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Recovery method of N-methyl pyrrolidone

A technology of methyl pyrrolidone and a recovery method, applied in directions such as organic chemistry, can solve the problems of insufficient separation, low recovery rate, high consumption, etc., and achieve the effects of improving recovery quality, reducing impurities and improving quality

Inactive Publication Date: 2020-04-17
赣州中能实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing N-methylpyrrolidone method generally has problems such as high energy consumption and low recovery rate in the recovery process, and it often needs to consume higher energy to separate N-methylpyrrolidone from other waste liquids, which not only wastes energy, but also And the separation is not clean enough, which affects the recovery quality of N-methylpyrrolidone

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A recovery method for N-methylpyrrolidone, comprising the following steps:

[0025] 1) Take the waste material of lithium battery electrode material, add deionized water of 1 times the weight of the waste material to it, stir it evenly, soak it for 1 hour; pulverize it, and use ultrasonic dispersion with a frequency of 40KHz during the pulverization process to obtain a waste material mixture ;

[0026] 2) Add polyaluminum chloride 0.1 times the total weight of the waste mixture to the waste mixture obtained in step 1); after stirring, let it stand for 10 minutes and filter to obtain solid flocs and filtrate;

[0027] 3) Send the filtrate obtained in step 2) into the reaction kettle, and perform vacuum treatment to reduce the pressure in the reaction kettle to 10KPa, heat the filtrate in the reaction kettle, and keep it when the temperature rises to 120°C Constant temperature, carry out fractional distillation on the filtrate, obtain N-methylpyrrolidone crude liquid and...

Embodiment 2

[0030] A recovery method for N-methylpyrrolidone, comprising the following steps:

[0031] 1) Take the waste of lithium battery electrode materials, add deionized water twice the weight of the waste to it, stir evenly, soak for 2 hours; crush it, and use ultrasonic dispersion with a frequency of 60KHz during the crushing process to obtain a waste mixture ;

[0032] 2) Add polyferric sulfate 0.2 times the total weight of the waste mixture to the waste mixture obtained in step 1); after stirring, let it stand for 20 minutes and filter to obtain solid flocs and filtrate;

[0033] 3) Send the filtrate obtained in step 2) into the reaction kettle, and perform vacuum treatment to reduce the pressure in the reaction kettle to 20KPa, heat the filtrate in the reaction kettle, and keep it when the temperature rises to 140°C Constant temperature, carry out fractional distillation on the filtrate, obtain N-methylpyrrolidone crude liquid and mixed liquid I after fractional distillation; ...

Embodiment 3

[0036] 1) Take the waste of lithium battery electrode materials, add deionized water 1.5 times the weight of the waste to it, stir it evenly and soak for 1.5 hours; crush it, and use ultrasonic dispersion with a frequency of 50KHz during the crushing process to obtain waste mixed liquid;

[0037] 2) Add flocculant 0.15 times the total weight of the waste mixture to the waste mixture obtained in step 1), the flocculant is made by mixing polyaluminum sulfate and polyferric chloride in a weight ratio of 1:3; after stirring Stand still for 15min, filter to obtain solid floc and filtrate;

[0038] 3) Send the filtrate obtained in step 2) into the reaction kettle, and perform vacuum treatment to reduce the pressure in the reaction kettle to 15KPa, heat the filtrate in the reaction kettle, and keep it when the temperature rises to 130°C Constant temperature, carry out fractional distillation on the filtrate, obtain N-methylpyrrolidone crude liquid and mixed liquid I after fractional...

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Abstract

The invention discloses a recovery method of N-methyl pyrrolidone. The recovery method comprises the following steps: 1) taking a waste material of a lithium battery electrode material, adding deionized water into the waste material, uniformly stirring, soaking, crushing, and performing ultrasonic wave dispersion in the crushing process to obtain a waste material mixed solution; 2) adding a flocculating agent into the waste material mixed solution obtained in the step 1), stirring, standing, and filtering to obtain solid floc and filtrate; 3) feeding the filtrate obtained in the step 2) into areaction kettle, heating the filtrate in the reaction kettle, and fractionating the filtrate; and 4) feeding the N-methyl pyrrolidone crude liquid obtained in the step 3) into the reaction kettle, heating the filtrate in the reaction kettle, and rectifying the N-methyl pyrrolidone crude liquid. The method is beneficial to improving the quality of subsequent N-methyl pyrrolidone fractionation, improving the recovery quality of N-methyl pyrrolidone and saving energy.

Description

technical field [0001] The invention relates to the technical field of N-methylpyrrolidone recovery, in particular to a recovery method for N-methylpyrrolidone. Background technique [0002] N-Methylpyrrolidone is an important chemical raw material, which belongs to polar aprotic solvent, can be miscible with water in any proportion, and can be completely mixed with almost all organic solvents (ethanol, acetaldehyde, ketone, aromatic hydrocarbon, etc.), Strong polarity, low viscosity, strong solubility, low toxicity, strong biodegradability, excellent chemical stability and thermal stability, mainly used in petrochemical industry, plastic industry, pharmaceuticals, pesticides, dyes and lithium-ion battery manufacturing industries, etc. industry. [0003] In the production of the lithium battery industry, a large amount of N-methylpyrrolidone needs to be used. After the lithium battery reaches the end of its service life, it needs to be scrapped. Recycling and reuse of N-met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 黄春锦刘甫先周伟
Owner 赣州中能实业有限公司
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