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Method for recovering and purifying 2-methylpyridine waste liquid

A technology of picoline and a purification method, applied in the field of recovery and purification of 2-picoline waste liquid, can solve the problems of affecting the amount of solution recovery, affecting the drying and use of materials, unfavorable cleaning of drying equipment, etc., so as to facilitate sufficient collection and operation Stable and cost-saving effect

Inactive Publication Date: 2021-10-22
四川熔增环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production of pesticides, a large amount of 2-picoline waste solvents containing impurities such as organic matter, water and salts are produced. Due to the high difficulty of purification, most of them are discarded and no longer used, resulting in great waste and great pollution to the environment after discharge. At the same time, in the existing technology, the material drying and recovery technology of the distillation column and tower kettle is limited, and the existing drying treatment equipment cannot fully contact the waste, which affects the drying and use of the material. The recovery weight is not conducive to the cleaning of drying equipment

Method used

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  • Method for recovering and purifying 2-methylpyridine waste liquid
  • Method for recovering and purifying 2-methylpyridine waste liquid
  • Method for recovering and purifying 2-methylpyridine waste liquid

Examples

Experimental program
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Effect test

Embodiment 1

[0039] according to figure 1 , a method for recovering and purifying 2-picoline waste solvent, characterized in that the step of extracting comprises:

[0040] Take the waste solvent containing 55% 2-picoline in 0.5m 3 / h is pumped into the pressure swing rectification column, and the positive pressure rectification obtains the isopropanol-water azeotropic component at the top of the tower. The middle liquid temperature is 99°C, the tank top temperature is 98°C, and the reflux ratio is 15:1.

[0041] The isopropanol-water azeotropic component that above-mentioned rectification obtains is with 1.5m 3 / h steam is passed into the pervaporation membrane, and the dehydrated isopropanol is circulated into the pressure swing rectification column.

[0042] From the side line of the pressure swing rectification tower at 0.20m 3 2-methylpyridine is mined in / h; industrial-grade 2-picoline with a purity of ≥99.9% (wt) is obtained.

[0043] Distillation tower kettle material accordin...

Embodiment 2

[0045] Based on embodiment 1, a kind of recovery and purification method of 2-picoline waste solvent is characterized in that, the extraction step comprises:

[0046] Take 60% 2-picoline waste solvent with 0.6m 3 / h is pumped into the pressure swing rectification column, and the positive pressure rectification obtains the isopropanol-water azeotropic component at the top of the tower. The middle liquid temperature is 118°C, the tank top temperature is 117°C, and the reflux ratio is 20:1.

[0047] The isopropanol-water azeotropic component that above-mentioned rectification obtains is with 1m 3 / h steam is passed into the pervaporation membrane, and the dehydrated isopropanol is circulated into the pressure swing rectification column.

[0048] From the side line of the pressure swing rectification tower at 0.29m 3 2-methylpyridine is mined in / h; industrial-grade 2-picoline with a purity of ≥99.9% (wt) is obtained.

[0049] Distillation tower kettle material according to 0.19...

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Abstract

The invention discloses a method for recovering and purifying 2-methylpyridine waste liquid. The method comprises the following steps that: a, agrochemical waste containing sulfonate, sodium chloride and 2-methylpyridine is weighed, then is introduced into a pressure-swing rectifying tower at a certain flow rate, and is rectified at a certain temperature and pressure; b, a rectified tower top component is an organic component azeotropic with water, the component enters a pervaporation membrane in the form of steam under certain flow and pressure control and undergoes dehydration, a dehydrated organic solvent is introduced into the pressure-swing rectifying tower at a certain flow, and water in the pressure-swing rectifying tower is circularly removed; and c, a 2-methylpyridine finished product is extracted at a certain flow rate from the side line position of the pressure-swing rectifying tower. The industrial-grade 2-methylpyridine is obtained through the methods of pressure swing distillation, pervaporation membrane-coupled distillation dehydration, azeotropic solvent recycling, side-drawing of the product and drying of a tower-bottom material through a rake type drying mechanism, and the industrial-grade 2-methylpyridine can be easily purified from a agrochemical waste solvent containing sulfonate and sodium chloride.

Description

technical field [0001] The invention relates to the technical field of solvent purification of waste solvents, in particular to a method for recovering and purifying 2-picoline waste liquid. Background technique [0002] With the development of organic synthesis technology and pesticide active molecule design skills and the demand for new pesticides in agricultural production, a variety of 2-picoline-containing pesticides came out after the 1960s. Daohua developed triclopyr, Ishihara developed fluazifop, etc. Germany Bayer and Japan Special Pesticides jointly developed imidacloprid. Today, 2-picoline pesticides have been developed into many varieties including fungicides, insecticides and acaricides, herbicides and plant growth regulators. In the production of pesticides, a large amount of 2-picoline waste solvents containing impurities such as organic matter, water and salts are produced. Due to the high difficulty of purification, most of them are discarded and no longer ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/16F26B25/00F26B25/04F26B25/12
CPCC07D213/16F26B25/04F26B25/12F26B25/002
Inventor 范文林黄啟虓纪王洋鲁加峰
Owner 四川熔增环保科技有限公司
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