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Oxygen vacancy containing phenol hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and phenol technology, applied in the field of catalysis, can solve problems such as complex preparation process and metal electronic structure not widely used

Active Publication Date: 2019-05-21
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the complicated preparation process, the method of using alloys to control the electronic structure of metals has not been widely used.

Method used

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  • Oxygen vacancy containing phenol hydrogenation catalyst and preparation method thereof
  • Oxygen vacancy containing phenol hydrogenation catalyst and preparation method thereof
  • Oxygen vacancy containing phenol hydrogenation catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Preparation of ZIF-67

[0034] First prepare 50 mL of 0.8 mol / L methanol solution of 2-methylimidazole and 50 mL of 0.1 mol / L methanol solution of cobalt nitrate hexahydrate. Prepare 50 mL of 20 g / L polyvinylpyrrolidone methanol solution, stir for 10 min, put 2-methylimidazole solution in, continue stirring for 10 min, add Co(NO 3 ) 2 ·6H 2 O methanol solution, mixed and stirred for 10 h, then stopped stirring, and left the mixture at room temperature for 1 h. After standing, the product was separated by centrifugation, washed 3 times with methanol, and finally washed at 80 o C dried in an oven for 8 h, and the sample was designated as ZIF-67.

[0035] (2) Preparation of CN materials

[0036]Take 1 g of prepared ZIF-67 in a tube furnace, the calcination atmosphere is argon, and the calcination temperature is 600 o C, the roasting time is 5 h. The temperature is raised from room temperature to the target temperature at a rate of 1 o C / min. The calcined sampl...

Embodiment 2

[0044] (1) Preparation of ZIF-67

[0045] First, prepare 100 mL of 1.2 mol / L methanol solution of 2-methylimidazole and 100 mL of 0.03 mol / L methanol solution of cobalt nitrate hexahydrate. Prepare 100 mL of 5 g / L polyvinylpyrrolidone methanol solution, put 2-methylimidazole solution into it while stirring, continue stirring for 30 min, add Co(NO 3 ) 2 ·6H 2 O methanol solution, mixed and stirred for 5 h, then stopped stirring, and left the mixture at room temperature for 5 h. After standing, the product was separated by centrifugation, washed 5 times with ethanol, and finally washed at 100 o C dried in an oven for 6 h, and the sample was designated as ZIF-67.

[0046] (2) Preparation of CN carrier

[0047] Get 1 g of prepared ZIF-67 in a tube furnace, the calcination atmosphere is argon, and the calcination temperature is 550 o C, the roasting time is 7 h. The temperature is raised from room temperature to the target temperature at a rate of 1 o C / min. The calcined s...

Embodiment 3

[0054] (1) Preparation of ZIF-67

[0055] First prepare 50 mL of 0.3 mol / L methanol solution of 2-methylimidazole and 50 mL of 0.15 mol / L methanol solution of cobalt nitrate hexahydrate. Prepare 50 mL of 30 g / L polyvinylpyrrolidone methanol solution, put 2-methylimidazole solution into it while stirring, continue stirring for 15 min, add Co(NO 3 ) 2 ·6H 2 O methanol solution, mixed and stirred for 15 h, then stopped stirring, and after standing for 3 h, the product was separated by centrifugation without washing, and finally at 60 o C dried in an oven for 24 h, and the sample was designated as ZIF-67.

[0056] (2) Preparation of CN carrier

[0057] Take 1 g of prepared ZIF-67 in a tube furnace, the roasting atmosphere is nitrogen, and the roasting temperature is 800 o C, the roasting time is 3 h. The temperature is raised from room temperature to the target temperature at a rate of 5 o C / min. The calcined samples were denoted as Co / CN. The prepared Co / CN samples were ...

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Abstract

The invention relates to an oxygen vacancy containing phenol hydrogenation catalyst and a preparation method thereof, and belongs to the technical field of catalysis. According to the catalyst, ZIF-67is adopted as a precursor, a N-doped carbon material (CN) is prepared from ZIF-67 through a high-temperature roasting and acid pickling method, then oxygen vacancy containing titanium dioxide nano islands are introduced through a sol-gel method and subsequent high-temperature roasting, and finally the catalyst is prepared through activated component salt stirring and dipping and H2 reduction. Theoxygen vacancy containing phenol hydrogenation catalyst and the preparation method thereof have the advantages that by mean of the CN material derived from anatase type TiO2 nano island modified ZIF-67, the interaction between a carrier and active components can be effectively enhanced, the number of the surface active component is increased, the electron-rich character is improved, the antioxygenic property of the active components is enhanced, the catalytic performance of cyclohexanone prepared through phenol hydrogenation is remarkably enhanced, the prepared catalyst has good catalytic stability.

Description

technical field [0001] The invention relates to an oxygen-vacancy phenol hydrogenation catalyst and a preparation method thereof, belonging to the technical field of catalysis. Background technique [0002] Cyclohexanone is an important chemical raw material for the production of nylon 6 and nylon 66. At present, the main industrial preparation route is cyclohexane oxidation. However, the reaction conditions of high temperature and high pressure and the characteristics of many by-products deviate from the concept of green chemistry. In recent years, the process of direct hydrogenation of phenol to cyclohexanone with low energy consumption and environmental protection has attracted more and more attention. Researchers have developed a series of catalysts for phenol hydrogenation reaction, such as Pt@titanium nanotubes, Ru / MIL-101, Pd@mpg-C 3 N 4 etc. Among them, the performance of the supported Pd catalyst is outstanding. Therefore, the development of new and efficient ca...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/08B01J37/06C07C45/00C07C49/403
Inventor 陈日志邵延华张久选姜红刘业飞邢卫红
Owner NANJING UNIV OF TECH
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