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A method for reactive distillation to continuously produce 3-methyl-3-penten-2-one

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

Active Publication Date: 2021-07-27
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A method for reactive distillation to continuously produce 3-methyl-3-penten-2-one
  • A method for reactive distillation to continuously produce 3-methyl-3-penten-2-one
  • A method for reactive distillation to continuously produce 3-methyl-3-penten-2-one

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Experimental program
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Effect test

Embodiment 1

[0034] Reactive distillation tower reaction section filled new microspheallopolymer ionic liquid P (VB-VS) HSO 4 The filler height is 3 m, the feed molar ratio of 2-butanone and acetaldehyde is 6: 1, which is filled with nitrogen to operate the rectification tower to operate the pressure of 0.2 MPa, and the temperature of the reaction rectification column is 75 ° C, The tower is fully refluxed; the reduced pressure rectification tower I reflow ratio is 3, the operating pressure is 50 kPa; the pressure is 10 kPa in the decompression rectification column, the reflow ratio is 2; the extraction rectification column is operated at normal pressure, the reflow ratio is 1.2; Extractant recovery tower operating pressure atmospheric, reflow ratio of 2.2, and extractant is benzene.

[0035] In the present embodiment, the conversion of acetaldehyde is 99.31%, and the yield of 3-methyl-3-pentene-2-ketone is 90.23%, and the purity is 98.82%.

Embodiment 2

[0040] Reactive distillation tower reaction section filled new microspheallopolymer ionic liquid P (VB-VS) HSO 4 The filling height is 3 m, and the feed molar ratio of 2-butanone and acetaldehyde is 8: 1, and the rectification tower is filled with a rectification column to reach 0.2 MPa, and the temperature of the reaction rectification column is 75 ° C, The tower is fully refluxed; the reduced pressure rectification tower I reflow ratio is 6, the operating pressure is 60 kPa; the pressure-reducing rectification column II tower operates 10 kPa, the reflow ratio is 2; the extraction rectification tower is operated at normal pressure, reflow ratio is 1.2; Extractant recovered in the tower operation pressure, reflow ratio of 2.2, and the extractant is dimethyl sulfoxide.

[0041] In the present embodiment, the conversion rate of acetaldehyde is 99.65%, and the yield of 3-methyl-3-pentene-2-ketone is 92.35%, and the purity is 99.32%.

Embodiment 3

[0046] Reactive distillation tower reaction section filled new microspheallopolymer ionic liquid P (VB-VS) HSO 4 The filling height is 4m, the feed molar ratio of 2-butanone and acetaldehyde is 10: 1, which is filled with nitrogen to operate the rectification tower to operate the pressure of 0.2 MPa, and the temperature of the reaction distillation column is 75 ° C, all The tower is fully refluxed; the reduced pressure rectification tower I reflow ratio is 8, the operating pressure is 65kPa; the pressure-reducing rectification column II tower operates 10 kPa, the reflow ratio is 2; the extraction rectification column is operated at pressure, the reflow ratio is 1.2; Extractant recovered in the tower operating pressure, reflow ratio of 2.2, and the extractant is chloroform.

[0047] In the present embodiment, the conversion of acetaldehyde is 99.87%, and the yield of 3-methyl-3-pentene-2-ketone is 93.52%, and the purity is 99.63%.

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Abstract

The invention discloses a method for the continuous production of 3-methyl-3-pentene-2-ketone by reactive distillation. The raw materials are 2-butanone and acetaldehyde, and a novel microspherical polymer ionic liquid P(VB-VS ) HSO 4 As a catalyst, acetaldehyde and 2-butanone undergo an aldol condensation reaction in the reactive distillation tower to generate 3-methyl-3-penten-2-ketone, and then the reaction solution is sent to the vacuum tower for rectification The reactants and products are separated to obtain high-purity 3-methyl-3-penten-2-one. The invention adopts new microspherical polymer ionic liquid instead of the traditional strong acid and strong base as the reaction catalyst, the reaction conditions are mild, the conversion rate and selectivity of acetaldehyde are high, and the acid in the traditional process is also omitted while reducing side reactions. The alkali neutralization process greatly reduces energy loss and waste water treatment, is energy-saving and environmentally friendly, and the excess 2-butanone can continue to be used as a reaction raw material after separation, reducing resource loss.

Description

Technical field [0001] The present invention belongs to the art of chemical synthesis, and more particularly to a reactionary rectification process for continuously producing 3-methyl-3-pentene-2-ketone. Background technique [0002] 3-methyl-3-pentene-2-ketone is mainly used in an intermediate of synthesis of gapson. At present, the synthesis of industrial condensate is mainly three steps: (1) acetaldehyde and 2-butanone catalytic synthesis 3-methyl-3-pentene-2-ketone; (2) 3-methyl-3- Pueentene-2-ketone is reacted with a laurel addition to obtain isopengenulak ketone; (3) isoparaminated to obtain a rollingone. Among them, production of (1) 3-methyl-3-pentene-2-ketone is an important step in gulflanone synthesis. [0003] The production of early 3-methyl-3-pentene-2-ketone is carbonic acid as a catalyst, and is carried out in the kettle reactor. However, due to the easy corrosive equipment of the inorganic acid, and the production process produces a large amount of wastewater, th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/74C07C49/203C07C45/78B01J31/02B01J31/06B01J35/08
CPCY02P20/10
Inventor 邱挺李玲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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