Mesopore carbon load nickel hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and nickel-loaded technology, which is applied in the direction of catalyst activation/preparation, chemical instruments and methods, and preparation of organic compounds, can solve the problems of low catalyst activity and uneven dispersion of active components, and achieve excellent catalytic performance, The effect of stable catalyst structure and excellent hydrogen storage performance

Inactive Publication Date: 2010-04-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical solution of the present invention is: by using an organic solvent as the impregnating solution, the problem of low catalyst activity caused by uneven dispersion of the active components on the surface of the carbon carrier is overcome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put a ceramic bowl filled with 15g of furfuryl alcohol at the bottom of the sealable reactor, spread 10g of attapulgite in a tray with air holes, and put the tray into the middle of the reactor. After sealing, put the reactor into an oven, and conduct deposition polymerization at 130°C for 4 hours. Then put the attapulgite deposited with furfuryl alcohol in a quartz tube furnace and carbonize at 800°C for 3h under the protection of nitrogen. The obtained carbonized product was soaked in 38wt% hydrofluoric acid for 18 hours, filtered and washed with deionized water, dried at 100°C for 10 hours, soaked in 0.5mol / L hydrochloric acid solution for 24 hours, filtered and washed to pH=7, and dried at 100°C for 18 hours mesoporous carbon.

[0030] Disperse 1 g of the mesoporous carbon carrier prepared in Example 1 in 6.8 ml of nickel acetate ethanol / water (volume fraction of water is 50%) solution (0.42 mol / L), disperse for 20 min under the action of ultrasound, and stand at 2...

Embodiment 2

[0035] Put a ceramic bowl filled with 20g of furfuryl alcohol at the bottom of the sealable reactor, spread 12g of attapulgite in a tray with air holes, and put the tray into the middle of the reactor. After sealing, put the reactor into an oven, and conduct deposition polymerization at 130°C for 8 hours. Then put the attapulgite deposited with furfuryl alcohol in a quartz tube furnace and carbonize at 750°C for 4h under the protection of nitrogen. The obtained carbonized product was soaked in 40wt% hydrofluoric acid for 24 hours, filtered and washed with deionized water, dried at 110°C for 10 hours, soaked in 0.5mol / L hydrochloric acid solution for 24 hours, filtered and washed to pH=6.5, and dried at 130°C for 12 hours mesoporous carbon.

[0036] Disperse 1 g of the mesoporous carbon carrier prepared in Example 2 in 6.8 ml of nickel nitrate methanol solution (0.5 mol / L), disperse under the action of ultrasound for 30 min, and then stand at 28° C. for 2 h. Stir and dry at 9...

Embodiment 3

[0041] Put a ceramic bowl filled with 22g furfuryl alcohol at the bottom of the sealable reactor, spread 11g of attapulgite in a tray with air holes, and put the tray into the middle of the reactor. After sealing, put the reactor into an oven, and conduct deposition polymerization at 100°C for 5 hours. Then the attapulgite with furfuryl alcohol deposited was placed in a quartz tube furnace and carbonized at 700°C for 5 hours under the protection of nitrogen. The obtained carbonized product was soaked in 35wt% hydrofluoric acid for 36 hours, filtered and washed with deionized water, dried at 120°C for 8 hours, soaked in 1mol / L hydrochloric acid solution for 12 hours, filtered and washed to pH=7, and dried at 110°C for 24 hours Mesoporous carbon is obtained.

[0042] Disperse 1 g of the mesoporous carbon prepared in Example 3 in 8.5 ml of nickel acetate ethanol solution (0.3 mol / L), disperse for 20 min under the action of ultrasound, and let stand at 22° C. for 3 h. Stir and d...

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PUM

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Abstract

The invention provides a mesopore carbon load nickel hydrogenation catalyst and a preparation method thereof. For the load type catalyst, a carrier is mesopore carbon, an active component is metal nickel, and the mass of the nickel is 5-50 percent of that of the carrier. The preparation method comprises the following steps: soaking the mesopore carbon carrier in an organic soaking liquid containing nickel salt precursor under the action of ultrasonic, standing at room temperature, drying, and activating the precursor containing a metal component through the reducibility of the carrier, i.e. by a thermal reduction mode. The invention has the advantages of high dispersity of the active component, excellent performance of the catalyst, simple preparation process and low cost and can be used for preparing p-aminophenol by carrying out liquid-phase hydrogenation on p-nitrophenol.

Description

technical field [0001] The invention relates to a supported metal catalyst for catalytic hydrogenation and a preparation method thereof, relates to a supported nickel-based catalyst for hydrogenation of p-nitrophenol, and belongs to the catalyst preparation technology. Background technique [0002] Catalytic hydrogenation technology is widely used in the hydrogenation of nitro compounds, nitriles, aromatics, olefinic bonds, aldehydes, ketones, and esters. At present, the commonly used catalysts for catalytic hydrogenation are framework nickel (Raney Ni) and supported noble metals (such as Pd / C). Although the former is cheap, it will cause environmental pollution during the preparation process; the latter is highly active but expensive, and The application of supported nickel-based catalysts in hydrogenation reactions has attracted much attention due to its low price, easy availability, high activity, good stability, and simple preparation. [0003] The impregnation method i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J21/18B01J35/10B01J37/02B01J37/16C07C215/76C07C213/02
Inventor 张利雄张钰董利姚建峰徐南平
Owner NANJING UNIV OF TECH
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