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A kind of processing method of glyphosate mother liquor

A glyphosate mother liquor and treatment method technology, which is applied in the field of glyphosate mother liquor treatment, can solve problems such as high sodium chloride content, reduced crop quality, increased energy consumption, etc.

Inactive Publication Date: 2016-08-17
HEBI NONGLIN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the process for treating mother liquor has the following problems: (1) The total amount of mother liquor after treatment increases (by adding 30% sodium hydroxide solution, a large amount of water is brought in), which increases the energy consumption during concentration and increases the cost of sewage treatment; (2) The use of glyphosate water solution prepared by concentrated mother liquor (containing a large amount of sodium chloride) makes the content of sodium chloride in the spit too high, which will easily cause poor soil dispersion, sticky soil, and become sodium-alkaline soil, which will cause damage to crops. Harm and eventually lead to crop yield reduction and quality decline, so the Ministry of Agriculture has issued document No. 1158, prohibiting the use and sale of this water agent; (3) The herbicidal efficacy of this glyphosate sodium salt solution is both in terms of quick-acting and thorough Both are less effective than other glyphosate salt preparations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] In the four-stage series packed absorption tower device equipped with circulation, 215g of dimethylamine gas is introduced from the bottom of the first-stage tower, and 1000g of glyphosate mother liquor is introduced from the top of the fourth-stage tower, and the second-stage and third-stage The tower participates in the cycle, which can control the first-stage tower and the second-stage tower liquid. The feed temperature of the body is below 40°C. 1103g of liquid is collected from the bottom of the first-stage tower, and the pH value is 8.6. This solution is rectified, and the rectification tower The top temperature is 89°C-91°C. After rectification, 167g of triethylamine (the content is 99.03%) is obtained, the recovery rate is 62%, and the water content is 0.015; the mother liquor after rectification is evaporated and acidified with hydrochloric acid until the pH value is 2. After cooling, crystallization, filtration, and drying, 9.5 g of glyphosate technical substan...

Embodiment 2

[0046] In the four-stage series packed absorption tower device equipped with circulation, 283g of dimethylamine gas is introduced from the bottom of the first-stage tower, and 1000g of glyphosate mother liquor is introduced from the top of the fourth-stage tower, and the second-stage and third-stage The tower participates in the circulation, which can control the first-stage tower and the second-stage tower liquid. The feed temperature of the body is below 40°C. 1208g of liquid is collected from the bottom of the first-stage tower, and the pH value is 10.3. The solution is rectified, and the rectification tower The top temperature is 89°C-91°C. After rectification, 196g of triethylamine (99.1%) is obtained, the recovery rate is 73%, and the water content is 0.018; the mother liquor after rectification is evaporated and acidified with hydrochloric acid until the pH is 2. After cooling, crystallization, filtration, and drying, 10.2 g of the technical glyphosate was obtained, and ...

Embodiment 3

[0048] In the four-stage series packed absorption tower device equipped with circulation, 310g of dimethylamine gas is introduced from the bottom of the first-stage tower, 1000g of glyphosate mother liquor is introduced from the top of the fourth-stage tower, and the second-stage and third-stage The tower participates in the cycle, which can control the first-stage tower and the second-stage tower liquid. The feed temperature of the body is below 40°C. 1256g of liquid is collected from the bottom of the first-stage tower, and the pH value is 11.8. This solution is rectified, and the rectification tower The top temperature is 89°C-91°C. After rectification, 266g of triethylamine (its content is 99.13%) is obtained, the recovery rate is 98.3%, and the water content is 0.018; the mother liquor after rectification is evaporated and acidified with hydrochloric acid until the pH value is 2. After cooling, crystallization, filtration, and drying, 10.5 g of the technical glyphosate was...

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Abstract

The invention provides a method for treating glyphosate mother liquor. The method comprises the following steps: introducing dimethylamine gas into the bottom of a gas-liquid countercurrent packed tower, absorbing the dimethylamine gas through taking the glyphosate mother liquor as an absorbent and collecting alkaline liquid at the bottom of the tower; introducing the liquid into a rectifying tower for rectification to obtain triethylamine and tower bottom liquid; dehydrating the tower bottom liquid at reduced pressure, adding hydrochloric acid to adjust the pH value of the tower bottom liquid to strong acidity, cooling, crystallizing and filtering to obtain glyphosate; and further distilling the filtered filtrate at reduced pressure to obtain dimethylamine hydrochloride. Compared with the prior art, the method provided by the invention has the advantages that the dimethylamine gas is utilized to replace other liquid alkalies to recover the catalyst triethylamine in the glyphosate mother liquor, the obtained glyphosate and the dimethylamine hydrochloride are useful chemical products and no waste is produced, so that the method is high in recovery rate, high in recovery product quality, friendly to environment and economic; in the meanwhile, the gas-liquid countercurrent packed tower is adopted in the method, so that the method is more safe in reaction and is beneficial to the continuous and large scale treatment of the glyphosate mother liquor.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a treatment method for glyphosate mother liquor. Background technique [0002] Glyphosate is a high-efficiency, broad-spectrum, systemic, and conductive organophosphorus chemical herbicide. It has the advantages of wide application, good weeding effect, low price, and good environmental compatibility. It is currently the most widely used herbicide in the world. One of the most widely used and produced chemical herbicides. It was developed by Monsanto in the United States in the early 1970s and registered in the United States in 1974. The production of glyphosate in my country started in the 1980s and was synthesized by the dimethyl phosphite method (also known as the glycine method) in 1986. The process of glyphosate has been industrialized in China. The raw materials of this method are easy to obtain, the process conditions are stable, the yield is high, and s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/38C07C211/05C07C209/86
Inventor 张卫亮刘玉安
Owner HEBI NONGLIN PHARMA
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