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Method for preparing caprolactone through cyclohexanone catalyzed oxidation

A technology for catalytic oxidation and cyclohexanone, which is applied in the fields of chemical synthesis and technology, can solve the problems that caprolactone cannot accurately control the reaction temperature, cannot be continuously produced, and has low epoxidation speed, and achieves easy operation and control of the preparation process, The effect of short reaction residence time and improved conversion rate

Inactive Publication Date: 2015-02-25
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The technical problem to be solved by the present invention is to propose a method for preparing caprolactone by oxidation of cyclohexanone that cannot accurately control the reaction temperature, has low selectivity, low safety, low epoxidation speed, many by-products, and cannot be continuously produced. Method for preparing ε-caprolactone by catalytic oxidation of cyclohexanone

Method used

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  • Method for preparing caprolactone through cyclohexanone catalyzed oxidation

Examples

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Effect test

Embodiment 1

[0034] The hydrogen peroxide of 30wt% and 98wt% acetic acid are mixed according to hydrogen peroxide: and the mol ratio of acetic acid is 1:1, adds catalyst concentrated H to wherein 2 SO 4 And stabilizer EDTA, the addition amount of catalyst is 6.31% of hydrogen peroxide quality, and the addition quality of stabilizer is 12.23% of hydrogen peroxide quality. The flow rate of cyclohexanone and the above mixture is controlled at 2.0ml / min and 4.6ml / min respectively, so that the molar ratio of acetic acid and cyclohexanone is 2.3:1, through the microchannel modular reaction device, the micro The reaction was carried out in a structural reactor, and the reaction retention time was 5.6 min. A length of polytetrafluorocapillary is connected to the back of the microchannel modular reaction device, and the polytetrafluorocapillary is immersed in an ice-water bath to terminate the reaction. The reactant is introduced into the separator, and 7wt% Na is added 2 CO 3 The aqueous solut...

Embodiment 2

[0036] 30wt% hydrogen peroxide and 98wt% acetic acid are mixed according to the molar ratio of hydrogen peroxide and acetic acid as 1:1, and catalyst concentrated H 3 PO 4 And stabilizer EDTA, the addition amount of catalyst is 4.32% of hydrogen peroxide quality, and the addition quality of stabilizer is 9.68% of hydrogen peroxide quality. The flow rate of cyclohexanone and the above mixture is controlled at 2.2ml / min and 4.4ml / min respectively, so that the molar ratio of acetic acid and cyclohexanone is 1.6:1, through the microchannel modular reaction device, the micro The reaction was carried out in a structural reactor, and the reaction retention time was 5.6 min. A length of polytetrafluorocapillary is connected to the back of the microchannel modular reaction device, and the polytetrafluorocapillary is immersed in an ice-water bath to terminate the reaction. The reactant is introduced into the separator, and 7wt% Na is added 2 CO 3 The aqueous solution was washed to a...

Embodiment 3

[0038] 30wt% hydrogen peroxide and 98wt% formic acid are mixed according to the molar ratio of hydrogen peroxide and formic acid as 1:1, and catalyst concentrated H 2 SO 4 And stabilizer EDTA, the addition amount of catalyst is 6.32% of hydrogen peroxide quality, and the addition quality of stabilizer is 12.23% of hydrogen peroxide quality. The flow rate of cyclohexanone and the above mixture is controlled at 2.0ml / min and 4.6ml / min respectively, so that the molar ratio of acetic acid and cyclohexanone is 2.3:1, through the microchannel modular reaction device, the micro The reaction was carried out in a structural reactor, and the reaction retention time was 5.6 min. A length of polytetrafluorocapillary is connected to the back of the microchannel modular reaction device, and the polytetrafluorocapillary is immersed in an ice-water bath to terminate the reaction. The reactant is introduced into the separator, and 7wt% Na is added 2 CO 3 The aqueous solution was washed to ...

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Abstract

The invention discloses a method for preparing caprolactone through cyclohexanone catalyzed oxidation. The method comprises the following steps: mixing aqueous solution of hydrogen peroxide and aqueous solution of formic acid, and adding a catalyst and a stabilizer, thereby preparing a mixed solution; respectively pumping cyclohexanone and the mixed solution into a micro-channel modular reaction device, reacting at the temperature of 45-100 DEG C, preserving the reaction retention time for 2-10 minutes, guiding the reaction products into a separation device, adding aqueous solution of Na2CO3 for washing and regulating the pH value to be neutral, extracting the aqueous solution by using ethyl acetate, merging obtained organic extracting solution, and performing spin evaporation to remove the solvent, thereby obtaining the target product caprolactone. The method disclosed by the invention refers to a continuous process, the preparation process is easy to operate and control, the safety is high, the reaction conditions are mild, the reaction time consumption is short, the product quality is stable, and after-treatment is simple. The method has the characteristics that the generation device is simple, easy in detachment and convenient to carry and move. Convenient adjustment can be performed by simply increasing or decreasing the number of the micro channels.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and technology, in particular to a method for preparing caprolactone by catalytic oxidation of cyclohexanone in a microchannel reactor. Background technique [0002] ε-caprolactone (ε-CL) is an important organic synthesis intermediate, which was successfully synthesized in the laboratory as early as the 1930s, but its industrialization was developed for the production of ε-caprolactam after World War II . Although the process of preparing ε-caprolactam by ε-CL ammonolysis has already been replaced by the Beckmann rearrangement method of cyclohexanone oxime, ε-CL still has important value in industry. [0003] As a new type of polyester monomer widely used, ε-caprolactone is mainly used to synthesize polycaprolactone (PCL) for different purposes. PCL has unique biocompatibility, biodegradability and good permeability. The material field has a wide range of applications. For example, P...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04
CPCC07D313/04
Inventor 郭凯方正陈克涛何伟欧阳平凯
Owner NANJING UNIV OF TECH
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