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Phenol hydrogenation catalyst and preparation method thereof

A technology of hydrogenation catalyst and phenol, which is applied in the field of catalysis and can solve problems such as complex process and difficult conditions

Active Publication Date: 2018-09-28
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composite mpg-C 3 N 4 The process is complex and the conditions are difficult to control

Method used

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  • Phenol hydrogenation catalyst and preparation method thereof
  • Phenol hydrogenation catalyst and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) ZIF-67-TiO 2 preparation of

[0032] 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. 0.01 g TiO 2 Disperse in 50 mL of 20 g / L polyvinylpyrrolidone methanol solution, stir for 10 min, put the 2-methylimidazole solution in, continue stirring for 10 min, add Co(NO 3 ) 2 ·6H 2 O methanol solution, after mixing and stirring for 10 h, stop stirring, and let the mixture stand 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 Dry in an oven at C for 6 h, and the sample is denoted as ZIF-67-TiO 2 -0.01.

[0033] (2) CN-TiO 2 Preparation of vector

[0034] Take 0.5 g of prepared ZIF-67-TiO 2 -0.01 In a tube furnace, the calcination atmosphere is argon, and the calcination temperature is 600 o C, the calcination time is 5 h. The temperature is raised from room temperature to ...

Embodiment 2

[0040] (1) ZIF-67-TiO 2 preparation of

[0041] First, prepare 50 mL of 1.6 mol / L methanol solution of 2-methylimidazole and 50 mL of 0.05 mol / L methanol solution of cobalt nitrate hexahydrate. 0.05 g TiO 2 Disperse in 50 mL of 10 g / L polyvinylpyrrolidone methanol solution, stir for 30 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 8 h and then stopped stirring, and the mixture was allowed to stand at room temperature for 5 h. After standing, the product was separated by centrifugation, washed 5 times with methanol, and finally washed at 50 o Dry in an oven at C for 24 h, and the sample is denoted as ZIF-67-TiO 2 -0.05.

[0042] (2) CN-TiO 2 Preparation of vector

[0043] Take 0.5 g of prepared ZIF-67-TiO 2 -0.05 In a tube furnace, the calcination atmosphere is helium, and the calcination temperature is 550 o C, the calcination time is 8 h. The temperature is raised from room te...

Embodiment 3

[0048] (1) ZIF-67-TiO 2 preparation of

[0049] First, prepare 50 mL of 0.4 mol / L methanol solution of 2-methylimidazole and 50 mL of 0.2 mol / L methanol solution of cobalt nitrate hexahydrate. 0.1 g TiO 2 Disperse in 50 mL of 40 g / L polyvinylpyrrolidone methanol solution, stir for 20 min, put 2-methylimidazole solution in, continue stirring for 30 min, add Co(NO 3 ) 2 ·6H 2 O methanol solution, after mixing and stirring for 20 h, stop stirring, and the mixture was directly separated from the product by centrifugation, and washed twice with ethanol, and finally at 70 o Dry in an oven at C for 12 h, and the sample is denoted as ZIF-67-TiO 2 -0.1.

[0050] (2) CN-TiO 2 Preparation of vector

[0051] Take 0.5 g of prepared ZIF-67-TiO 2 -0.1 In a tube furnace, the calcination atmosphere is nitrogen, and the calcination temperature is 800 o C, the calcination time is 4 h. The temperature is raised from room temperature to the target temperature at a rate of 4 o C / min. C...

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Abstract

The invention relates to a phenol hydrogenation catalyst and a preparation method thereof and belongs to the technical field of catalysis. ZIF-67-TiO2, as a precursor, is calcined in a slow-programmedheating manner to obtain a Co / CN-TiO2 material, which is then subjected to acid pickling to obtain a CN-TiO2 supporter; the CN-TiO2 supporter finally is subjected to stirring impregnation with activecomponent salts and hydrogen reduction to obtain the catalyst. The method is advantaged in that the ZIF-67 is modified by a less amount of anatase-type TiO2, so that specific surface area of the supporter is significantly increased and electron transmission capability is enhanced. Catalytic performance of producing cyclohexanone by hydrogenation of phenol is significantly improved. The prepared catalyst has excellent catalytic stability.

Description

technical field [0001] The invention relates to a 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 and an important intermediate for the production of nylon 6 and nylon 66. At present, the main industrial preparation route is cyclohexane oxidation. However, cyclohexane oxidation under high temperature and high pressure will generate many by-products, which is an environmentally unfriendly production process. 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. [0003] In recent years, carbon-nitrogen materials have attracted extensive attention from researchers. The introduction of N elements can not only change the acidity and alkalinity, conductivity, and hydrophilicity / hydrophobicity of carbon materials, but...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/08B01J37/10B01J37/02B01J37/18C07C45/00C07C49/403
CPCC07C45/00B01J27/24B01J37/0201B01J37/086B01J37/10B01J37/18C07C49/403
Inventor 陈日志张久选姜红刘业飞邢卫红
Owner NANJING UNIV OF TECH
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