilled distillate was colorless and transparent triethylamine, which was dehydrated with calcium oxide to obtain 200.0 g of 98.5% triethylamine with a water content of 0.4% and a recovery rate of triethylamine of 99.5%.

[0041] Add hydrochloric acid to the residual liquid at the bottom of the distillation to adjust to neutral filtration and separation to obtain a calcium chloride solution with a con...

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Abstract

The invention discloses a method for treating glyphosate mother solution, which comprises the following steps of: adding aqueous solution of calcium hydroxide into the glyphosate mother solution to regulate pH until the solution is alkaline and make triethylamine hydrochloride in the mother solution generate triethylamine simultaneously; adding the treated glyphosate mother solution into a distillation tower for distillation, and collecting 40 to 100 DEG C fractions on the top of the tower; adding a dehydrating agent into the fractions on the top of the tower to obtain the triethylamine; and adding hydrochloric acid into the mother solution at the bottom of the tower to regulate the pH until the solution is neutral, performing solid-liquid separation and treating and discharging separatedwaste water. The process is simple and high-efficiency; the recovery rate of the triethylamine is over 98.5 percent; the chemical oxygen demand (COD) of the discharged waste water is less than 500mg / L, total phosphate (TP) is less than 1mg / L and ammonia nitrogen is less than 15mg / L; the zero emission of the waste water is basically realized; and the method has great environmental benefit and economical benefit.

Description

technical field [0001] The invention relates to a treatment method for glyphosate mother liquor, in particular to a treatment method for recovering triethylamine from glyphosate crystallization mother liquor obtained by producing glyphosate by a dialkyl phosphite method so that there is basically no waste water discharge. technical background [0002] As a high-efficiency, broad-spectrum, and low-toxicity herbicide, glyphosate is widely used and has become the most widely used herbicide in the world. At present, dialkyl phosphite is mostly used in the preparation of glyphosate in China. Ester method and iminodiacetic acid method. [0003] At present, the treatment process of the glyphosate crystallization mother liquor produced in the process of producing glyphosate by dialkyl phosphite method is mainly to neutralize the crystallization mother liquor with liquid alkali, so that the triethylamine in the mother liquor is separated out, and then transferred to synthesis after d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/05C07C209/86C02F9/10C01F11/32
Inventor 刘月栋孙国庆李志清陈琦李文静
Owner SHANDONG WEIFANG RAINBOW CHEM
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