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Preparation method of graphite oxide

A technology of graphite and flake graphite is applied in the field of preparation of graphite oxide to achieve the effect of safe and simple operation and low equipment requirements

Inactive Publication Date: 2014-10-29
SUZHOU SHIYOUJIA ELECTRONICS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the Hummers method also has many disadvantages, such as: water needs to be added to the concentrated sulfuric acid dispersion, this step is in conflict with the safe operation in basic inorganic chemistry, and it is quite dangerous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 40mL of concentrated sulfuric acid to a dry beaker, cool it to below 10°C with ice water, add 2g flake graphite and 1gNaNO under constant stirring with a magnetic stirring bar 3 The solid mixture, and then slowly add 6g powder potassium permanganate, while controlling the reaction temperature below 20 ° C; 4 After the addition, remove the water bath, wait until the temperature rises to 35°C, strictly control the temperature at about 35°C and continue to stir for 30 minutes; slowly add 92mL of deionized water, continue to stir for 15min; then add 142ml of deionized water to dilute, and react at room temperature 12h, then add a certain amount of hydrogen peroxide with a mass fraction of 30% to reduce the residual oxidizing agent, continue for several minutes, and the solution becomes bright yellow;

[0022] Centrifuge while hot to obtain a yellowish-brown residue; wash with 5% HCl solution and deionized water for 3 times, and centrifuge once for each wash, with the sp...

Embodiment 2

[0024] Add 46mL of concentrated sulfuric acid to a dry beaker, cool it down to below 10°C with ice water, add 2g flake graphite and 1gNaNO under constant stirring with a magnetic stirring bar 3 The solid mixture, and then slowly add 6g powder potassium permanganate, while controlling the reaction temperature below 20 ° C; 4 After the addition, remove the water bath, wait until the temperature rises to 35°C, strictly control the temperature at about 35°C and continue to stir for 30 minutes; slowly add 92mL of deionized water, continue to stir for 15min; then add 142ml of deionized water to dilute, and react at room temperature 12h, then add a certain amount of hydrogen peroxide with a mass fraction of 30% to reduce the residual oxidant, and last for a few minutes, the solution turns bright yellow; centrifuge while it is hot to obtain a yellow-brown residue; use a volume fraction of 5% HCl solution and remove Wash with ionic water for 3 times, centrifuge once for each wash, cont...

Embodiment 3

[0026] Add 50mL of concentrated sulfuric acid to a dry beaker, cool it down to below 10°C with ice water, add 2g of flake graphite and 1g of NaNO under constant stirring with a magnetic stirring bar 3 The solid mixture, and then slowly add 6g powder potassium permanganate, while controlling the reaction temperature below 20 ° C; 4 After the addition, remove the water bath, wait until the temperature rises to 35°C, strictly control the temperature at about 35°C and continue to stir for 30 minutes; slowly add 92mL of deionized water, continue to stir for 15min; then add 142ml of deionized water to dilute, and react at room temperature 12h, then add a certain amount of hydrogen peroxide with a mass fraction of 30% to reduce the residual oxidant, and last for a few minutes, the solution turns bright yellow; centrifuge while it is hot to obtain a yellow-brown residue; use a volume fraction of 5% HCl solution and remove Wash with ionic water for 3 times, centrifuge once for each was...

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Abstract

The invention discloses a preparation method of graphite oxide. The preparation method comprises the steps: adding concentrated sulfuric acid in a dry beaker, cooling with ice water, adding a solid mixture of flake graphite and NaNO3 under constant stirring, and then slowly adding a potassium permanganate powder; after finishing addition of KMnO4, removing the water bath, and continuing stirring; slowly adding deionized water, stirring, then adding deionized water for dilution, carrying out a reaction under a condition of normal temperature, then adding hydrogen peroxide, reducing a residual oxidant until the solution becomes bright yellow, and then centrifuging to obtain a yellow-brown residue; respectively washing by an HCl solution and deionized water for 3 times, and centrifuging for one time after each washing until the filtrate is neutral; and finally placing the filter cake in a 60 DEG C drying box, and fully drying. The preparation method is safe and simple in operation and low in equipment requirements, can prepare graphite oxide with relatively high carbon-oxygen ratio; and moreover, the graphite oxide prepared by the method can be used for preparing graphene, and graphene is further applied in battery materials, composite materials, electronic devices, energy storage materials and other fields.

Description

[0001] technical field [0002] The invention relates to the field of graphite, in particular to a preparation method of graphite oxide. Background technique [0003] Graphene is an emerging nanocarbon material in the same family as carbon nanotubes and fullerenes. After it was discovered in 2004 and existed stably, it immediately became a research hotspot in various fields. It has a two-dimensional structure of carbon arranged in a honeycomb shape, and is stabilized by the repulsive force generated by the electron clouds on both sides. Due to its excellent mechanical, electrical, thermal and optical properties, it has broad application prospects in multiple fields such as battery materials, composite materials, electronic devices, and energy storage materials. [0004] The preparation of graphene has always been the focus of attention. The preparation methods that have been reported so far mainly include mechanical exfoliation method, epitaxial growth method, chemical va...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 陈鑫
Owner SUZHOU SHIYOUJIA ELECTRONICS TECH
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