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Preparation method of supported palladium catalyst

A supported palladium and catalyst technology, applied in the field of catalysis, can solve problems such as complex process and difficult conditions, and achieve high activity and high selectivity

Active Publication Date: 2017-02-22
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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  • Preparation method of supported palladium catalyst
  • Preparation method of supported palladium catalyst
  • Preparation method of supported palladium catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of ZIF-67

[0031] First prepare 50 mL of 0.8 mol / L 2-methylimidazole methanol solution, 50 mL of cobalt nitrate hexahydrate, and 0.135 mol / L methanol mixed solution of polyvinylpyrrolidone concentrations respectively. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add the mixed solution of cobalt nitrate hexahydrate and polyvinylpyrrolidone under stirring, mix and stir for 5 minutes, and let stand for 24 hours. Centrifuge, wash twice with methanol, and finally place in an oven at 80°C for 6 hours.

[0032] (2) Preparation of CN carrier

[0033] 0.5g ZIF-67 was placed in a tube furnace and calcined at 600°C for 5h in an argon atmosphere. 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 600 . Prepared Co / CN 600 Pass through a 30% nitric acid solution, pickle at 60°C for 3 hours under continuous stirring, wash with deionized water 4 times, and...

Embodiment 2

[0039] (1) Preparation of ZIF-67

[0040]First prepare 40 mL of 0.1 mol / L methanol solution of 2-methylimidazole, 60 mL of methanol mixed solution with concentrations of 0.013 mol / L and 0.017 mol / L of cobalt nitrate hexahydrate and polyvinylpyrrolidone respectively. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add the mixed solution of cobalt nitrate hexahydrate and polyvinylpyrrolidone under stirring, mix and stir for 10 minutes, and let stand for 12 hours. Centrifuge, wash with methanol three times, and finally place in an oven at 60°C for 10 hours.

[0041] (2) Preparation of CN carrier

[0042] 0.5g ZIF-67 was placed in a tube furnace and calcined at 600°C for 5h in an argon atmosphere. The temperature was raised from room temperature to the target temperature at a rate of 0.5°C / min. Calcined samples are denoted as Co / CN 600 . Prepared Co / CN 600 After passing through nitric acid solution with a mass concentration of 15%, pickling at 60°C for ...

Embodiment 3

[0047] (1) Preparation of ZIF-67

[0048] First prepare 25 mL of 0.4 mol / L methanol solution of 2-methylimidazole, 75 mL of methanol mixed solution with concentrations of 0.05 mol / L and 0.068 mol / L of cobalt nitrate hexahydrate and polyvinylpyrrolidone respectively. First put the 2-methylimidazole solution in a 250mL Erlenmeyer flask, add the mixed solution of cobalt nitrate hexahydrate and polyvinylpyrrolidone under stirring, mix and stir for 8 minutes, and let stand for 18 hours. Centrifuge, wash with methanol three times, and finally place in an oven at 90°C for 7 hours.

[0049] (2) Preparation of CN carrier

[0050] 0.5g ZIF-67 was placed in a tube furnace and calcined at 700°C for 4.5h in an argon atmosphere. The temperature was raised from room temperature to the target temperature at a rate of 2°C / min. Calcined samples are denoted as Co / CN 700 . Prepared Co / CN 700 After passing through a nitric acid solution with a mass concentration of 20%, pickling at 60°C for ...

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Abstract

The invention relates to a preparation method of a supported palladium catalyst. According to the catalyst, with ZIF-67 being a precursor, a slow temperature programming method is adopted for calcining ZIF-67 so that ZIF-67 is subjected to pyrolysis to be a Co / CN material; then an acid pickling method is adopted for preparing a carbon-nitrogen (CN) carrier, and then the catalyst is prepared after stirring and dipping are carried out with active component salt and H2 reacting is carried out. The preparation method has the advantages that the preparation technology is simple, the CN material with micropores and mespores has a large specific surface area, and dispersion of the active component and diffusion of reactant are promoted; the prepared Pd@CN catalyst has good stability and shows excellent catalytic performance in the reaction of phenol selective hydrogenation cyclohexanone preparation.

Description

technical field [0001] The invention relates to a method for preparing a supported catalyst, in particular to a method for preparing a supported palladium catalyst used in a hydrogenation process, and belongs to the technical field of catalysis. Background technique [0002] Cyclohexanone, as an important intermediate in the production of nylon 6 and nylon 66, is mainly produced by oxidation of cyclohexane. However, cyclohexane oxidation needs to be carried out under high temperature and high pressure, and many by-products will be generated, which is a very environmentally unfriendly production process. Recently, due to the advantages of environmental protection and low energy consumption, the process of direct hydrogenation of phenol to cyclohexanone has attracted widespread attention. [0003] The reaction mechanism of the hydrogenation of phenol to cyclohexanone is as follows: phenol is chemically adsorbed on the surface of the carrier, and the hydrogen gas activated by ...

Claims

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Application Information

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IPC IPC(8): B01J29/072C07C45/00C07C49/403
CPCC07C45/006B01J29/072B01J37/0201B01J37/0236C07C49/403
Inventor 陈日志丁帅帅姜红刘业飞邢卫红
Owner NANJING UNIV OF TECH
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