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Method for preparing doped graphene from supercritical fluid

A supercritical fluid and supercritical flow technology, applied in the field of graphene, can solve the problems of high magazine content, large equipment investment, cumbersome steps, etc., and achieve the effects of simple process, low environmental pollution, and few production equipment.

Inactive Publication Date: 2016-03-02
FUJIAN XFH NEW ENERGY MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the first three schemes can produce high-quality graphene, the investment in equipment is large and the cost is high; while the liquid phase redox method is relatively low in cost, but the steps are cumbersome, the content of impurities is high, and a large amount of strong alkali is used. , strong oxidizing, strong reducing substances, serious environmental pollution

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  • Method for preparing doped graphene from supercritical fluid

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Effect test

Embodiment 1

[0021] A method for preparing doped graphene by supercritical fluid, comprising the steps of:

[0022] 1) preparation of graphene oxide:

[0023] Add graphite into the mixture of strong oxidizing acid and nitrate, after mixing evenly, add a strong oxidizing agent containing potassium, raise the temperature of the system to 35°C, and continue stirring for 12 hours, then slowly add a certain amount of water, raise the temperature of the system to 80°C and Keep it for 30 minutes, then add water and a certain amount of hydrogen peroxide, after fully stirring the reaction, wash repeatedly with dilute acid solution and deionized water to remove various ions in the system, and then collect the solid by vacuum drying to obtain graphene oxide; The mass ratio of reactants is strong oxidizing acid: nitrate: potassium-containing strong oxidizing agent: hydrogen peroxide: graphite=10:5:2:5:1.

[0024] 2) Preparation of doped graphene

[0025] Put the graphene oxide obtained above and the...

Embodiment 2

[0030] A method for preparing doped graphene by supercritical fluid, comprising the steps of:

[0031] 1) preparation of graphene oxide:

[0032] Add graphite into the mixture of strong oxidizing acid and nitrate, after mixing evenly, add a strong oxidizing agent containing potassium, raise the temperature of the system to 40°C, and continue stirring for 4 hours, then slowly add a certain amount of water, raise the temperature of the system to 60°C and Keep it for 60 minutes, then add water and a certain amount of hydrogen peroxide, after fully stirring the reaction, wash repeatedly with dilute acid solution and deionized water to remove various ions in the system, and then collect the solid by vacuum drying to obtain graphene oxide; The mass ratio of reactants is strong oxidizing acid: nitrate: potassium-containing strong oxidizing agent: hydrogen peroxide: graphite=40:1:8:1:1.

[0033] 2) Preparation of doped graphene

[0034] Put the graphene oxide obtained above and the ...

Embodiment 3

[0039] A method for preparing doped graphene by supercritical fluid, comprising the steps of:

[0040] 1) preparation of graphene oxide:

[0041] Add graphite into the mixture of strong oxidizing acid and nitrate, after mixing evenly, add a strong oxidizing agent containing potassium, raise the temperature of the system to 36°C, and continue stirring for 8 hours, then slowly add a certain amount of water, raise the temperature of the system to 70°C and Keep it for 50 minutes, then add water and a certain amount of hydrogen peroxide, after fully stirring the reaction, wash repeatedly with dilute acid solution and deionized water to remove various ions in the system, and then collect the solid by vacuum drying to obtain graphene oxide; The mass ratio of reactants is strong oxidizing acid: nitrate: potassium-containing strong oxidizing agent: hydrogen peroxide: graphite=20:3:5:4:1.

[0042] 2) Preparation of doped graphene

[0043] Put the graphene oxide obtained above and the ...

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Abstract

The invention discloses a method for preparing doped graphene from supercritical fluid. The method includes the following steps:1, preparation of graphene oxide, wherein graphite is added to a mixture of strong oxidizing acid and nitrate, after uniform mixing is conducted, strong oxidant containing potassium is added, water and a certain amount of hydrogen peroxide are added, after a full stirring reaction is conducted, cleaning is conducted repeatedly through a dilute acid solution and deionized water, various ions in a system are removed, then solid is collected through vacuum drying, and the graphene oxide is obtained; 2, preparation of the doped graphene, wherein after the obtained graphene oxide and an active doped element compound are premixed, a reaction is conducted in a supercritical state, and the element doped graphene is obtained. The reaction process is simple, the price is low, and emission of poisonous gas and solvent is avoided; a product has excellent electrochemical performance, and the doped graphene can be used for lithium ion batteries, lithium air batteries, super capacitor electrode materials and novel energy battery materials, such as fuel cell oxygen reduction catalysts.

Description

technical field [0001] The invention relates to the technology in the field of graphene, and in particular provides a method for preparing doped graphene through a supercritical fluid. Background technique [0002] The preparation method of graphene has always been a hot issue that people pay attention to. At present, the main synthesis methods include mechanical exfoliation method, epitaxial growth method, chemical vapor phase deposition and liquid phase redox method. Although the first three schemes can produce high-quality graphene, the investment in equipment is large and the cost is high; while the liquid phase redox method is relatively low in cost, but the steps are cumbersome, the content of impurities is high, and a large amount of strong alkali is used. , Strong oxidizing, strong reducing substances, serious environmental pollution. Supercritical fluid is a clean, non-polluting, cheap and highly efficient dispersion medium with abundant sources. Contents of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCY02P20/54
Inventor 李芳赵东辉戴涛周鹏伟
Owner FUJIAN XFH NEW ENERGY MATERIALS CO LTD
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