A highly dispersed silica nanotube-supported nickel catalyst and its preparation method

A technology of silica and nanotubes, which is applied in the field of highly dispersed silica nanotube-supported nickel catalysts and its preparation, can solve the problems of high dispersion catalysts and other problems, and achieve simple and rapid methods, easy-to-obtain synthetic raw materials, and high resistance to accumulation. The effect of carbon capacity

Active Publication Date: 2020-11-13
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, it is relatively difficult to prepare highly dispersed catalysts with these methods when the loading of nanoparticles is high (20 wt%–30 wt%)

Method used

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  • A highly dispersed silica nanotube-supported nickel catalyst and its preparation method
  • A highly dispersed silica nanotube-supported nickel catalyst and its preparation method
  • A highly dispersed silica nanotube-supported nickel catalyst and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Put 1 gram of carbon nanotubes into a 200ml flask, add 100ml of ethanol, 50ml of water, 6.9ml of ammonia (28wt%) and CTAB (concentration of 5g per liter) in sequence and stir well. Then, 1 mL of tetraethyl orthosilicate was added, reacted for 2 days, and centrifuged. After washing with a mixed solvent of ethanol and water, centrifuging, and drying at room temperature for 12 hours, a carbon nanotube@silica core-shell nanocomposite was obtained. Among them, the thickness of the silica nanotube shell is 10nm ( figure 2 ). XRD diffraction Figure 6 The diffraction pattern of middle b is at 23.5 o Diffraction peaks of silica appear. In addition, the intensity of the diffraction peak of the carbon nanotube becomes weak. These all indicate the successful synthesis of carbon nanotubes@silica core-shell structure.

[0028] (2) Add ammonia water to the carbon nanotube@silica core-shell composite obtained in the previous step, and 1 g of nickel nitrate, and adjust the p...

Embodiment 2

[0033] (1) Put 1 gram of carbon nanotubes into a 200ml flask, add 100ml of ethanol, 50ml of water, 6.9ml of ammonia (28wt%) and CTAB (concentration of 5g per liter) in sequence and stir well. Then, 5 mL of methyl orthosilicate was added, reacted for 5 days, and centrifuged. After washing with a mixed solvent of ethanol and water, centrifuging, and drying at room temperature for 12 hours, a carbon nanotube@silica core-shell nanocomposite was obtained.

[0034] (2) Add the carbon nanotube@silica core-shell composite obtained in the previous step, 2 grams of nickel chloride, and ammonia water to adjust the pH to 12. Put the mixed solution into an autoclave, heat to 180°C, react for 48 hours, and cool to room temperature. Centrifuge, wash with methanol, ethanol, and water in sequence, and put it in a 100-degree drying oven. Get a carbon nanotube@silica@nickel silicate triple core-shell structure (such as image 3 shown). Specific area is 805m 2 g -1 , the nickel loading is 2...

Embodiment 3

[0037] (1) Put 0.5 g of carbon nanotubes into a 200 ml flask, add 100 ml of ethanol, 50 ml of water, 6.9 ml of ammonia (28 wt%) and CTAB (concentration of 5 g per liter) in sequence and stir well. Then, 1 mL of sodium silicate was added, reacted for 1 day, and centrifuged. After washing with a mixed solvent of ethanol and water, centrifuging, and drying at room temperature for 12 hours, a carbon nanotube@silica core-shell nanocomposite was obtained.

[0038] (2) Add ammonia water to the carbon nanotube@silica core-shell composite obtained in the previous step, 2 g of nickel acetylacetonate, and adjust the pH to 10. Put the mixed solution into an autoclave, heat to 150°C, react for 1 hour, and cool to room temperature. Centrifuge, wash with methanol, ethanol, and water in sequence, and put it in a 100-degree drying oven. Get a carbon nanotube@silica@nickel silicate triple core-shell structure (such as image 3 shown). Specific area is 505m 2 g -1 , the nickel loading is 2...

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Abstract

The invention belongs to the technical field of advanced nano composites and particularly relates to a high-dispersion silica nanotube-supported nickel catalyst and a preparation method thereof. A silica precursor is hydrolyzed first under alkaline conditions by means of microemulsion process to coat the surface of nanotubes with a uniform layer of silica, and carbon nanotube-silica core-shell structure is formed; the carbon nanotube-silica core-shell structure and a nickel precursor are treated under alkaline conditions by means of hydrothermal process to obtain carbon nanotube-silica-nickelsilicate precursor tri-layer core-shell structure; a carbon nanotube template is removed by high temperature calcining to obtain silica-nickel silicate core-shell structure; finally, the nickel silicate precursor is decomposed in situ by means of high temperature reduction to obtain high-dispersion nickel nano particles supported on the surface of the silica nanotubes. The preparation method can ensure high dispersion of the nickel nano particles under high nickel load.

Description

technical field [0001] The invention belongs to the field of advanced nanocomposite materials and technology, and in particular relates to a highly dispersed silica nanotube-supported nickel catalyst and a preparation method thereof. Background technique [0002] The size effect of nanoparticles has been widely concerned in the fields of catalysis, medicine, environmental protection and energy storage. This is because nanometer-sized metal catalysts often have more active sites, that is, they have high catalytic activity. However, active metal nanoparticles are prone to sintering at high temperature, which reduces or even loses their catalytic activity. The preparation of nano-catalysts with high dispersion is an important way to improve the anti-sintering ability of nano-metals, and has always been the focus of research in the field of catalysis. [0003] At present, many methods have been used to prepare highly dispersed nanocatalysts. For example: impregnation method (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J37/10B01J37/08B01J37/18B01J37/16B01J32/00B01J35/10C01B3/40
CPCB01J23/755B01J35/006B01J35/008B01J35/1019B01J37/0018B01J37/088B01J37/10B01J37/16B01J37/18C01B3/40C01B2203/0227C01B2203/1058Y02P20/52
Inventor 李自卫李敏
Owner GUIZHOU UNIV
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