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A kind of method that adds stabilizing agent to suppress the chloroform acidification of n-methylpyrrolidone/chloroform separation process

A technology of separation process and stabilizer, which is applied in the field of chemical reaction, can solve the problems of complex separation, etc., and achieve the effects of high process safety, improved recycling efficiency, and simple operation

Active Publication Date: 2018-03-20
AFCHINA CORP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low boiling point of these amine compounds, although they can inhibit the decomposition of chloroform, the separation from NMP is more complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Experiments were carried out according to this method, using p-nitrophenol as a stabilizer, adding 2.0% of the stabilizer to the NMP / chloroform solution with a mass fraction of NMP of 80%, and stirring to dissolve the stabilizer. Let NMP / chloroform enter vacuum distillation and separation, the separation process temperature is 120° C., and the vacuum degree is 0.90 atmospheric pressure. When detecting the degree of acidification, the volume ratio of NMP / chloroform sample to deionized water is 1:1. After three hours of stable separation process, the pH of the aqueous phase was found to be stable around 4.8, and the acidification phenomenon was suppressed.

Embodiment 2

[0023] Experiments were carried out according to this method, and 1-naphthol was used as a stabilizer. In an NMP / chloroform solution with a mass fraction of NMP of 10%, a stabilizer with a mass fraction of 10.0% was added and stirred to dissolve the stabilizer. Let the NMP / chloroform enter the vacuum distillation separation, the temperature of the separation process is 150° C., and the vacuum degree is 0. When detecting the degree of acidification, the volume ratio of NMP / chloroform sample to deionized water is 1:5. After three hours of stable separation process, the pH of the aqueous phase was found to be stable around 5.2, and the acidification phenomenon was suppressed.

Embodiment 3

[0025] Experiments were carried out according to this method, using glycerol as a stabilizer, adding a 20.0% stabilizer in a NMP / chloroform solution with a mass fraction of 1%, and stirring to dissolve the stabilizer. Let NMP / chloroform enter vacuum distillation and separation, the separation process temperature is 70° C., and the vacuum degree is 0.95 atmospheric pressure. When detecting the degree of acidification, the volume ratio of NMP / chloroform sample to deionized water is 1:10. After three hours of stable separation process, the pH of the aqueous phase was found to be stable around 7.0, and the acidification phenomenon was suppressed.

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Abstract

The invention discloses a method for inhibiting chloroform acidifying during separation of N-methylpyrolidone (NMP) and chloroform by adding a stabilizing agent, and belongs to the technical field of chemical reaction engineering. According to the method, a high-boiling-point alcohols and phenols stabilizing agent is added into the NMP / chloroform system, and gives play to effect of inhibiting acidifying during separation of NMP / chloroform. The method is capable of effectively inhibiting acidifying phenomenon during separation of NMP / chloroform and improving NMP recovery utilization efficiency, and possesses the advantages of simple operation, low cost, high safety and the like.

Description

technical field [0001] The invention belongs to the technical field of chemical reaction, and particularly relates to a method for inhibiting chloroform acidification in the NMP / chloroform separation process by adding a stabilizer, specifically referring to adding hydroxyl-containing alcohols or phenols. Background technique [0002] N-methylpyrrolidone (NMP) is an important chemical raw material, which is widely used in many fields such as polymerization solvent and extraction agent. However, separating NMP from the mixture and recycling it after purification is a difficult problem often encountered in the use of NMP. Using chloroform to extract and separate NMP from NMP / water mixture is a commonly used separation method in industry. For example, in the production of para-aramid fiber, polyphenylene sulfide fiber and many other products, chloroform extraction is used. Separate NMP. The advantages of using chloroform to extract NMP from water are high production efficiency...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D207/267C07C17/42C07C19/04
CPCC07C17/42C07D207/267C07C19/04
Inventor 庹新林王佩坚许甲崔庆海
Owner AFCHINA CORP CO LTD
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