Method for preparing epsilon-caprolactone by using carbon nanotube

A carbon nanotube and caprolactone technology, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low efficiency and high cost of benzaldehyde, and achieve high catalytic activity and high industrial value. , the effect of high catalytic activity

Inactive Publication Date: 2018-09-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to develop the carbon material of different doping forms to improve the catalytic activity of carbon material, and solve existing cyclohexanone Baeyer-Villiger oxidation reaction. 2 In the / aldehyde system, the efficiency of the pro-oxidant benzaldehyde is low and the cost is high. Provide a pro-oxidant-acrolein, combined with fluorinated carbon nanotubes as a non-metallic catalyst, to provide a catalyst with high catalytic efficiency, easy recovery of the catalyst, and low cost. The method for the synthesis of ε-caprolactone

Method used

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  • Method for preparing epsilon-caprolactone by using carbon nanotube
  • Method for preparing epsilon-caprolactone by using carbon nanotube
  • Method for preparing epsilon-caprolactone by using carbon nanotube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0033] Add 17mL of 1,2-dichloroethane, 1.3g of o-dichlorobenzene (internal standard), 0.59g of cyclohexanone, 1.35g of acrolein and 50mg of the catalyst shown in Table 2 into the autoclave and stir Heat to 80°C, feed oxygen, start timing, and maintain its pressure at 1MPa during the reaction, stop timing after reacting for 4 hours, cool the reactor to room temperature, filter the liquid-solid phase mixture, and obtain a solid catalyst and containing unreacted A liquid mixture of reactants and reaction products. The liquid phase mixture is detected and analyzed with a gas chromatograph (GC) (see figure 1 ). The GC detection results are shown in Table 2 (the influence of different carbon materials on the Baeyer-Villiger oxidation reaction of cyclohexanone).

[0034] The sulfur-doped carbon nanotubes, phosphorus-doped carbon nanotubes, and nitrogen-doped carbon nanotubes used in this example are all self-made and made by chemical vapor deposition. The specific preparation metho...

Embodiment 4～7

[0043] Add 17mL of the solvent shown in Table 3, 1.3g o-dichlorobenzene (internal standard), 0.59g cyclohexanone, 1.35g acrolein and 50mg fluorinated carbon nanotubes (F content is 53.78at%) to Stir and heat the autoclave to 80°C, feed oxygen, start timing, and maintain the pressure at 1 MPa during the reaction, stop timing after reacting for 4 hours, cool the autoclave to room temperature, filter the liquid-solid phase mixture to obtain a solid Catalyst and liquid phase mixture containing unreacted reactants and reaction products. The liquid phase mixture was detected and analyzed by gas chromatography (GC). The GC detection results are shown in Table 3 (the influence of different solvents on the Baeyer-Villiger oxidation reaction of cyclohexanone).

[0044] table 3

[0045] Example

[0046] It can be seen from Table 3 that when 1,2-dichloroethane is used as the solvent, the selectivity of ε-caprolactone and acrylic acid and the efficiency of acrolein are the best...

Embodiment 8～11

[0048] Add 17mL 1,2-dichloroethane, 1.3g o-dichlorobenzene (internal standard), 0.59g cyclohexanone, 1.35g acrolein and 50mg fluorinated carbon nanotubes (F content is 53.78at%) Stir and heat to the high-pressure reactor to the temperature shown in Table 4, feed oxygen, start timing, and maintain the pressure at 1MPa during the reaction. After reacting for 4 hours, stop timing, cool the reactor to room temperature, and filter the liquid-solid phase mixture to obtain a solid catalyst and a liquid phase mixture containing unreacted reactants and reaction products. The liquid phase mixture was detected and analyzed by gas chromatography (GC). The gas chromatogram of the reaction solution after the reaction of embodiment 1 is as follows figure 1 shown. The GC detection results are shown in Table 4 (the influence of reaction temperature on the Baeyer-Villiger oxidation reaction of cyclohexanone).

[0049] Table 4

[0050] Example

[0051] As can be seen from Table 4, ...

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Abstract

The invention discloses a method for preparing epsilon-caprolactone by using a carbon nanotube. In the method, cyclohexanone, a pro-oxidant and a certain amount of catalyst are added into a certain amount of organic solvent, the molecular oxygen is taken as the oxidizing agent, the pro-oxidant is acrolein, the catalyst is a carbon material, and the mixture is stirred and reacted for 0.1-24 hours at the pressure of 0.1-2 MPa at the temperature of 50-90 DEG C. The method has the advantages that the efficiency of the pro-oxidant is high, the selectivity of the epsilon-caprolactone and crylic acidis high, the catalyst is easy to recycle, the oxidizing agent is green and environmentally friendly, the operation is simple, and the cost is low.

Description

technical field [0001] The invention relates to the field of preparation of ε-caprolactone, in particular to a method for preparing ε-caprolactone by utilizing carbon nanotubes. Background technique [0002] ε-caprolactone is an important organic synthesis intermediate and a new type of polyester monomer. It is mainly used for the synthesis of polyε-caprolactone and its copolymerization or blending modification with other esters to improve its gloss and transparency. sex and anti-adhesive etc. The linear aliphatic polyester obtained by ring-opening polymerization of ε-caprolactone is polycaprolactone (PCL). PCL has good thermoplasticity, molding processability and environmental protection. With the enhancement of people's awareness of environmental protection, it is also expected to replace the existing ordinary plastics and enter the market of disposable packaging materials and mulch films in large quantities. Based on its many advantages and broad application prospects, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04B01J27/22B01J27/08C07C51/235C07C57/04
CPCB01J27/08B01J27/22C07C51/235C07D313/04C07C57/04Y02P20/584
Inventor 余皓杨利情曹永海王红娟彭峰
Owner SOUTH CHINA UNIV OF TECH
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