Preparation method of phenol hydrogenation catalyst

A hydrogenation catalyst, phenol technology, applied in the field of catalysis, can solve the problems of high temperature and high pressure, products accompanied by by-products, unfriendly to the environment, etc.

Active Publication Date: 2017-12-01
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former has defects in the production process, such as: harsh operating conditions (high temperature and high pressure), products accompanied by by-products, etc., which are environmentally unfriendly processes
However, the introduction of an additional nitrogen source during ZIF synthesis to resynthesize CN materials has not been reported.

Method used

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  • Preparation method of phenol hydrogenation catalyst
  • Preparation method of phenol hydrogenation catalyst
  • Preparation method of phenol hydrogenation catalyst

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 2-methylimidazole methanol solution and 50 mL of 0.1 mol / L cobalt nitrate hexahydrate methanol solution. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add 0.25g of dicyandiamide under stirring, and then add 50mL of cobalt nitrate hexahydrate methanol solution, mix and stir for 24 hours. After standing still, the product was centrifuged and washed twice with methanol, and finally the final sample was baked in an oven at 80°C for 6h.

[0035] (2) Preparation of CN carrier

[0036] Take 0.5 g of the prepared ZIF-67 in a tube furnace, the calcination atmosphere is argon, the calcination temperature is 600° C., and the calcination time is 5 h. The temperature was raised from room temperature to the target temperature at a rate of 1°C / min. Calcined samples are denoted as Co-CN D . Prepared Co-CN D The sample was pickled in 30% nitric acid solution for 3 hours at 60°C under contin...

Embodiment 2

[0042] (1) Preparation of ZIF-67

[0043] First prepare 50mL of 0.4mol / L methanol solution of 2-methylimidazole and 50mL of 0.05mol / L methanol solution of cobalt nitrate hexahydrate. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add 0.5g of dicyandiamide under stirring, add 50mL of methanolic cobalt nitrate hexahydrate solution after stirring evenly, mix and stir and let it stand for 12 hours. After standing still, the product was centrifuged and washed 7 times with methanol, and finally the final sample was baked in an oven at 50°C for 24h.

[0044] (2) Preparation of CN carrier

[0045] Take 0.5 g of the prepared ZIF-67 in a tube furnace, the calcination atmosphere is nitrogen, the calcination temperature is 700° C., and the calcination time is 4 hours. The temperature was raised from room temperature to the target temperature at a rate of 0.8°C / min. Calcined samples are denoted as Co-CN D . Prepared Co-CN D The sample was pickled in 35% nitric ...

Embodiment 3

[0050] (1) Preparation of ZIF-67

[0051] First prepare 50mL of 0.1mol / L methanol solution of 2-methylimidazole and 50mL of 0.02mol / L methanol solution of cobalt nitrate hexahydrate. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add 0.4g of dicyandiamide under stirring, add 50mL of methanolic cobalt nitrate hexahydrate solution after stirring evenly, mix and stir and let it stand for 12 hours. After standing still, the product was centrifuged and washed 4 times with methanol, and finally the final sample was dried in an oven at 100°C for 10 h.

[0052] (2) Preparation of CN carrier

[0053] Take 0.5 g of the prepared ZIF-67 in a tube furnace, the calcination atmosphere is helium, the calcination temperature is 800° C., and the calcination time is 8 h. The temperature was raised from room temperature to the target temperature at a rate of 3°C / min. Calcined samples are denoted as Co-CN D . Prepared Co-CN D The sample was pickled in 40% nitric acid s...

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Abstract

The invention relates to a preparation method of a phenol hydrogenation catalyst, belonging to the technical field of catalysis. The catalyst uses dicyanodiamide-modified ZIF-67 as a precursor, ZIF-67 is calcined through a slow temperature programming method so as to produce a Co-CN material, then Co is removed through an acid pickling method so as to obtain a carbon-nitrogen (CN) carrier, and the carrier is stirred and soaked in a palladium chloride water solution and then is reduced in the H<2> atmosphere so as to prepare the catalyst. The preparation method has the advantages that dicyanodiamide is added in synthesis of ZIF-67 so as to improve the specific surface area of the carrier CN material, prohibit oxidization of zerovalent palladium, and acquire more zerovalent palladium; and the prepared Pd@CN catalyst presents excellent catalysis performance in reaction of hydrogenation of phenol to cyclohexanone.

Description

technical field [0001] The invention relates to a preparation method of a phenol hydrogenation catalyst, in particular to a preparation method of a supported palladium catalyst used in a hydrogenation process, and belongs to the technical field of catalysis. Background technique [0002] As a very important industrial raw material, cyclohexanone is mainly produced by two processes: cyclohexane oxidation and phenol hydrogenation. The former has defects in the production process, such as: harsh operating conditions (high temperature and high pressure), products accompanied by by-products, etc., which are environmentally unfriendly processes. The one-step hydrogenation of phenol to cyclohexanone has the advantages of mild reaction conditions and high selectivity, and has attracted more and more attention. [0003] According to the reaction mechanism of phenol hydrogenation to cyclohexanone, many corresponding catalysts have been developed. Studies have shown that the selectiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J23/44C07C45/00C07C49/403
CPCB01J23/44B01J27/24C07C45/006C07C49/403
Inventor 陈日志丁帅帅姜红刘业飞邢卫红
Owner NANJING UNIV OF TECH
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