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Method for continuous production of 3-methyl-3-penten-2-one in micro-channel reactor

A micro-channel reactor and micro-channel technology are applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., which can solve problems such as corrosion equipment, serious environmental pollution, and high requirements for production equipment, and achieve the goal of avoiding waste water, The effect of reducing waste and reducing energy consumption

Active Publication Date: 2020-02-14
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The disclosed methods of the above patents all adopt strong acid or strong base as catalyst, and the production process will produce a large amount of waste water, which seriously pollutes the environment.
Moreover, the relevant catalysts will corrode the equipment, which requires higher production equipment

Method used

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  • Method for continuous production of 3-methyl-3-penten-2-one in micro-channel reactor
  • Method for continuous production of 3-methyl-3-penten-2-one in micro-channel reactor
  • Method for continuous production of 3-methyl-3-penten-2-one in micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Catalyst [Ps-mim]HSO 4 Mix evenly with 5% of the quality of the raw material 2-butanone, adjust the metering pumps respectively, control the molar ratio of 2-butanone and acetaldehyde to be 5:1, and the external heat exchanger controls the preheating module temperature, the temperature of the preheating module is 60°C, and the preheating time is 0.5h. After the preheating is completed, the two raw materials are synchronously passed into the integrated microchannel mixer and mixed evenly. The reaction temperature in the microchannel reactor with an inner diameter of 3 mm is 60 ° C, and the reaction residence time is 15 minutes. The conversion rate of acetaldehyde and the yield of product were analyzed.

[0037]In this example, the conversion rate of acetaldehyde was 97.5%, the yield of 3-methyl-3-penten-2-one was 82.3%, and the purity was 98.8%.

Embodiment 2

[0042] Catalyst [Ps-mim]HSO 4 Mix evenly with 5% of the quality of the raw material 2-butanone, adjust the metering pumps respectively, control the molar ratio of 2-butanone and acetaldehyde to be 10:1, and the external heat exchanger controls the preheating module temperature, the temperature of the preheating module is 65°C, and the preheating time is 0.5h. After the preheating is completed, the two raw materials are synchronously passed into the integrated microchannel mixer and mixed evenly. The reaction temperature in the microchannel reactor with an inner diameter of 1 mm is 65 ° C, and the reaction residence time is 10 minutes. The conversion rate of acetaldehyde and the yield of product were analyzed.

[0043] In this example, the conversion rate of acetaldehyde was 99.2%, the yield of 3-methyl-3-penten-2-one was 85.4%, and the purity was 99.1%.

Embodiment 3

[0048] Catalyst [Ps-mim]HSO 4 Mix evenly with 3% of the mass of the raw material 2-butanone, adjust the metering pumps respectively, control the molar ratio of 2-butanone and acetaldehyde to be 15:1, and the external heat exchanger controls the preheating module temperature, the temperature of the preheating module is 60°C, and the preheating time is 0.5h. After the preheating is completed, the two raw materials are synchronously passed into the integrated microchannel mixer and mixed evenly. The reaction temperature in the microchannel reactor with an inner diameter of 1 mm is 60 ° C, and the reaction residence time is 8 minutes. The conversion rate of acetaldehyde and the yield of product were analyzed.

[0049] In this example, the conversion rate of acetaldehyde was 99.4%, the yield of 3-methyl-3-penten-2-one was 86.6%, and the purity was 99.4%.

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Abstract

The invention discloses a method for continuous production of 3-methyl-3-penten-2-one in a micro-channel reactor and belongs to the technical field of organic synthesis processes. The method comprisesthe following specific steps: mixing 2-butanone with an ionic liquid [Ps-min]HSO4; simultaneously pumping a raw material acetaldehyde and a mixed solution of 2-butanone and a catalyst into a preheating module through metering pumps respectively, and introducing the components into an integral micro-channel mixer; performing uniform mixing, further introducing the components into a micro-channel reactor, and performing a reaction; and introducing the components into a cooling module, performing sample, and performing separation so as to obtain 3-methyl-3-penten-2-one. By adopting the method, aproduct can be efficiently and rapidly synthesized; the ionic liquid [Ps-min]HSO4 replaces a conventional inorganic acid to be used as a catalyst of the reaction, the reaction condition is mild, andthe product yield is high; meanwhile, the catalyst is easily separated from reaction products, the acid-base neutralization process of a conventional process is avoided, production of wastewater can be reduced, and the environment can be protected.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a method for continuously producing 3-methyl-3-penten-2-one with a microchannel reactor. Background technique [0002] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a method for continuously producing 3-methyl-3-penten-2-one through reactive distillation. 3-Methyl-3-penten-2-one is an important raw material for the synthesis of spice ambroxone in industry. In view of the limited sources of natural ambergris, and the demand for it in the perfume market is increasing, it is urgent to develop synthetic fragrances with ambergris aroma to meet the market demand, and ambergris is one of the more successful ones. At present, there are three main steps in the industrial synthesis of ambroxone: (1) catalyzed synthesis of 3-methyl-3-penten-2-one by acetaldehyde and 2-butanone; (2) 3-methyl-3-pent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C49/203B01J31/02
CPCC07C45/74B01J31/0284B01J31/0285C07C49/203
Inventor 李玲洪鹏王晓达葛雪惠王清莲邱挺叶长燊郑丹丹黄智贤
Owner FUZHOU UNIV
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