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Nitrogen-doped graphene material

A technology of nitrogen-doped graphene and graphene, which is applied in nanotechnology for materials and surface science, active material electrodes, electrical components, etc., and can solve problems such as low product utilization, complicated and time-consuming operations, and difficulties in obtaining raw materials , to simplify the production process, easy to store, and good stability

Active Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems in the preparation of nitrogen-doped graphene materials in the prior art, there are complex equipment, cumbersome process, complicated and time-consuming operation, low product utilization rate, difficulty in obtaining raw materials, and the nitrogen doping content caused by the large loss of nitrogen-doped precursors during the nitrogen-doping process. Low-level problems, the present invention provides an efficient, fast, large-scale method for synthesizing high-nitrogen-doped graphene materials, the nitrogen content of the obtained nitrogen-doped graphene is high, the utilization rate of raw materials is significantly improved, and the product does not need processes such as washing, separation, and drying , can be directly used as lithium battery anode material, with good application performance

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Weigh 1.0g of graphene oxide and disperse it in 20mL of 37% formaldehyde aqueous solution, place it in an ultrasonic instrument and disperse evenly, record it as dispersion A.

[0038] (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.

[0039] (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.

[0040] (4) Put the black solid powder obtained in step (3) into a microwave reaction chamber, and purging with argon gas a...

Embodiment 2

[0042] (1) Weigh 1.0g graphene oxide and disperse it in 30mL 37% formaldehyde aqueous solution, place it in an ultrasonic instrument and disperse evenly, record it as dispersion liquid A.

[0043] (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.

[0044] (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.

[0045] (4) Put the black solid powder obtained in step (3) into a microwave reaction chamber, and purging with argon gas ...

Embodiment 3

[0047] (1) Weigh 1.0g graphene oxide and disperse it in 30mL 37% formaldehyde aqueous solution, place it in an ultrasonic instrument and disperse evenly, record it as dispersion liquid A.

[0048] (2) Weigh 10.0g 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.

[0049] (3) Mix Dispersion A and Dispersion B, raise the temperature of the water bath to 70°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.

[0050] (4) Put the black solid powder obtained in step (3) into a microwave reaction chamber, and purging with argon gas...

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Abstract

The invention relates to a nitrogen-doped graphene material, which is prepared by the following steps: taking formaldehyde as a bridge, and carrying out moderate crosslinking on the formaldehyde and melamine to form a nitrogen-doped precursor; carrying out hydrothermal reaction to make the nitrogen-doped precursor and graphene interacted and uniformly fused; and carrying out solvent-free microwavereaction to synthesize high-nitrogen-content doped graphene. In the preparation process of the nitrogen-doped graphene material, the loss caused by sublimation of the nitrogen-doped precursor in theheating process in the traditional nitrogen doping process is avoided, and the nitrogen doping efficiency is improved; and the reaction conditions are progressively increased from mild to intense, anduniform fusion of interaction of the nitrogen-doped precursor and the graphene is realized. The prepared nitrogen-doped graphene material is good in stability, not prone to denaturation in air, easyto store and large in specific surface area; a good channel is provided for lithium ion transmission when the nitrogen-doped graphene material serves as a lithium ion battery negative electrode material; and the nitrogen-doped graphene material has large specific capacity and good cycling stability.

Description

technical field [0001] The invention relates to a nitrogen-doped graphene material, in particular to a graphene 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] Graphene is a two-dimensional honeycomb lattice structure carbonaceous material that is tightly packed by a single layer of carbon atoms. Since the discovery by Andre K. Geim of the University of Manchester in 2004, graphite Enenes have received great attention in both experimental and theoretical sciences. Graphene is only one carbon atom thick, making it the thinnest known material, yet extremely strong and hard, stronger than diamond and 100 times stronger than the world's hardest steel. Due to its special nanostructure and excellent performance, it has potential application prospects in the fields of catalysis, lithium storage, c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/587H01M10/0525B82Y30/00
CPCH01M4/587H01M10/0525B82Y30/00H01M2004/021H01M2004/027Y02E60/10
Inventor 郭金王少军凌凤香张会成廖莎
Owner CHINA PETROLEUM & CHEM CORP
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