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N-vinyl pyrrolidone purification system and method

A vinylpyrrolidone and purification method technology, applied in the field of N-vinylpyrrolidone preparation, can solve the problems of many reaction steps, environmental pollution, low production efficiency, etc., reduce the chance of self-polymerization of materials, reduce production costs, The effect of improving utilization efficiency

Pending Publication Date: 2021-10-08
乌兰察布市珂玛新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When adopting the acetylene synthesis method (Reppe method) to synthesize NVP, most of them use a strong base such as KOH as a catalyst to catalyze the vinylation reaction of a-pyrrolidone and acetylene. The defects of this method are very obvious, and there are many reaction steps. The five-step reaction of hydrogenation, catalytic dehydrogenation to form a ring, ammonolysis, and alkyne addition to obtain the monomer, the amount of non-volatile polymerization by-products generated during the synthesis reaction of the monomer is relatively large, so the post-treatment of the product is cumbersome, not only It leads to a decrease in the yield of the target product NVP, and complicates the separation and purification of NVP
[0003] At present, the separation and purification of NVP adopts semi-continuous separation. In the last step, batch distillation is required to produce NVP products with qualified purity. The residence time of this step is about 24-30 hours. Since N-vinylpyrrolidone is a heat-sensitive substance, the material is in the rectification The residence time in the tower is as high as 30-40 hours. Due to the high temperature in the rectification process, a large amount of N-vinylpyrrolidone is self-polymerized, thereby reducing the yield of the target product NVP. Not only the production efficiency of the enterprise is not high, but also The production cost of enterprises has risen. In addition, the by-products of self-polymerization have also brought certain environmental pollution problems.

Method used

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  • N-vinyl pyrrolidone purification system and method
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  • N-vinyl pyrrolidone purification system and method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment approach 1

[0107] figure 1 It is a schematic diagram of the NVP refining system and process flow according to Embodiment 1 of the present invention.

[0108] Such as figure 1 As shown, a kind of N-vinylpyrrolidone refining system comprises: the first rectifying unit 1, the first crystallization system 8 and the third rectifying unit 7 connected in series through the pipeline, the second rectifying unit 2 and the second rectifying unit connected in series The second crystallization system 9, and the NVP storage tank. Wherein, the first rectification unit 1 receives the synthetic reaction solution 00 containing NVP, carries out rectification treatment and outputs the first distillate 11 and the first still out 12, and the first crystallization system 8 receives the first distillate 11, carries out crystallization purification and outputs The first crystallization solution 81 and the first mother liquor 82, the third rectification unit 7 receives the first crystallization solution 81 and ...

Embodiment approach 2

[0117] figure 2 Schematic diagram of the NVP purification system and process flow according to Embodiment 2. The synthetic reaction solution 00 of NVP is prepared by the acetylene synthesis method. After gas-liquid separation, the synthetic reaction solution 00 comprises 30-55% (wt%) of NVP, 45-70% (wt%) of a-p, and 00 of the synthetic reaction solution. 960 liters / hour enters the first rectification unit 1 to carry out primary NVP purification (ie primary rectification purification). It is different from Embodiment 1 mainly in the following aspects:

[0118] Such as figure 2 As shown, the second rectification unit 2 of the NVP refining system includes two packed columns connected in sequence, that is, the fourth rectification tower 4 and the fifth rectification tower 5, and the fourth rectification tower 4 receives the first rectification unit 1 The first still goes out 12, carries out distillation purification, and outputs the 4th still and goes out 41 and the 4th still g...

Embodiment approach 3

[0122] image 3 Schematic diagram of the NVP purification system and process flow according to Embodiment 3. The synthetic reaction solution 00 of NVP is prepared by the acetylene synthesis method. After gas-liquid separation, the synthetic reaction solution 00 comprises 30-55% (wt%) of NVP, 45-70% (wt%) of a-p, and 00 of the synthetic reaction solution. 960 liters / hour enters the first rectification unit 1 to carry out primary NVP purification (ie primary rectification purification). It is different from Embodiment 2 mainly in the following aspects:

[0123] Such as image 3 As shown, the second rectification unit 2 of the NVP refining system also includes a third rectification tower 3, the third rectification tower 3 is arranged on the front end of the fourth rectification tower 4 and connected in series with it, and the third rectification tower 3 receives from The first still of the first rectification unit 1 goes out 12 and outputs the third still and goes out 31 and t...

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Abstract

The invention relates to an N-vinyl pyrrolidone purification system and method. The N-vinyl pyrrolidone purification system comprises a first rectification unit, a first crystallization system and a third rectification unit which are sequentially connected in series through pipelines, a second rectification unit and a second crystallization system which are connected in series,and an NVP storage tank, wherein the first rectification unit receives a synthesis reaction liquid containing NVP, carries out rectification treatment and outputs a first distillate and a first kettle distillate, the first crystallization system receives the first distillate, carries out crystallization purification and outputs a first crystallization liquid, the third rectification unit receives the first crystallization liquid, carries out rectification treatment and outputs a seventh distillate, the second rectification unit carries out rectification treatment on the first kettle distillate and then outputs a second distillate, the second kettle distillatereturns to the first rectification unit for rectification treatment, the second crystallization system crystallizes the second distillate to obtain a second crystallization liquid, and the NVP storage tank receives the seventh distillate and the second crystalline liquid. According to the invention, cascade rectification and gradient crystallization are coupled, NVP can be continuously refined, and the yield of NVP can be improved.

Description

technical field [0001] The invention belongs to the technical field of N-vinylpyrrolidone preparation, and in particular relates to an N-vinylpyrrolidone purification system and method. Background technique [0002] N-methylpyrrolidone (NVP) is a kind of fine chemicals with excellent performance, which puts forward high requirements on the purity of NVP. When adopting the acetylene synthesis method (Reppe method) to synthesize NVP, most of them use a strong base such as KOH as a catalyst to catalyze the vinylation reaction of a-pyrrolidone and acetylene. The defects of this method are very obvious, and there are many reaction steps. The five-step reaction of hydrogenation, catalytic dehydrogenation to form a ring, ammonolysis, and alkyne addition to obtain the monomer, the amount of non-volatile polymerization by-products generated during the synthesis reaction of the monomer is relatively large, so the post-treatment of the product is cumbersome, not only Cause target prod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D3/14B01D9/02C07D207/267
CPCB01D3/143B01D9/004B01D9/0059C07D207/267
Inventor 赵虎胜刘海涛李凯宇郭中山王冬焦艳东祁宝英
Owner 乌兰察布市珂玛新材料有限公司
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