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Nitrogen-doped graphene and preparation method thereof

A nitrogen-doped graphene and graphite technology, applied in graphene, chemical instruments and methods, nano-carbon, etc., can solve the problems of limiting energy storage performance and limited amount of nitrogen doping.

Inactive Publication Date: 2014-08-20
OCEANS KING LIGHTING SCI&TECH CO LTD +2
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  • Abstract
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  • Application Information

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Problems solved by technology

Among them, nitrogen-doped graphene has greatly improved its energy storage performance due to the incorporation of nitrogen (nitrogen replaces carbon atoms on graphene), but according to current reports, the amount of nitrogen doped in graphene is limited, which greatly limits the energy storage performance. improved performance

Method used

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  • Nitrogen-doped graphene and preparation method thereof

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preparation example Construction

[0019] Such as figure 1 Shown, the preparation method of the nitrogen-doped graphene of one embodiment, comprises the steps:

[0020] Step S110: using graphite to prepare graphite oxide.

[0021] Using graphite to prepare graphite oxide can be prepared by conventional methods. Preferably, the step of using graphite to prepare graphite oxide includes:

[0022] According to mass volume ratio is 0.5 gram~1.5 gram: 110ml~120ml, graphite is added in the mixed solution that is made up of concentrated sulfuric acid and concentrated nitric acid, and be placed in ice-water mixed bath and stir and mix, form mixed solution; And

[0023] According to the mass ratio of graphite to potassium permanganate is 0.5~1.5:3~12, add potassium permanganate into the mixed solution, stir for 0.5 hours to 3 hours for intercalation reaction, then heat to 25°C~45°C to keep warm React for 10 minutes to 40 minutes, then add deionized water, then heat to 60°C~95°C and keep it warm for 10 minutes to 40 min...

Embodiment 1

[0055] The preparation of the nitrogen-doped graphene of the present embodiment is as follows:

[0056] (1) Add 1 g of graphite (99.5% by mass) to a mixture of 90 ml of concentrated sulfuric acid with a mass fraction of 98% and 25 ml of concentrated nitric acid with a mass fraction of 65%, and place it in an ice-water mixing bath Stir and mix for 20 minutes to form a mixed solution.

[0057] (2) Slowly add 6g of potassium permanganate into the mixed solution, stir for 1 hour for intercalation reaction, then heat to 25°C for 40 minutes, then add 92ml of deionized water, then heat to 85°C for 30 minutes Minutes to obtain the reaction solution, add 10ml hydrogen peroxide (mass fraction: 30%) to the reaction solution to remove potassium permanganate, the filter residue through suction filtration is washed three times with 100ml of dilute hydrochloric acid and 150ml of deionized water successively, and then Dry in a vacuum oven at 60°C for 12 hours to obtain graphite oxide.

[00...

Embodiment 2

[0061] The preparation of the nitrogen-doped graphene of the present embodiment is as follows:

[0062] (1) Add 0.5g of graphite (mass fraction 99.5%) to a mixture of 85 ml of concentrated sulfuric acid with a mass fraction of 98% and 25 ml of concentrated nitric acid with a mass fraction of 65%, and place in an ice-water mixing bath Stir and mix for 20 minutes to form a mixed solution.

[0063] (2) Slowly add 3g of potassium permanganate into the mixed solution, stir for 1 hour for intercalation reaction, then heat to 35°C for 30 minutes, then add 92ml of deionized water, then heat to 60°C for 40 minutes Minutes to obtain the reaction solution, add 10ml hydrogen peroxide (mass fraction: 30%) to the reaction solution to remove potassium permanganate, the filter residue through suction filtration is washed three times with 100ml of dilute hydrochloric acid and 150ml of deionized water successively, and then Dry in a vacuum oven at 40°C for 16 hours to obtain graphite oxide.

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Abstract

The invention relates to a preparation method for nitrogen-doped graphene. The method comprises the steps of: preparing graphite oxide from graphite; adding the graphite oxide into deionized water, conducting ultrasonic treatment, then adding aniline and carrying out ultrasonic mixing, thus obtaining a suspending solution; at a temperature of 0DEG C-10DEG C, adding hydrochloric acid into the suspending solution till the pH value of the suspending solution reaches 3-5, then adding benzoyl peroxide, carrying out polymerization reaction under stirring for 12h-20h, and then performing filtering, washing and drying to obtain a graphene oxide-polyaniline mixture; and in an oxygen-free atmosphere, subjecting the graphene oxide-polyaniline mixture to heating and heat preservation reaction, and conducting cooling, thus obtaining the nitrogen-doped graphene. The nitrogen-doped grapheme prepared by the method provided by the invention has a high nitrogen content. In addition, the invention also relates to a nitrogen-doped graphene.

Description

technical field [0001] The invention relates to the field of material synthesis, in particular to a nitrogen-doped graphene and a preparation method thereof. Background technique [0002] Due to its unique two-dimensional monolayer structure and excellent physical properties (high theoretical specific surface area, high electrical conductivity, high mechanical properties, etc.), graphene has received extensive attention from various fields since it was prepared in 2004. Its appearance has had a huge impact on the field of materials, and at the same time it has brought great opportunities and challenges to materials researchers. I believe that in the next few years it will bring a revolution to the field of materials and people's lives Bring many products with excellent performance. Due to the monolayer of graphene, its theoretical capacity can reach 2630m 2 / g, has broad application prospects in lithium-ion batteries and supercapacitor electrode materials, and there are re...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/19
CPCC01B31/0476C01B32/192
Inventor 周明杰钟辉王要兵刘大喜
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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