Method for preparing graphene oxide by chemical peeling

A graphene and fossil technology, applied in the field of chemical exfoliation to prepare graphene oxide, can solve problems such as harsh preparation conditions and difficult operation, and achieve the effects of realizing large-scale industrial production, improving production efficiency and high yield

Inactive Publication Date: 2011-09-07
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires harsh preparation

Method used

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  • Method for preparing graphene oxide by chemical peeling
  • Method for preparing graphene oxide by chemical peeling
  • Method for preparing graphene oxide by chemical peeling

Examples

Experimental program
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Effect test

Embodiment 1

[0028] (1) Preparation of graphite oxide

[0029] Take 0.1g of expanded graphite and 10mL of concentrated sulfuric acid and mix evenly in an ice-water bath, then slowly add 0.6g of potassium permanganate, and then react in a water bath at 30°C for 0.25h, then add 40mL of distilled water to react for 0.5h, and then Add 5mL of 30wt% hydrogen peroxide, stir for 0.5h, and centrifuge with 5wt% hydrochloric acid solution until it no longer contains SO 4 2- Ions (with 5wt%Ba(NO 3 ) 2 solution detection), and then washed with distilled water until neutral, that is, a dark red viscous graphite oxide filter cake was obtained; the filter cake was washed down with absolute ethanol, dried in an oven at 50°C, and black graphite oxide was obtained;

[0030] (2) Preparation of graphene oxide

[0031] Add 0.02g of graphite oxide into 15mL of ethylene glycol solution, disperse at 40kHz ultrasonic frequency for 0.5h, then centrifuge at 3000rpm for 20min, pour out the upper suspended solution...

Embodiment 2

[0033] (1) Preparation of graphite oxide

[0034] Take 0.5g of expanded graphite and 60mL of concentrated sulfuric acid and mix evenly in an ice-water bath, then slowly add 12g of potassium permanganate, react in a water bath at 35°C for 1 hour, then add 200mL of distilled water for 2 hours, then add 15mL of 30wt% hydrogen peroxide, stirred for 1h, then centrifuged and washed with 5wt% hydrochloric acid solution until it no longer contains SO 4 2- Ions (with 5wt%Ba(NO 3 ) 2 solution detection), and then washed with distilled water until neutral, and a dark red viscous graphite oxide filter cake was obtained. Rinse down the filter cake with absolute ethanol and dry it in an oven at 70°C to obtain black graphite oxide;

[0035] (2) Preparation of graphene oxide

[0036] Add 0.05g of graphite oxide to 50mL of N,N-dimethylformamide solution, disperse at 50kHz ultrasonic frequency for 3h, then centrifuge at 5000rpm for 60min, and pour off the upper suspension solution , place...

Embodiment 3

[0040] (1) Preparation of graphite oxide

[0041] Take 0.2g of expanded graphite and mix evenly with 10mL of concentrated sulfuric acid, then slowly add 10mL of concentrated nitric acid, and keep stirring. Next, 5 g of potassium permanganate was slowly added, and reacted in a water bath at 38° C. for 2 h. Then add 100mL of distilled water to react for 1h, then add 5mL of 30wt% hydrogen peroxide, stir for 2h, and centrifuge with 5wt% hydrochloric acid solution until it no longer contains SO 4 2- Ions (with 5wt%Ba(NO 3 ) 2 solution detection), and then washed with distilled water until neutral, and a dark red viscous graphite oxide filter cake was obtained. Rinse down the filter cake with absolute ethanol and dry it in an oven at 65°C to obtain black graphite oxide;

[0042] (2) Preparation of graphene oxide

[0043] Take 0.08g of graphite oxide and add it to 60mL of ethanol solution, disperse it at an ultrasonic frequency of 40kHz for 4h, then centrifuge at a speed of 400...

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Abstract

The invention relates to a method for preparing graphene oxide by chemical peeling, belonging to the field of graphene oxide preparation. The method comprises the following steps: (1) graphite oxide preparation: selecting expanded graphite, strong acid, oxidant and distilled water according to the proportion of (0.1-0.8g):(10-90ml):(0.6-12g):(40-300ml); mixing the expanded graphite with the strong acid evenly, adding oxidant and then carrying out a reaction on the mixture for 0.25-4 hours in a condition of 30-45 DEG C; adding distilled water to react for 0.5-2.5 hours and washing the filter cake to neutral with distilled water; rinsing the filter cake with absolute ethyl alcohol, drying the cake in a condition of 30-45 DEG C to obtain the graphite oxide. (2) graphene oxide preparation: selecting the graphite oxide and organic solvent according to the proportion of (0.02-0.1g):(15-70ml); adding the graphite oxide to the solvent and dispersing with a 40-50kHz ultrasonic sound for 0.5-10 hours; centrifugating at a rate of 3000-5000r/min for 20-90 minutes; taking the suspension solution and drying in a condition of 30-45DEG C to obtain the graphene oxide. The method in the invention is safe in operation and has low costs.

Description

technical field [0001] The invention belongs to a preparation method of graphene oxide, in particular to a method for preparing graphene oxide by chemical exfoliation. Background technique [0002] Graphene is a new carbonaceous material with a two-dimensional honeycomb lattice structure formed by a single layer of carbon atoms tightly packed. It is considered to be the basic structural unit of fullerene, carbon nanotube (CNT) and graphite. Because of its special mechanical, quantum and electrical properties, it has become the most active research frontier in the field of materials science and condensed matter physics. The typical conduction rate of electrons in graphene is 8×10 5 m / s, although this is much slower than the speed of light, it is much faster than the electron conduction speed in general semiconductors. In addition to excellent electrical properties, the tensile modulus (1.01TPa) and ultimate strength (116GPa) of graphene are comparable to single-walled carbo...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 李珍李飞王增奎沈毅马海晶杜城
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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