Purifying method of N-methylpyrrolidone

A technology for methylpyrrolidone and purification methods, applied in chemical instruments and methods, separation methods, organic chemistry, etc., can solve the problems of low yield, unstable yield, easy moisture absorption, etc., and achieve simple process route and low manufacturing cost Low, consistent quality results

Inactive Publication Date: 2010-04-21
北京益利精细化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

N-methylpyrrolidone is easy to absorb moisture, and it is difficult to produce a large amount of products that meet the requirements. The traditional purification method is to add benzene and azeotropic distillation, which not only has a low yield, but also is unstable, and it is easy to cause benzene to the product. Impurity pollution

Method used

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  • Purifying method of N-methylpyrrolidone
  • Purifying method of N-methylpyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The N-methylpyrrolidone to be purified is passed through a specification of Activated carbon column, activated carbon particles are strip-shaped particles, adsorbing methylamine to make the content below 0.005%; and then passing the specification as Two series-connected molecular sieve columns of model 3A absorb moisture to reduce the moisture to less than 0.01%; finally, the solid particles are removed by ultra-fine filtration, and enter the finished product bottle in a dry environment, and the yield of the finished product is 95%. Wherein, the flow rate of N-methylpyrrolidone in the purification process is 0.4 liters / hour.

Embodiment 2

[0017] The N-methylpyrrolidone to be purified is passed through a specification of Activated carbon column, activated carbon particles are Spherical or strips, absorbing methylamine to make the content below 0.005%; then the specification is Two series-connected molecular sieve columns of model 4A absorb water to reduce the water to less than 0.01%; finally, the solid particles are removed by ultra-fine filtration, and enter the finished product bottle in a dry environment. The yield of the finished product is 96%. Wherein, the flow rate of N-methylpyrrolidone during the purification process is 0.5 liter / hour.

Embodiment 3

[0019] The N-methylpyrrolidone to be purified is passed through a specification of Activated carbon column, the diameter of activated carbon particles is 2mm, absorbing methylamine to make the content below 0.005%; and then the specification is Two series-connected molecular sieve columns of model 5A absorb moisture to reduce the moisture to less than 0.01%; finally, the solid particles are removed by ultra-fine filtration, and enter the finished product bottle in a dry environment, and the yield of the finished product is 97%. Wherein, the flow rate of N-methylpyrrolidone in the purification process is 0.6 liters / hour.

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Abstract

The invention relates to a purifying method of N-methylpyrrolidone, comprising the following steps: absorbing aminomethane from N-methylpyrrolidone to be purified through an activated-charcoal column; then removing water through a molecular sieve column; and finally removing solid particulates through ultrafiltration to obtain a finished product. The purifying method of N-methylpyrrolidone is used for purifying the N-methylpyrrolidone by utilizing a solid (activated charcoal and a molecular sieve) absorbing method instead of a distillation method. The method has simple process route and easy operation; the activated-charcoal column is used for removing the aminomethane in the N-methylpyrrolidone so that the content of the aminomethane reach below 0.005 percent, and the molecular sieve column ensures that the water content in the N-methylpyrrolidone is lowered to below 0.01 percent, thereby efficiently removing impurities. The N-methylpyrrolidone purified by the method has stable quality, high yield of at least 95 percent and low manufacturing cost; and the activated charcoal and the molecular sieve are recyclable after losing efficacy, thereby having the advantages of cost saving and environment protection.

Description

technical field [0001] The invention relates to a purification method of N-methylpyrrolidone, which is used for removing impurities such as methylamine and moisture therein. Background technique [0002] N-Methylpyrrolidone is a valuable solvent, which is used as a high-boiling-point, low-volatility solvent for electronic component cleaning agents and biological products in the microelectronics industry. The conventional production method of N-methylpyrrolidone is to react methylamine with r-butyrolactone, and its main impurities are water and methylamine. [0003] Due to the relatively high quality requirements for industrial-grade N-methylpyrrolidone, the moisture content is required to be below 0.01%, and the methylamine content is required to be lower. N-methylpyrrolidone is easy to absorb moisture, and it is difficult to produce a large amount of products that meet the requirements. The traditional purification method is to add benzene and azeotropic distillation, whic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267B01D15/00
Inventor 刘殿莹郭存林赵玉峰杨秀玉
Owner 北京益利精细化学品有限公司
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