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Method for preparing grapheme through oxidation reduction

A technology of graphene and graphite, which is applied in the field of redox preparation of graphene, can solve problems such as serious agglomeration, reduction effect is not as good as hydrazine hydrate, and toxicity limits popularization and application, and achieves low production cost, safe preparation method and environmental friendliness, Inexpensive effect

Active Publication Date: 2012-06-20
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reducing agents currently used mainly include hydrazine hydrate, sodium borohydride, p-phenylenediamine, etc. Although these reducing agents can effectively reduce graphite oxide, their huge toxicity limits the promotion and application
Recently, some people have successively used green oxidants such as ascorbic acid, glucose, citric acid, amino acids, sulfides, etc., but their reduction effect is not as good as hydrazine hydrate, and the agglomeration is serious

Method used

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  • Method for preparing grapheme through oxidation reduction
  • Method for preparing grapheme through oxidation reduction
  • Method for preparing grapheme through oxidation reduction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Preparation of graphite oxide:

[0028] Get 1g (83 mesh) natural flake graphite and 50ml mass concentration is 98% sulfuric acid after mixing evenly, add 1.0g potassium nitrate, add 6g potassium permanganate rapidly in the water bath of 15 ℃, mix well, add the potassium permanganate The process maintains the system temperature at 0-20°C. Then the temperature of the system was raised to 40°C, reacted for 3h, then added 30ml of water, and simultaneously raised the temperature of the system to 80°C for 30min, then reduced the excess potassium permanganate with 50ml of distilled water and 10ml of hydrogen peroxide (30wt%), and centrifugally washed to The pH was 5, and the graphite oxide solid was obtained by vacuum drying at 40°C. XRD characterization as figure 1 As shown in curve b, the interlayer distance of graphite oxide can be obtained to be 0.863nm, which is greatly increased compared with the interlayer distance of 0.34nm of initial graphite (a), indicating that...

Embodiment 2

[0034] 1) Preparation of graphite oxide:

[0035] Get 1g (83 mesh) natural flake graphite and 45ml mass concentration is 98% sulfuric acid after mixing uniformly, add 1.2g potassium nitrate, add 3g potassium permanganate rapidly in the water bath of 10 ℃, mix uniformly, add potassium permanganate The process maintains the system temperature at 0-20°C. Then the temperature of the system was raised to 50° C., reacted for 2 hours, then added 50 ml of water, and the system was heated to 90° C. for 20 minutes, and then the excess potassium permanganate was reduced with 100 ml of distilled water and 6 ml of hydrogen peroxide (30 wt %), and centrifugally washed to The pH was 6, and the graphite oxide solid was obtained by vacuum drying at 60°C. Similar to the characterization results of Example 1, the interlayer distance obtained by XRD analysis is 0.853 nm, which indicates that the graphite oxide has a good oxidation effect.

[0036] 2) Preparation of graphene oxide suspension:

...

Embodiment 3

[0041] 1) Preparation of graphite oxide:

[0042] Take 1g (16 mesh) of natural flake graphite and 40ml of mass concentration of 98% sulfuric acid and mix evenly, add 1.5g of potassium nitrate, quickly add 6g of potassium perchlorate in a water bath at 5°C, mix well, and maintain the temperature of the system during the process of adding potassium perchlorate 0-20°C. Then raise the temperature of the system to 60°C, react for 1.5h, then add 80ml of water, and at the same time raise the temperature of the system to 95°C for 10min, then add 200ml of distilled water to terminate the reaction, centrifugally wash until the pH is 7, and vacuum dry at 70°C to obtain graphite oxide solid. Consistent with the characterization results of Example 1, the interlayer distance of graphite oxide is 0.835nm, which is significantly increased compared with the initial graphite, indicating that the oxidation effect of graphite oxide is very good.

[0043] 2) Preparation of graphene oxide suspens...

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Abstract

The invention relates to a method for preparing grapheme through oxidation reduction and belongs to grapheme preparation technique. The method specifically comprises the following steps: a modified Hummer method is used for preparing graphite oxide, and an oscillator is adopted for shaking and peeling off single layer graphite oxide softly. During the step of preparing grapheme through reduction, compared with kinds of conventional major reducing agents, the method has the advantages that the reduction procedures and conditions are optimized, and further the grapheme with excellent performance is obtained. In the invention, by optimizing the preparation technique and conditions, the grapheme, which is large in size, is single-layered, is excellent in electrical conductivity and has high quality is obtained, and the method has the characteristics of low cost, high product yield and easiness in industrialization.

Description

Technical field: [0001] The invention relates to a method for preparing graphene by redox, which belongs to the preparation technology of graphene. Background technique: [0002] The term graphene refers to a single layer of carbon atoms tightly packed into a two-dimensional hexagonal honeycomb lattice structure. In 2004, two scientists, Andre Geim and Konstantin Novoselov from the University of Manchester in the United Kingdom, made groundbreaking progress in the preparation of two-dimensional space material graphene (Graphene) (K.S.Novoselov, A.K.Geim et al Science 306, 666 (2004)), obtained won the 2010 Nobel Prize in Physics. The discovery of graphene immediately caused a sensation in the scientific community. Graphene is a brand new material with an unprecedentedly small thickness and high mechanical strength. At the same time, it also has good electrical conductivity higher than copper, and in terms of thermal conductivity, it surpasses all other materials known so f...

Claims

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Application Information

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IPC IPC(8): C01B31/04C01B32/184C01B32/19C01B32/198
Inventor 暴宁钟何大方绍邵峰查晨阳邱新民杨文哲
Owner NANJING UNIV OF TECH
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