Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method

A technology of graphene and graphite, which is applied in the field of graphene preparation, can solve the problems of poor stability control, poor quality of graphene, high cost, etc., and achieve the effect of thorough stripping, easy processing, and low equipment requirements

Inactive Publication Date: 2012-05-02
深圳市长宜景鑫投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among the many methods, there are disadvantages that cannot be ignored. Some methods are too costly and the yield is too low. Some methods have high yield but the quality of graphene is too poor, there are many defects, and the stability of the experiment is not good. control, and most methods are energy-intensive

Method used

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  • Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method
  • Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method
  • Method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Add 10g of graphite powder or flake graphite (50 mesh to 1000 mesh) or expanded graphite into 200mL to 1L of chlorosulfonic acid mixed acid, the ratio of mixed acid is: chlorosulfonic acid / concentrated sulfuric acid / perchloric acid=8 / 1~4 / 1~3, Stir evenly and seal well. After ultrasonic treatment for 30 minutes, soak statically or stir magnetically for 2-24 hours. Then, a 30% aqueous hydrogen peroxide solution was slowly added dropwise to the mixture while stirring. After adding 100-500mL of hydrogen peroxide, the above mixture will expand rapidly and turn into a black viscous colloid, like black wet soil. The dropping process is dangerous, pay attention to the dropping speed. The resulting gel was then washed to neutral with deionized water. Then the obtained graphene dispersion can be better dispersed by ultrasonic treatment, so that the agglomerated graphene in the cleaning process can be separated into a fluffy floc, and the ultrasonic treatment can be done for 3...

Embodiment 2

[0040] The experimental method is the same as in Example 1, except that after obtaining the black gel, it is dropped into 500-1000ml of polar organic reagents, and these polar organic reagents can be: methyl formamide (DMF), N-methylpyrrolidone ( NMP), dimethyl sulfoxide (DMSO), etc. Ultrasonic treatment of these organic dispersions of graphene can reduce the agglomeration of graphene and obtain more single-layer graphene. Then wash with water to pH 6-7. The obtained graphene surface will have these small molecule organic solvents adsorbed on the surface, which is conducive to its dispersion in some solvents.

Embodiment 3

[0042] Experimental method is the same as embodiment 1, just when soaking, some surfactants and some polymers are added in the acid solution, these surfactants and polymers have: sodium dodecylsulfonate, hexadecylbenzenesulfonate Sodium tritonate, triton X-100, polystyrene, sodium polystyrene sulfonate, polyaniline, sodium polyaminobenzene sulfonate, polypyrrole, polythiophene, PEDOT, etc. Adding some polymers can reduce the re-aggregation of graphene during the exfoliation process, and can also improve its dispersion. The addition of some polymers directly completes the compounding with the polymer during the exfoliation process of graphene, which can be used as a This graphene composite material is directly applied in some fields.

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Abstract

The invention discloses a method for preparing high-quality graphene in large scale by intercalation stripping of graphite by chemical method. The main principle and approach are as follows: inserting some reagent into graphite intercalation by chemical method, then adding energy or some reagent to make intercalation material rapidly and violently react to release air and stripping graphite into graphene. The specific embodiment proposal comprises means of liquid phase stripping, solid phase stripping and two-step liquid phase and solid phase combined stripping. The prepared graphene has high single intercalation quality and few detects since it does not go through oxidation and reduction processes. The oxygen content is only 1.63% and is the lowest in known graphene preparation method by graphite. There is no impurity or molecule absorbed on the graphene surface. The invention has low cost, high yield, simple and feasible preparation method and low energy consumption and is suitable for large scale generation.

Description

technical field [0001] The invention belongs to the technical field of graphene materials, in particular to a method for preparing graphene by chemically intercalating and exfoliating graphite, in particular to the violent reaction between the interlayer of intercalated graphite and another or several reagents to release gas Exfoliation, which stretches apart graphite sheets, is a method for producing graphene in large quantities and cheaply. Background technique [0002] Since the advent of graphene in 2004, it has received extensive scientific attention due to its excellent electrical properties. For example, its carrier transport behavior is similar to that of neutrinos in the theory of relativity, and the quantum Hall effect and bipolar field effect can be observed at room temperature. Moreover, the unique physical and mechanical properties of graphene further broaden its application space: extremely high Young's modulus, thermal conductivity as high as 5300W / mK, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 吴何舜
Owner 深圳市长宜景鑫投资有限公司
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