Preparation method and application of high-efficiency nitrogen-doped carbon nanotube

A technology of nitrogen-doped carbon and multi-walled carbon nanotubes, which is applied to the production method of high-efficiency nitrogen-doped carbon nanotubes and the application field of nitrogen-doped carbon nanotubes, and can solve the problem of affecting performance, low nitrogen doping amount, etc. problems, to achieve the effect of improved anti-agglomeration ability, high nitrogen doping amount, and advanced technology

Active Publication Date: 2018-02-13
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using one-step nitrogen-doped carbon nanotubes, the nitrogen doping amount is low, not exceeding 4.05% (L.M.Ombaka.J.Solid State Chem, 235(2016), 202-211), which affects its performance

Method used

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  • Preparation method and application of high-efficiency nitrogen-doped carbon nanotube
  • Preparation method and application of high-efficiency nitrogen-doped carbon nanotube
  • Preparation method and application of high-efficiency nitrogen-doped carbon nanotube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Embodiment 1, hydrothermal oxidation of carbon nanotubes

[0064] ①. Measure 0.23mL of nitric acid and 74.77mL of deionized water, add them into a beaker, stir for 10min, and make a 0.05mol / L nitric acid aqueous solution;

[0065] ②. Weigh the specific surface area to be 180m 2 / g, the pore volume is 0.90ml / g, and the average pore diameter is 2g of the original multi-walled carbon nanotubes of 12.8nm, add in the above-mentioned nitric acid aqueous solution;

[0066] ③. Transfer the above mixture to an autoclave equipped with a temperature controller and a propeller stirring system. The autoclave is sealed and flushed with nitrogen three times to exhaust the dissolved oxygen in the solution. Stir at a speed of 1 / min, then heat up to 120°C and keep for 1h, finally cool the autoclave to room temperature and release the pressure, wash with ionized water until neutral, filter with suction, and dry in an oven at a drying temperature of 90°C for a drying time of 12h .

[00...

Embodiment 2

[0084] The operation and steps are the same as in Example 1, but the concentration of nitric acid used in the oxidation is changed to 0.5mol / L, the oxidation temperature is changed to 180°C, the oxidation pressure is changed to 0.8MPa, the stirring speed is changed to 200r / min, and the oxidation time becomes 2h; when high-temperature nitrogen doping, the quality of melamine becomes 4.5g, obtains high-temperature nitrogen-doped multi-walled carbon nanotubes, and the specific surface area of ​​nitrogen-doped carbon nanotubes is 171m 2 / g, the pore volume is 0.87ml / g, the average pore diameter is 12.7nm, and the elemental analysis atomic percentage is that the carbon element content is 83.6%, the oxygen element content is 6.8%, and the nitrogen element content is 9.6%.

[0085] Preparation of nitrogen-doped carbon nanotube-confined copper catalyst

[0086] ①. Weigh 0.189g Cu(NO 3 ) 2 ·3H 2 O, measure 3 mL of deionized water, add it to a beaker, and stir it magnetically for 10 ...

Embodiment 3

[0095] The operation and steps are the same as in Example 1, but the concentration of the hydrothermal oxidation nitric acid aqueous solution is changed to 0.5mol / L, the oxidation temperature is changed to 200°C, the oxidation pressure is changed to 1.0MPa, the stirring speed is changed to 300r / min, and the oxidation The time becomes 3h; when high-temperature nitrogen doping, the mass of melamine becomes 6g, and high-temperature nitrogen-doped multi-walled carbon nanotubes are obtained, and the specific surface area of ​​nitrogen-doped carbon nanotubes is 135m 2 / g, the pore volume is 0.76ml / g, the average pore diameter is 15.1nm, and the elemental analysis atomic percentage is that the carbon element content is 82.3%, the oxygen element content is 7.4%, and the nitrogen element content is 10.3%.

[0096] Preparation of nitrogen-doped carbon nanotube-confined copper catalyst

[0097] ①. Weigh 0.265g Cu(NO 3 ) 2 ·3H 2 O, measure 3 mL of deionized water, add it to a beaker, a...

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Abstract

The invention discloses a preparation method of a high-efficiency nitrogen-doped carbon nanotube. The preparation method comprises the following steps: adding a multiwalled carbon nanotube into a nitric acid solution; closing the solution in an autoclave; pressurizing to 0.4 to 1.0 MPa, and stirring; then heating to 120 to 200 DEG C and keeping for 1 to 4 hours; finally, cooling to room temperature by the autoclave; washing to neutral and carrying out suction filtration and drying; mixing the carbon nanotube with a melamine solid according to the mass ratio being 1 to (1 to 4), and uniformly grinding by using mortar; and carrying out high-temperature sintering in nitrogen, washing to neutral and then drying to obtain the nitrogen-doped carbon nanotube. The nitrogen doping amount of the high-efficiency nitrogen-doped carbon nanotube disclosed by the invention is 4.6 to 10.3 weight percent.

Description

technical field [0001] The invention relates to a method for preparing high-efficiency nitrogen-doped carbon nanotubes and the application of the nitrogen-doped carbon nanotubes. Background technique [0002] Carbon materials are widely used in the field of catalysis due to their rich pore structure and easy surface modification. For example, carbon-supported copper catalysts are often used in the synthesis of dimethyl carbonate, especially activated carbon-supported copper catalyzed gas-phase oxidative carbonylation of methanol, such as patents CN102600843A and CN102872879A. Although the activated carbon-supported copper catalyst exhibits high initial activity, the activated carbon is mainly microporous, and most of the copper species are located on the outer surface of the activated carbon, which is easy to agglomerate during the catalyst preparation and reaction process, resulting in a decrease in dispersion and rapid catalytic activity. decline. The chemical properties...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/168B82Y40/00B01J21/18C07C68/00B01J35/10B01J23/72B01J27/24C07C69/96
CPCB01J21/185B01J23/72B01J35/1019B01J35/1042B01J35/1061B82Y40/00C01P2002/54C01P2006/12C01P2006/14C01P2006/17C07C68/01C07C69/96
Inventor 张国强李忠闫俊芬王佳君贾东森
Owner TAIYUAN UNIV OF TECH
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