Nitrogen-doped carbon nanotube and preparation method thereof

A technology for nitrogen-doped carbon and carbon nanotubes, which is applied in the fields of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of low nitrogen content of nitrogen-doped carbon nanotubes, and achieves simple equipment and process and easy operation. , the effect of easy large-scale industrial production

Inactive Publication Date: 2014-09-10
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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Problems solved by technology

[0004] At present, the easy-to-achieve large-scale industrial preparation method of nitrogen-doped carbon nanotubes is the high-temperature thermal doping method, but the biggest problem of this method is that the nitrogen content of the prepared nitrogen-doped carbon nanotubes is low

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preparation example Construction

[0023] The preparation process of the nitrogen-doped carbon nanotubes of the present invention is roughly as follows: carbon nanotubes→modified carbon nanotubes→nitrogen-doped carbon nanotubes.

[0024] Specifically, the preparation process of nitrogen-doped carbon nanotubes of the present invention is divided into the following steps:

[0025] (1) Modified carbon nanotubes: Mix carbon nanotubes with a purity of 99% and alkali metal hydroxides or alkaline earth metal hydroxides at a mass ratio of 1:0.5 to 1:3 and place them in the reactor, and then put them into the reactor. The inert gas with a flow rate of 400ml / min is passed into the reactor to make the atmosphere in the reactor an inert environment, and then the temperature is raised to 800-900°C at a heating rate of 5-10°C / min, and it is fully reacted for 2 hours. At room temperature, the obtained solid product was added into a 10% hydrochloric acid solution and heated to 90°C, stirred for 6 hours, filtered, washed with d...

Embodiment 1

[0033] (1) Modified carbon nanotubes: Mix carbon nanotubes with a purity of 99% and potassium hydroxide at a mass ratio of 1:2 and place them in a test tube, then pass argon gas with a flow rate of 400ml / min into the test tube, Form an argon atmosphere, raise the temperature to 800°C at a heating rate of 5°C / min, fully react for 2 hours, then cool down to room temperature, add the obtained solid product into a 10% hydrochloric acid solution, heat to 90°C, and stir for 6 hours Filter, then wash with deionized water, then place 60°C in a vacuum oven and dry for 12h to obtain modified carbon nanotubes;

[0034] (2) Preparation of nitrogen-doped carbon nanotubes: Add the modified carbon nanotubes to an anhydrous ethanol solution dissolved in urea (the mass of modified carbon nanotubes and urea is 1:2), and fully stir for 2 hours Then dry at 80°C for 6 hours, place it in an argon atmosphere with a flow rate of 400ml / min, then raise the temperature (heating rate is 20°C / min) to 800°...

Embodiment 2

[0036] (1) Modified carbon nanotubes: Mix carbon nanotubes with a purity of 99% and sodium hydroxide at a mass ratio of 1:3 and place them in a test tube, then pass nitrogen gas with a flow rate of 400ml / min into the test tube to form In a nitrogen atmosphere, the temperature was raised to 900°C at a heating rate of 5°C / min. After fully reacting for 2 hours, it was lowered to room temperature. The obtained solid product was added to a 10% hydrochloric acid solution and heated to 90°C. After stirring for 6 hours, it was filtered. Wash with deionized water again, then place 60 ℃ of vacuum ovens and dry 12h, obtain the carbon nanotube of modification;

[0037] (2) Preparation of nitrogen-doped carbon nanotubes: Add the modified carbon nanotubes to an anhydrous ethanol solution dissolved in urea (the mass of the modified carbon nanotubes and ammonia water is 1:1), and fully stir for 2 hours Afterwards, dry at 80°C for 6 hours, place it in a nitrogen atmosphere with a flow rate of ...

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Abstract

The invention relates to a nitrogen-doped carbon nanotube and a preparation method thereof. The method comprises the following steps: (a) mixing a carbon nanotube with alkali metal hydroxide or alkaline earth metal hydroxide according to a mass ratio of 1: 0.5 to 1: 3, then placing the obtained mixture in a reactor, introducing inert gas into the reactor so as to allow an inert atmosphere to be formed in the reactor, carrying out heating to 800 to 900 DEG C, then carrying out cooling to room temperature after a full reaction and cleaning and drying the obtained solid product so as to obtain a modified carbon nanotube; and (b) mixing the modified carbon nanotube with a nitrogen doping agent, successively carrying out full stirring and drying, placing the obtained mixture in the inert atmosphere, then carrying out heating to 800 to 900 DEG C, maintaining the temperature for 0.5 to 1 h, then carrying out cooling to room temperature and cleaning and drying the obtained solid product so as to obtain the nitrogen-doped carbon nanotube. According to the invention, the carbon nanotube activated by potassium hydroxide has a great number of defects and has high nitrogen content during nitrogen doping; and the preparation method has the advantages of low cost and easy realization of large-scale industrial production.

Description

technical field [0001] The invention relates to the field of chemical material synthesis, in particular to a nitrogen-doped carbon nanotube and a preparation method thereof. Background technique [0002] In the 1990s, the use of carbon materials as energy storage materials promoted the vigorous development of supercapacitors and lithium-ion batteries. As a one-dimensional carbon material, carbon nanotubes have very high electrical conductivity, and carbon nanotubes are very easy to derivatize, so their derivatives have also attracted extensive attention from researchers. [0003] Carbon nanotube derivatives mainly include nitrogen-doped carbon nanotubes and boron-doped carbon nanotubes. Among them, the nitrogen atom in the nitrogen-doped carbon nanotube has one more electron than the outer layer of the carbon atom, and it is N-type doped, which has better energy storage performance than the carbon nanotube without doping, and the nitrogen-doped The higher the nitrogen cont...

Claims

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Application Information

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IPC IPC(8): C01B31/00B82Y30/00C01B32/168
Inventor 周明杰钟辉王要兵袁新生
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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