Preparation method of graphene

A graphene and graphite technology, applied in the field of graphene preparation, can solve the problems of high toxicity of reducing agents, environmental and human hazards, and limited use, and achieve the effects of easy operation, promotion of stripping, and low energy consumption

Inactive Publication Date: 2012-11-07
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The chemical reduction method is considered to be an effective method for mass production of graphene. Commonly used reducing agents include hydrazine hydrate and hydroquinone, etc., but these reducing agents are extremely toxic and have great harm to the environment and human body, which limits the its use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Under ice-water bath conditions, 3 g of graphite was slowly added to 120 mL of concentrated sulfuric acid with a mass fraction of 98% under stirring, and 15 g of potassium permanganate was slowly added, at 35 o C constant temperature water bath, keep stirring for 2 h, after the reaction, slowly add 500 mL of deionized water to dilute, stir for a few minutes, add 22.5 mL of 30% H 2 o 2 , filtered after standing, fully washed the filter cake until neutral, and dried at room temperature to obtain graphite oxide. At room temperature, mix pyridine and ethanol at a volume ratio of 1:1, graphite oxide is mixed in the above solution, the concentration of graphite oxide in the above mixed solution is 2 mg / mL, ultrasonically disperse for 30 min, and transfer the dispersion to into the autoclave at 120 o C was heated and reacted for 48 h to obtain graphene. Wash with deionized water, wash with absolute ethanol, and dry to obtain graphene. After nitrogen adsorption and desorpti...

Embodiment 2

[0016] Under ice-water bath conditions, 3 g of graphite was slowly added to 120 mL of concentrated sulfuric acid with a mass fraction of 98% under stirring, and 15 g of potassium permanganate was slowly added, at 35 o C constant temperature water bath, keep stirring for 2 h, after the reaction, slowly add 500 mL of deionized water to dilute, stir for a few minutes, add 22.5 mL of 30% H 2 o 2 , filtered after standing, fully washed the filter cake until neutral, and dried at room temperature to obtain graphite oxide. At room temperature, mix pyridine and ethylene glycol at a volume ratio of 1:5, graphite oxide is mixed in the above solution, the concentration of graphite oxide in the above mixed solution is 6 mg / mL, ultrasonically disperse for 45 min, and then disperse The liquid is transferred to the autoclave at 150 o C is heated and reacted for 12 h to obtain graphene. Wash with deionized water, wash with absolute ethanol, and dry to obtain graphene. After nitrogen adsor...

Embodiment 3

[0018] Under ice-water bath conditions, 3 g of graphite was slowly added to 120 mL of concentrated sulfuric acid with a mass fraction of 98% under stirring, and 15 g of potassium permanganate was slowly added, at 35 o C constant temperature water bath, keep stirring for 2 h, after the reaction, slowly add 500 mL of deionized water to dilute, stir for a few minutes, add 22.5 mL of 30% H 2 o 2 , filtered after standing, fully washed the filter cake until neutral, and dried at room temperature to obtain graphite oxide. At room temperature, mix pyridine and benzyl alcohol at a volume ratio of 1:10, graphite oxide is mixed in the above solution, the concentration of graphite oxide in the above mixed solution is 10 mg / mL, ultrasonically disperse for 60 min, and then the dispersion transferred to an autoclave at 200 o C was heated and reacted for 24 h to obtain graphene. Wash with deionized water, wash with absolute ethanol, and dry to obtain graphene. After nitrogen adsorption a...

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Abstract

The invention belongs to the technical field of carbon material manufacturing techniques, and relates to a preparation method of graphene. The preparation method comprises the following steps: mixing pyridine and alcohol organic solvent in a ratio of 1:10-1:1 at room temperature, wherein the alcohol organic solvent can be any one or combination of methanol, ethanol, benzyl alcohol and the like; carrying out ultrasonic dispersion on graphite oxide in the mixed solution, wherein the concentration of the graphite oxide in the mixed solution is 1-8 mg/mL; transferring the dispersed solution into a high-pressure reaction kettle; and heating to 120-200 DEG C to react for 12-48 hours, thereby obtaining the graphene. The graphene prepared by the method provided by the invention has the advantages of high degree of reduction and large specific area, and avoids using any high-toxicity reducer. The graphene prepared by the method provided by the invention can be widely used in the fields of supercapacitors, capacitor type desalting and the like.

Description

technical field [0001] The invention belongs to the technical field of carbon material manufacturing technology, and relates to a preparation method of graphene. The graphene prepared by the invention can be widely used in the fields of supercapacitors, capacitive desalination, lithium ion batteries and the like. Background technique [0002] As a new type of two-dimensional honeycomb structure carbon material, graphene has good electrical conductivity (7200 S / m), large theoretical specific surface area (2600 m 2 / g), high mechanical stability and other superior properties, it has attracted widespread attention. At present, the methods for preparing graphene mainly include: (1) micromechanical exfoliation method, such as Andre et al., University of Manchester, United Kingdom, prepared graphene by adhesive tape method, although this method can obtain high-quality few-layer graphene , but the low yield and cumbersome process limit its use; (2) chemical vapor deposition m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/192
Inventor 张登松施利毅王慧颜婷婷温晓茹张剑平
Owner SHANGHAI UNIV
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