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A kind of preparation method of graphite oxide

A technology of graphite and graphite powder, which is applied in the field of preparation of graphite oxide, can solve the problems of low carbon and oxygen in graphite oxide and low degree of graphite oxidation, achieve significant economic and social benefits, and be conducive to popularization and application

Active Publication Date: 2017-01-25
鸡西市鼎源石墨有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Usually the oxidant used to prepare graphite oxide is KClO 4 , KMnO 4 , but there is a low degree of graphite oxidation, and the prepared graphite oxide has a low carbon-oxygen ratio.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] A kind of preparation method of graphite oxide comprises the following steps:

[0016] 1) Mix 350 mg of graphite powder, 350 mg of sodium nitrate and 20 ml of concentrated sulfuric acid, and ultrasonically disperse at 10°C for 18 minutes;

[0017] 2) Slowly add 2.5 grams of oxidizing agent, and then ultrasonically disperse for 5 minutes;

[0018] 3) Stir in a water bath at 40°C for 2 hours, and slowly add 18 ml of deionized water dropwise during the stirring process;

[0019] 5) Stir in a 90°C water bath for 25 minutes;

[0020] 5) Add 100 ml of 3vol.% hydrogen peroxide, wash with 1M hydrochloric acid, add deionized water, centrifuge and wash until neutral, vacuum dry at 80°C for 12 hours, and grind to obtain brown graphite oxide powder.

[0021] The oxidizing agent is chromium trioxide bipyridine and chromium trioxide pyridine hydrochloride in a weight ratio of 1:1.

[0022] The carbon to oxygen ratio (weight ratio) of the prepared graphite oxide was 12.

Embodiment 2

[0024] A kind of preparation method of graphite oxide comprises the following steps:

[0025] 1) Mix 200 mg of graphite powder, 200 mg of sodium nitrate and 10 ml of concentrated sulfuric acid, and ultrasonically disperse at 10°C for 15 minutes;

[0026] 2) Slowly add 2 grams of oxidizing agent, and then ultrasonically disperse for 5 minutes;

[0027] 3) Stir in a water bath at 30°C for 2 hours, and slowly add 15 ml of deionized water dropwise during the stirring process;

[0028] 6) Stir in a 90°C water bath for 20 minutes;

[0029] 5) Add 100 ml of 3vol.% hydrogen peroxide, wash with 1M hydrochloric acid, add deionized water, centrifuge and wash until neutral, vacuum dry at 80°C for 12 hours, and grind to obtain brown graphite oxide powder.

[0030] The oxidizing agent is chromium trioxide dipyridine.

[0031] The carbon to oxygen ratio (weight ratio) of the prepared graphite oxide was 12.

Embodiment 3

[0033] A kind of preparation method of graphite oxide comprises the following steps:

[0034] 1) Mix 500 mg of graphite powder, 500 mg of sodium nitrate and 30 ml of concentrated sulfuric acid, and ultrasonically disperse at 10°C for 20 minutes;

[0035] 2) Slowly add 3 grams of oxidizing agent, and then ultrasonically disperse for 5 minutes;

[0036] 3) Stir in a water bath at 50°C for 2 hours, and slowly add 20 ml of deionized water dropwise during the stirring process;

[0037] 7) Stir in a 90°C water bath for 30 minutes;

[0038] 5) Add 100 ml of 3vol.% hydrogen peroxide, wash with 1M hydrochloric acid, add deionized water, centrifuge and wash until neutral, vacuum dry at 80°C for 12 hours, and grind to obtain brown graphite oxide powder.

[0039] The oxidizing agent is chromium trioxide pyridine hydrochloride.

[0040] The carbon to oxygen ratio (weight ratio) of the prepared graphite oxide was 12.

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PUM

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Abstract

The invention discloses a preparation method of graphite oxide. The preparation method is to use dipyridine chromium oxide and / or pyriddinium chlorochromate to substitute oxidizing agents KClO4 and KMnO4 used in the existing graphite oxide preparation process, so as to prepare the graphite oxide with a high carbon-oxygen ratio. The preparation method provides an excellent raw material for preparing the high-performance graphene, is beneficial to promote and apply, and is excellent in economic benefits and social benefits.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a preparation method of graphite oxide. Background technique [0002] As a new nano-scale carbon material, graphene has many excellent properties, and its unique properties originate from sp 2 A hybrid two-dimensional single-layer graphite structure, which endows graphene with many special physical and chemical properties, such as high electron mobility, high transparency, flexible structure and huge theoretical specific surface area, etc. At present, the method of reducing graphite oxide is usually used to prepare graphene. Therefore, the quality of graphite oxide directly determines the quality of the prepared graphene. Usually the oxidant used to prepare graphite oxide is KClO 4 , KMnO 4 , but there is a low degree of graphite oxidation, and the prepared graphite oxide has a low carbon-oxygen ratio. Contents of the invention [0003] The object of the pres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04
Inventor 王仁章牛玉李福颖
Owner 鸡西市鼎源石墨有限公司