Recovery method of N-methylpyrrolidone

A technology of methylpyrrolidone and recovery method, which is applied in the direction of organic chemistry, can solve the problems of low energy consumption, high energy consumption, and low recovery rate, and achieve the goals of simplifying operation technology, reducing energy consumption, and improving recovery rate and pass rate Effect

Active Publication Date: 2014-07-23
HUIZHOU BYD BATTERY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the technical problems of high energy consumption and low recovery rate of the existing recovery method of N-met

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] Example 1

[0016] Take 5000kg of NMP raw material containing 23% water and put it into the batch distillation kettle, under -0.09MPa vacuum, heat and rectify with 130℃ heat conduction oil, total reflux time 0.5h, reflux ratio control 4, carry out water removal treatment, obtain crude NMP A1 , The first step of distillation requires 5 hours; then the heat transfer oil is heated to 180°C, the total reflux time is 1h, the reflux ratio is controlled 2, and the NMP is purified by distillation to obtain NMP B1, which is required for the second step of distillation The time is 7 hours.

Example Embodiment

[0017] Example 2

[0018] Take 5000kg of NMP raw material containing 15% water and put it into the batch distillation kettle, under -0.05MPa vacuum, heat and rectify with 100℃ heat conduction oil, total reflux time 0.5h, reflux ratio control 5, carry out water removal treatment, obtain crude NMP A2 , The first step of distillation requires 9 hours; then the heat transfer oil is heated to 200℃, the total reflux time is 1h, the reflux ratio is controlled to 5, and the NMP is purified by distillation to obtain NMP B2, which is required for the second step of distillation The time is 10 hours.

Example Embodiment

[0019] Example 3

[0020] Take 5000kg of NMP raw material containing 35% water and put it into the batch distillation kettle, under -0.08MPa vacuum, heat and rectify with 160℃ heat conduction oil, total reflux time 0.5h, reflux ratio control 2, and carry out water removal treatment to obtain crude NMP A3 , The first step of distillation requires 4.5 hours; then the heat transfer oil is heated to 160℃, the total reflux time is 1h, the reflux ratio is controlled to 0.1, and the NMP is purified by distillation to obtain NMP B3, which is required for the second step of distillation The time is 12 hours.

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Abstract

The invention provides a recovery method of N-methylpyrrolidone. A single-tower intermittent vacuum rectification technology is adopted to process an N-methylpyrrolidone recovery solution with a high water content, during the technology process, the heating temperature is 100 to 160 DEG C, the pressure is -0.099 to -0.05 MPa, most of water is removed through vacuum rectification so as to obtain a crude product of N-methylpyrrolidone, and then the crude product of N-methylpyrrolidone is subject to rectification at a temperature of 160 to 210 DEG C under a pressure of -0.099 to -0.05 MPa to separate the N-methylpyrrolidone from other heavy impurities so as to obtain the N-methylpyrrolidone product. The recovery method is used to process the N-methylpyrrolidone recovery solution, which is generated during the production process of lithium battery electrodes, to obtain a recovery product of N-methylpyrrolidone; the purity of the product can reach 99.95% or more, the water content is 500 ppm or less, the product can fully satisfy the requirements of lithium battery production, and circulation recovery and reutilization are achieved.

Description

technical field [0001] The present invention relates to the recovery method of N-methylpyrrolidone. Background technique [0002] N-methylpyrrolidone (NMP for short) is widely used in many industries such as petrochemical industry, plastic industry, pharmaceuticals, pesticides, dyes and lithium-ion battery manufacturing. Among them, in the lithium battery electrode manufacturing process, through the recovery of NMP waste gas, NMP recovery liquid containing a large amount of waste residue, waste water and other impurities is obtained. One of the existing technologies is to carry out continuous vacuum distillation to the recovered liquid. This method can obtain high-purity NMP solvent, which is suitable for mass production, has large investment, high energy consumption, and is not conducive to the recovery of a small amount of NMP waste solution. . In addition, some manufacturers carry out mixed batch rectification of normal pressure and reduced pressure on the recovered liq...

Claims

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Application Information

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IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 姚利周天承
Owner HUIZHOU BYD BATTERY
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