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Preparation method and application of nitrogen-sulfur co-doped carbon nanotube

A technology of nitrogen-sulfur co-doping and carbon nanotubes, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problem of low preparation efficiency, harsh conditions, and nitrogen-sulfur co-doping nanomaterials Complicated process and other issues, to achieve large specific surface area, low cost, and improve electrochemical performance

Active Publication Date: 2018-09-14
CHANGZHOU UNIV
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  • Description
  • Claims
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Problems solved by technology

[0006] In order to solve the deficiencies in the prior art of preparing nitrogen-sulfur co-doped nanomaterials with complex process, harsh conditions, and low production efficiency, the present invention provides a simple and feasible method for preparing nitrogen-sulfur co-doped carbon nanotubes, and utilizes Angstrom The catalytic oxygen reduction performance of nitrogen-sulfur co-doped carbon nanotubes prepared by Luoshi's own advantages as a template is greatly improved

Method used

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  • Preparation method and application of nitrogen-sulfur co-doped carbon nanotube
  • Preparation method and application of nitrogen-sulfur co-doped carbon nanotube
  • Preparation method and application of nitrogen-sulfur co-doped carbon nanotube

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preparation example Construction

[0023] The preparation process of the nitrogen and sulfur co-doped carbon nanotubes of the present invention is specifically as follows:

[0024] (1) Modified halloysite: Disperse pure halloysite in 0.1-0.5 mol / L hydrochloric acid and continue mechanical stirring for 8-24 hours to obtain acidified modified halloysite.

[0025] (2) Synthesis of halloysite / polythiophene composite material: Dissolve modified halloysite and thiophene in an organic solvent at the same time (the mass ratio of thiophene monomer to halloysite is 0.5-2:1; halloysite and organic solvent The mass ratio of 0.05~0.15:1), keep the magnetic stirring for 20~40min, then add the oxidant anhydrous ferric chloride to the system (the mass ratio of anhydrous ferric chloride to thiophene is 3~5:1), 0 Continue to stir and react for 6-12 hours at ~5°C, filter, wash with absolute ethanol, and dry to obtain halloysite / thiophene composite material;

[0026] (3) Synthesize halloysite / polythiophene / polypyrrole composite material...

Embodiment 1

[0033] (1) Modified halloysite: Disperse pure halloysite in 0.2mol / L hydrochloric acid and continue mechanical stirring for 16 hours to obtain acidified modified halloysite.

[0034] (2) Synthesis of halloysite / polythiophene composite materials: 3g modified halloysite and 0.5g thiophene were simultaneously dissolved in 20mL chloroform (the mass ratio of thiophene monomer to halloysite was 0.5:1; halloysite and organic The mass ratio of solvent is 0.15:1), keep magnetic stirring for 20min, then add 2g of oxidant anhydrous ferric chloride (the mass ratio of anhydrous ferric chloride to thiophene is 4:1), continue stirring at 5℃ React for 12h, filter, wash with absolute ethanol, and dry to obtain halloysite / polythiophene composite material;

[0035] (3) Synthesize halloysite / polythiophene / polypyrrole composite material: mix 1g of composite material in (2) with 20mL deionized water (the mass ratio of composite material and deionized water is 0.05:1), ultrasonically disperse for 30 minu...

Embodiment 2

[0039] (1) Modified halloysite: Disperse pure halloysite in 0.1 mol / L hydrochloric acid and continue mechanical stirring for 12 hours to obtain acidified modified halloysite.

[0040] (2) Synthesis of halloysite / polythiophene composite material: 3g modified halloysite and 3g thiophene are simultaneously dissolved in 60mL toluene (the mass ratio of thiophene monomer to halloysite is 1:1; halloysite and organic solvent The mass ratio of 0.05:1), keep magnetic stirring for 30min, then add 9g of oxidizing agent anhydrous ferric chloride (the mass ratio of anhydrous ferric chloride to thiophene is 3:1), continue to stir the reaction at 0℃ 9h, filter, wash with absolute ethanol, and dry to obtain halloysite / polythiophene composite;

[0041] (3) Synthesize halloysite / polythiophene / polypyrrole composite material: mix 1g of the composite material in (2) with 12.5mL deionized water (the mass ratio of composite material to deionized water is 0.08:1), ultrasonically disperse for 20 minutes, A...

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Abstract

The invention relates to a method of controllably preparing a nitrogen-sulfur co-doped carbon nanotube by taking halloysite as a template, and belongs to the scientific and technical field of batterymaterials. The method includes taking the halloysite, thiophene and pyrrole as raw materials, performing low-temperature polymerization on the halloysite and the thiophene to obtain a halloysite / thiophene composite material, mixing the halloysite / thiophene composite material with the pyrrole to obtain halloysite / conducting polymer composite material, performing high-temperature treatment on the composite material, and removing the halloysite to obtain the nitrogen-sulfur co-doped carbon nanotube. The invention further provides application of the nitrogen-sulfur co-doped carbon nanotube obtained by the preparation method. The nitrogen-sulfur co-doped carbon nanotube is applied to fuel cell catalysis on negative-electrode oxygen reduction reactions.

Description

Technical field [0001] The invention relates to a method for controlling the preparation of nitrogen and sulfur co-doped carbon nanotubes by using halloysite as a template, and belongs to the field of battery material science and technology. Background technique [0002] Fuel cell technology is the leader in new energy technology, but because its cathode oxygen reduction reaction (ORR) is relatively slow, it requires a large number of catalysts to catalyze it. For many years, platinum (Pt)-based catalysts have been considered the best choice for oxygen reduction catalysts, but platinum-based catalysts generally have high costs and poor stability. In recent years, metal-free carbon-based catalysts have been considered as possible replacements for Pt-based catalysts due to their oxygen reduction active sites, low price and good stability. [0003] Carbon nanotubes as a kind of sp 2 Hybrid structure of carbon materials has a good structural foundation in mechanics and thermodynamics,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/90H01M4/96B82Y30/00
CPCB82Y30/00H01M4/9091H01M4/96Y02E60/50
Inventor 刘文杰汝钱洵左士祥姚超杜涛王亮李霞章罗士平
Owner CHANGZHOU UNIV
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