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High-specific surface active graphene with mesoporous and preparation method and application thereof

A high specific surface, graphene technology, applied in chemical instruments and methods, nanotechnology for materials and surface science, inorganic chemistry, etc., can solve the problem of excessive reaction, low production efficiency, and ineffective activation of activators and other problems to achieve the effect of reducing the difficulty of operation and improving production efficiency

Active Publication Date: 2012-12-19
THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the strong alkali reagent that this invention selects is the strong alkali aqueous solution of preparation, and concentration is 0.2-20mol / L, and the corrosion to equipment is serious, and operating procedure is loaded down with trivial details, and production efficiency is not high, and the graphene of high specific surface activity prepared is mostly for microporous
[0008] Moreover, in the prior art, the chemical activation method for preparing graphene with a large specific surface area is very difficult to control the selection and usage of the activator. Too strong activation ability leads to excessive activation of graphene, and often the desired product cannot be obtained. , and even cause excessive reaction due to too strong activation ability, generating salts of activator and carbon; and activators with poor activation ability often cannot achieve good activation effect, and cannot increase the specific surface area of ​​graphene.
[0009] In graphene with high specific surface activity, the pore size of graphene plays an important role in the electrical and chemical properties of graphene. If the pore size is too large, the integrity of graphene will be poor; if the pore size is too small, the specific surface activity of graphene will decrease. poor performance

Method used

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  • High-specific surface active graphene with mesoporous and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0053] A method utilizing phosphoric acid as an activator to prepare a high specific surface active graphene material with mesopores, comprising the following preparation steps:

[0054] Graphene is obtained by exfoliating graphite oxide by microwave, and 30g of graphene is weighed; phosphoric acid with a concentration of 85wt% and graphene are mixed and impregnated at a weight ratio of 3:1 for 2 days, and the impregnation temperature is 55°C; then the uniformly mixed raw materials are loaded into nickel In the reactor, after the reactor is closed, nitrogen is introduced to replace the air in the reactor, and the temperature is raised under the protection of nitrogen at a rate of 10-12°C / min, and the activation starts at 550°C, and the temperature is kept for 120min. After the reaction is completed, it is protected by nitrogen Lower the temperature to room temperature, take out the product, wash it with water, and dry it to make the product. Its BET specific surface area is 200...

Embodiment 2

[0056] A method utilizing phosphoric acid as an activator to prepare a high specific surface active graphene material with mesopores, comprising the following preparation steps:

[0057] Graphene is obtained by exfoliating graphite oxide by microwave, and 40g of graphene is weighed; phosphoric acid with a concentration of 85wt% and graphene are mixed and impregnated at 5:1 by weight for 20h, and the immersion temperature is 45°C; then the uniformly mixed raw materials are loaded into nickel In the reactor, after the reactor is closed, nitrogen gas is introduced to replace the air in the reactor, and the temperature is raised under the protection of nitrogen gas at a heating rate of 10-12°C / min to 450°C and dehydration at a constant temperature of 120min; then continue at a heating rate of 10- 12°C / min, heat up to 800°C, start activation, keep the temperature for 120min, after the reaction is completed, cool down to room temperature under the protection of nitrogen, take out the...

Embodiment 3

[0059] A method utilizing phosphoric acid as an activator to activate and prepare a high specific surface active graphene material with mesopores, comprising the following preparation steps:

[0060]Graphene is obtained by exfoliating graphite oxide by microwave, and 30g of graphene is weighed; phosphoric acid with a concentration of 85% and graphene are mixed and impregnated at a weight ratio of 4:1 for 1d, and the impregnation temperature is 50°C; then the uniformly mixed raw materials are loaded into nickel In the reactor, after the reactor is closed, argon is introduced to replace the air in the reactor, and the temperature is raised under the protection of argon at a rate of 10-12°C / min, and activation starts at 400°C, and the temperature is maintained for 120min. Cool down to room temperature under the protection of argon, take out the product, wash with water, and dry to make the product. The BET specific surface area is 1600m 2 / g, the pore volume is 1.0cm 3 / g, the a...

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Abstract

The invention relates to a preparation method of high specific surface active graphene with mesoporous. The method comprises the following steps of: carrying out mixing and impregnation on graphene obtained by stripping graphite oxide and phosphoric acid; then carrying out activation; and by washing, filtering and drying, obtaining the high specific surface active graphene with the mesoporous. The method belongs to the technical field of preparation of a graphene material. The method provided by the invention has simple process, low pollution, low carbonization temperature and low cost and has strong market competitiveness and wide application prospect; the active graphene material provided by the invention has large pore volume and average aperture and has good application prospect on the application aspects of energy storage and the like.

Description

technical field [0001] The invention relates to a preparation method of a high specific surface activity graphene material, in particular to a preparation method of a high specific surface activity graphene with mesopores, and belongs to the technical field of graphene material preparation. Background technique [0002] Graphene is a carbon atom with sp 2 The hexagonal honeycomb lattice planar film composed of hybrid orbitals, which is only one carbon atom thick, is the thinnest (thickness 0.335nm) but also the hardest (can withstand the pressure of about two tons of heavy objects) , without breaking) nanomaterials are considered to be the basic structural units of fullerenes, carbon nanotubes and graphite. [0003] Graphene is currently the hardest nanomaterial (tensile modulus E≈1.01TPa and ultimate strength σ≈130GPa), with high light transmittance (only absorbs 2.3% of light); high thermal conductivity (up to 5300W / m K) , Electron mobility (more than 15000cm 2 / V·s) hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04B82Y30/00C01B32/192
Inventor 李永锋
Owner THE SIXTH ELEMENT CHANGZHOU MATERIALS TECH
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