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A kind of oxygen-vacancy phenol hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and phenol technology, applied in the field of catalysis, can solve the problems such as the metal electronic structure is not widely used, the complex preparation process, etc., and achieve the effect of improving the hydrogenation performance of phenol and enhancing the electron transport ability.

Active Publication Date: 2021-11-19
NANJING TECH UNIV
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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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  • A kind of oxygen-vacancy phenol hydrogenation catalyst and preparation method thereof
  • A kind of oxygen-vacancy phenol hydrogenation catalyst and preparation method thereof
  • A kind of oxygen-vacancy 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, after mixing and stirring for 15 h, stop 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 phenol hydrogenation catalyst and a preparation method thereof, belonging to the technical field of catalysis. The catalyst uses ZIF-67 as a precursor, and ZIF-67 is prepared by high-temperature calcination and acid washing to obtain nitrogen-doped carbon material (CN), and then the sol-gel method and subsequent high-temperature calcination are introduced to contain oxygen vacancies. Titanium dioxide nano-islands, finally stirred and impregnated with active component salt, H 2 Reduction made catalyst. The advantage of this invention is that, through anatase TiO 2 The nano-island modified ZIF-67 derived CN material can effectively enhance the interaction between the carrier and the active component, increase the number of surface active components and electron-rich properties, enhance the anti-oxidation performance of the active component, and significantly enhance its phenol addition. The catalytic performance of cyclohexanone from hydrogen, and 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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Patent Type & Authority Patents(China)
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 TECH UNIV
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