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Continuous reaction technological method for preparing epsilon-caprolactone, and microchannel reaction equipment

A technology of microchannel reaction and process method, applied in the field of organic synthesis process, to reduce the generation of by-products, improve reaction efficiency, and improve safety

Inactive Publication Date: 2014-01-29
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] So far, there has been no process research and equipment technology report on the synthesis of ε-caprolactone by oxidation of cyclohexanone in a continuous flow reaction mode. Oxy-acid, re-oxidation of cyclohexanone to prepare ε-caprolactone process technology scheme and corresponding equipment technology

Method used

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  • Continuous reaction technological method for preparing epsilon-caprolactone, and microchannel reaction equipment
  • Continuous reaction technological method for preparing epsilon-caprolactone, and microchannel reaction equipment
  • Continuous reaction technological method for preparing epsilon-caprolactone, and microchannel reaction equipment

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Effect test

Embodiment 1

[0031] (1) Device: Microchannel reaction device The microchannel adopts ordinary round pipes ( image 3 -a), the material is PFA, and the channel feature size is 2.0mm. refer to figure 1 Shown technological process of the present invention, set up as figure 2 microchannel reaction device.

[0032] (2) Preparation of peroxyacid: Set the mass flow rate ratio of metering pump A and metering pump B to acetic anhydride: 30% hydrogen peroxide = 1.0:1. After the two materials are fully preheated, the The mixed reaction is carried out in the reaction zone, the reaction temperature is set at 20°C, the residence time of the reaction material is controlled by adjusting the flow rate of the metering pump and the length of the microchannel to be 10s, and the material is collected from the outlet of the microchannel reaction system to obtain The mass fraction is 15.5% peracetic acid.

[0033] (3) Preparation of ε-caprolactone: Adjust the configuration scheme of the preheating zone, rea...

Embodiment 2

[0035] (1) Device: Microchannel reaction device The microchannel adopts a rectangular flat pipe ( image 3 -b), the material is stainless steel, the characteristic dimensions of the channel are a=2.0mm, b=2.0mm (a is the channel flow width, b is the channel flow thickness). refer to figure 1 Shown technological process of the present invention, set up as figure 2 microchannel reaction device.

[0036] (2) Preparation of peroxyacid: Set the mass flow rate ratio of metering pump A and metering pump B to acetic anhydride: 50% hydrogen peroxide = 1.2:1. After the two materials are fully preheated, the The mixed reaction is carried out in the reaction zone, the reaction temperature is set at 40°C, the residence time of the reaction material is controlled by adjusting the flow rate of the pump to be 100s, and the material is collected from the outlet of the microchannel reaction system, which is the process with a mass fraction of 18.7%. Oxyacetic acid.

[0037] (3) Preparation...

Embodiment 3

[0039] (1) Device: Microchannel reaction device The microchannel adopts a pulsed circular pipe microchannel with a built-in throttling orifice ( image 3 -c shown), the material is glass, the channel characteristic dimension Ф 1 =3.0mm, Ф 2 =1.0mm, (Ф 1 is the flow diameter of the main channel of the circular pipe, Ф 2 is the flow diameter of the flow-limiting orifice of the throttle orifice in the circular pipe). refer to figure 1 Shown technological process of the present invention, set up as figure 2 microchannel reaction device.

[0040] (2) Preparation of peroxyacid: Set the mass flow rate ratio of metering pump A and metering pump B to acetic anhydride: 50% hydrogen peroxide = 1.5:1. The mixed reaction is carried out in the reaction zone, the reaction temperature is set at 40°C, the residence time of the reaction material is controlled by adjusting the flow rate of the metering pump and the length of the microchannel to be 180s, and the material is collected from ...

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Abstract

The invention relates to a continuous reaction technological method for preparing epsilon-caprolactone, and microchannel reaction equipment, belonging to the technical field of organic synthesis. The method takes cyclohexanone as initial reaction raw material and peracetic acid generated in the reaction of hydrogen peroxide and acetic anhydride as an oxidizing agent, and the processes such as peroxy acid preparation, cyclohexanone oxidation and the like are continuously completed in a microchannel reactor system. The continuous reaction technological method effectively controls the temperature in the reaction process, is high in safety, does not need an additional solvent, catalyst and stabilizing agent, is beneficial to separation and purification of caprolactone, and enables the high-yield continuous production of the epsilon-caprolactone to be possible; the microchannel reaction equipment provided by the invention highly meets the requirements of the reaction technology. The conversion rate of the cyclohexanone reaches 50-95%, and the selectivity of the epsilon-caprolactone is 80-100%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and specifically relates to a continuous reaction process method for preparing ε-caprolactone by oxidation of cyclohexanone as a raw material, and its corresponding process equipment technology. More specifically, it is a continuous reaction process for preparing ε-caprolactone from hydrogen peroxide and acetic anhydride to synthesize peracetic acid in a microchannel reactor, and then oxidizing cyclohexanone with peracetic acid, and the corresponding equipment technology. [0002] technical background [0003] ε-caprolactone is an important organic synthesis intermediate, widely used as a synthetic monomer for new polyester materials to modify various resins to improve their gloss, transparency and anti-sticking properties. Polycaprolactone and its copolymer obtained by copolymerizing it as a monomer are a kind of fully biodegradable polymer materials with good biocompatib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04B01J19/00
CPCB01J19/0093C07D313/04
Inventor 严生虎韩玲玲张跃沈介发刘建武
Owner CHANGZHOU UNIV
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