Method for continuously producing 3-methyl-3-pentene-2-one by reactive distillation

A technology of reactive distillation and reactive distillation column, applied in the field of chemical synthesis, can solve the problems of low utilization rate of raw materials, large amount of waste water, difficult recovery of catalysts, etc., achieve high conversion rate and selectivity, reduce waste water treatment, improve The effect of conversion and selectivity

Active Publication Date: 2019-06-11
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the fact that inorganic acid is easy to corrode equipment, and the production process produces a large amount of waste water, this process has been phased out
Chinese patent CN106045834A uses liquid alkali as catalyst, which has problems such as difficult recovery of catalyst and further treatment of alkali liquor
The process catalyst using solid acid can be recycled and does not produce waste water, which is a more green and environmentally friendly route, but the low utilization rate of raw materials still restricts the application of this process

Method used

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  • Method for continuously producing 3-methyl-3-pentene-2-one by reactive distillation
  • Method for continuously producing 3-methyl-3-pentene-2-one by reactive distillation
  • Method for continuously producing 3-methyl-3-pentene-2-one by reactive distillation

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A Novel Microspherical Polymer Ionic Liquid P(VB-VS)HSO Filled in the Reaction Section of a Reactive Distillation Column 4 , the packing height is 3m, the feed molar ratio of 2-butanone and acetaldehyde is controlled to be 6:1, nitrogen is filled to make the operating pressure of the rectification tower reach 0.2MPa, and the temperature of the reaction section of the reaction rectification tower is 75°C. The tower adopts total reflux; the reflux ratio of the vacuum distillation tower I is 3, and the operating pressure is 50kPa; the operating pressure of the vacuum distillation tower II tower is 10kPa, and the reflux ratio is 2; the extractive distillation tower operating pressure is normal pressure, and the reflux ratio is 1.2; The operating pressure in the extraction agent recovery tower is normal pressure, the reflux ratio is 2.2, and the extraction agent is benzene.

[0035] In this example, the conversion rate of acetaldehyde was 99.31%, the yield of 3-methyl-3-pent...

Embodiment 2

[0040] A Novel Microspherical Polymer Ionic Liquid P(VB-VS)HSO Filled in the Reaction Section of a Reactive Distillation Column 4 , the packing height is 3m, the feed molar ratio of 2-butanone and acetaldehyde is controlled to be 8:1, nitrogen is filled to make the operating pressure of the rectification tower reach 0.2MPa, and the temperature of the reaction section of the reaction rectification tower is 75°C. The tower adopts total reflux; the reflux ratio of vacuum distillation column I is 6, and the operating pressure is 60kPa; the operating pressure of vacuum distillation column II tower is 10kPa, and the reflux ratio is 2; the extractive distillation column operating pressure is normal pressure, and the reflux ratio is 1.2; The operating pressure in the extraction agent recovery tower is normal pressure, the reflux ratio is 2.2, and the extraction agent is dimethyl sulfoxide.

[0041] In this example, the conversion rate of acetaldehyde was 99.65%, the yield of 3-methyl-...

Embodiment 3

[0046] A Novel Microspherical Polymer Ionic Liquid P(VB-VS)HSO Filled in the Reaction Section of a Reactive Distillation Column 4 , the packing height is 4m, the feed molar ratio of 2-butanone and acetaldehyde is controlled to be 10:1, nitrogen is filled to make the operating pressure of the rectification tower reach 0.2MPa, and the temperature of the reaction section of the reaction rectification tower is 75°C. The tower adopts full reflux; the reflux ratio of the vacuum distillation column I is 8, and the operating pressure is 65kPa; the operating pressure of the vacuum distillation column II tower is 10kPa, and the reflux ratio is 2; the extractive distillation column operating pressure is normal pressure, and the reflux ratio is 1.2; The operating pressure in the extraction agent recovery tower is normal pressure, the reflux ratio is 2.2, and the extraction agent is chloroform.

[0047] In this example, the conversion rate of acetaldehyde was 99.87%, the yield of 3-methyl-...

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Abstract

The invention discloses a method for continuously producing 3-methyl-3-pentene-2-one by reactive distillation. 2-butanone and acetaldehyde are used as raw materials, a novel microspherical polymer ionic liquid P(VB-VS)HSO4 is adopted as a catalyst, acetaldehyde and 2-butanone are subjected to an aldol condensation reaction in a reactive distillation column to generate 3-methyl-3-pentene-2-one, andthen, a reaction solution is delivered into a reduced-pressure distillation column and is subjected to reactant and product separation to obtain high-purity 3-methyl-3-pentene-2-one. According to themethod, the novel microspherical polymer ionic liquid is used as a reaction catalyst instead of traditional strong acid / alkali, so that the reaction condition is mild, the conversion rate and selectivity of acetaldehyde are high, side reactions are reduced, meanwhile, an acid-base neutralization process in a traditional process is further omitted, the energy loss and wastewater treatment are greatly reduced, and the method is capable of saving energy and environment-friendly; and the superfluous 2-butanone can be further used as a reaction raw material after being separated, so that the resource loss is reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a method for continuously producing 3-methyl-3-penten-2-one through reactive distillation. Background technique [0002] 3-Methyl-3-penten-2-one is mainly used as an intermediate in the synthesis of ambroxone in industry. At present, the synthesis of ambroxone in industry mainly includes three steps: (1) catalytic synthesis of 3-methyl-3-penten-2-one by acetaldehyde and 2-butanone; (2) 3-methyl-3- Addition reaction between penten-2-one and myrcene to obtain isopril-salmonklamentone; (3) cyclization reaction of isopril-salmonklamentone to obtain ambroxone. Among them, the production of 3-methyl-3-penten-2-one in step (1) is an important step in the synthesis of ambroxone. [0003] The early production of 3-methyl-3-penten-2-one was carried out in a tank reactor with inorganic acid as a catalyst. However, due to the corrosion of equipment by inorganic acids and the la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C49/203C07C45/78B01J31/02B01J31/06B01J35/08
CPCY02P20/10
Inventor 邱挺李玲张洪鹏王晓达叶长燊黄智贤杨臣陈锦溢郑丹丹尤新强林小城葛雪惠王清莲
Owner FUZHOU UNIV
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