Nitrogen-doped carbon nanotube material

A technology for acidifying carbon nanotubes and nanotubes, which is applied to nanocomposite materials and their application fields, can solve the problems of low product utilization rate, complicated and time-consuming operation, low nitrogen doping content, etc., and achieves simplified production process, easy storage, The effect of large specific surface area

Active Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0007] In order to solve the problems in the preparation of nitrogen-doped carbon nanotube materials in the prior art, such as complex equipment, cumbersome process, complicated and time-consuming operation, low product utilization rate and low nitrogen doping content caused by a large amount of nitrogen-doped precursor loss during the nitrogen doping process , the present invention provides an efficient, fast, large-scale method for synthesizing high-nitrogen content-doped carbon nanotube materials, the obtained nitrogen-doped carbon nanotubes have high nitrogen content, the utilization rate of raw materials is significantly improved, and the product does not need washing, separation, drying and other processes. It can be directly used as a negative electrode material for lithium batteries, with good application performance

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preparation example Construction

[0036] Preparation of acidified carbon nanotubes: put 1g of carbon nanotubes and 200mL of concentrated sulfuric acid into a three-necked flask, ultrasonically disperse evenly, slowly add 60mL of 70% concentrated nitric acid dropwise, reflux and stir at 60°C for 1h, cool naturally to room temperature, add Dilute with a large amount of deionized water, let it stand for stratification, remove the supernatant, and dialyze the black precipitate at the bottom with deionized water to replace the small molecules in it, so that the surface can be balanced, and a long-term stable and uniform dispersion of carbon nanotubes can be obtained. liquid. The carbon nanotube aqueous dispersion is freeze-dried to obtain acidified carbon nanotube powder, which is placed in a desiccator for subsequent use. Its SEM picture is as follows figure 1As shown, the structure of one-dimensional carbon nanotubes can be clearly seen, and the walls of carbon nanotubes after acidification treatment are relativ...

Embodiment 1

[0039] (1) Weigh 1.0 g of acidified carbon nanotubes and disperse them in 20 mL of 37% formaldehyde aqueous solution, place them in an ultrasonic instrument and disperse evenly, and record them as dispersion liquid A.

[0040] (2) Weigh 3.0g of melamine and add it to 40mL of deionized water, place it in an ultrasonic instrument and ultrasonically disperse it evenly, and record it as dispersion liquid B.

[0041] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 60°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 120° C. for 12 hours to react. Suction filtration, vacuum drying to obtain a black solid powder.

[0042] (4) Put the black solid powder obtained in step (3) into a microwave reaction chambe...

Embodiment 2

[0044] (1) Weigh 1.0 g of acidified carbon nanotubes and disperse them in 30 mL of 37% formaldehyde aqueous solution, place them in an ultrasonic instrument and disperse evenly, and record them as dispersion liquid A.

[0045] (2) Weigh 5.0g of melamine and add it to 40mL of deionized water, place it in an ultrasonic instrument and ultrasonically disperse it evenly, and record it as dispersion liquid B.

[0046] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 60°C and stir for 10 minutes. Then triethanolamine was added to the reaction solution to adjust the pH value of the reaction solution system to 8.0, and the mixture was uniformly mixed by ultrasonic, then the reaction solution was poured into a high-pressure reactor, and the temperature was raised to 120° C. for 12 hours to react. Suction filtration, vacuum drying to obtain a black solid powder.

[0047] (4) Put the black solid powder obtained in step (3) into a microwave reaction chambe...

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Abstract

The invention relates to a nitrogen-doped carbon nanotube material, which is prepared through steps: adopting formaldehyde as a bridge, enabling formaldehyde and melamine to be subjected to moderate crosslinking to form a nitrogen-doped precursor, then performing hydrothermal reaction, enabling the nitrogen-doped precursor and carbon nanotubes to be interacted and uniformly fused, and then performing solvent-free microwave reaction to synthesize high-nitrogen-content doped carbon nanotubes. In the preparation process of the nitrogen-doped carbon nanotube material, the loss caused by sublimation of a nitrogen-doped precursor in the heating process in the traditional nitrogen doping process is avoided, the nitrogen doping efficiency is improved, the reaction conditions are progressively increased from mild to intense, and uniform fusion of interaction of the nitrogen-doped precursor and carbon nanotubes is realized. The prepared nitrogen-doped carbon nanotube material is good in stability, not prone to denaturation in air, easy to store and large in specific surface area, a good channel is provided for lithium ion transmission when the nitrogen-doped carbon nanotube material is usedas a lithium ion battery negative electrode material, and the nitrogen-doped carbon nanotube material has large specific capacity and good cycling stability.

Description

technical field [0001] The invention relates to a nitrogen-doped carbon nanotube material, in particular to a carbon nanotube lithium battery negative electrode material doped with high nitrogen content, and provides a preparation method thereof, belonging to the technical field of nanocomposite materials and their applications. Background technique [0002] Carbon nanotubes are hollow cylinders formed by curling graphite layers, and its bonding method is mainly deformed Sp2 orbitals. When the graphite layer is rolled into carbon nanotubes, the Sp2 hybridization will be partially deformed, so Sp2 tends to form re-hybridization with Sp3. This re-hybridization structure and two-orbital confinement characteristics can endow carbon nanotubes with excellent mechanical, thermal, and thermal properties. Electrical, optical, magnetic and chemical properties. Therefore, carbon nanotubes have higher mechanical strength, better electrical and thermal conductivity, and higher chemical ...

Claims

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Application Information

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IPC IPC(8): C01B32/168H01M4/583H01M10/0525
CPCC01B32/168H01M4/583H01M10/0525C01B2202/36C01B2202/34C01B2202/32C01B2202/22Y02E60/10
Inventor 郭金廖莎张会成王少军凌凤香
Owner CHINA PETROLEUM & CHEM CORP
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