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Preparation method of dispersible silane functionalized graphene

A graphene and dispersibility technology, applied in the field of preparation of dispersible silane-functionalized graphene, can solve the problems of non-amino silane coupling agent silane research, unsatisfactory dispersion effect, graphene agglomeration, etc. Low requirements, few layers, mild conditions

Inactive Publication Date: 2012-02-15
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

The patent application document with the application number 2010102879852 modifies graphene by aminosilane coupling agent, and then strengthens the silica gel, which has good dispersion in water, ethanol, tetrahydrofuran, dimethyl sulfoxide and other solvents (Changchun Application of Chinese Academy of Sciences Institute of Chemistry, invention patent, application number: 2010102879852), however, this patent application document only describes the aminosilane coupling agent, and does not study the non-aminosilane coupling agent silane
In fact, as far as a single sheet of graphene oxide is concerned, it also contains many identical or different active functional groups. When it is chemically modified with multifunctional silane, it is often very easy between graphene oxide sheets and graphene oxide sheets. Chemical crosslinking occurs, leading to the final graphene agglomeration and agglomeration, which is difficult to disperse or the dispersion effect is not ideal

Method used

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  • Preparation method of dispersible silane functionalized graphene

Examples

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Embodiment 1

[0022] Preparation of trimethylmethoxysilane functionalized graphene:

[0023] Step 1: Dissolve 100mg of graphite oxide in 100ml of absolute ethanol, ultrasonically disperse for 1 hour to form a uniform dispersion of 1mg / ml, adjust the pH of the dispersion to 3 with dilute hydrochloric acid; The silane mass ratio is 1:0.5, add trimethylmethoxysilane, react at 60°C for 24 hours, centrifuge, remove the supernatant, and wash the subnatant with absolute ethanol and deionized water several times to completely remove Unreacted trimethylmethoxysilane until the washing solution is neutral to obtain silane-modified graphene oxide.

[0024] Step 2: Disperse the above-mentioned silane-modified graphene oxide in 100ml of absolute ethanol and sonicate for 1 hour to become a uniform and stable modified graphene oxide dispersion, then add 1g of hydrazine hydrate and reduce it at 60°C for 48 hours, Then the reaction solution was suction filtered, and the resulting filter cake was washed with...

Embodiment 2

[0028] Triethylmethoxysilane, phenyldimethylmethoxysilane, diphenylmethylmethoxysilane, vinyldimethylmethoxysilane, trimethylethoxysilane, triethylethyl Oxysilane, phenyldimethylethoxysilane, diphenylmethylethoxysilane, vinyldimethylethoxysilane instead of trimethylmethoxysilane, the rest are the same as in Example 1.

Embodiment 3

[0030] Preparation of trimethylchlorosilane functionalized graphene:

[0031] Step 1: Dissolve 100mg of graphite oxide in 10ml of absolute ethanol, and ultrasonically disperse for 1 hour to form a uniform dispersion of 1mg / ml; then under the protection of nitrogen atmosphere, the mass ratio of graphene oxide and trimethylchlorosilane is 1:1 Add trimethylchlorosilane at the ratio of 60 ° C for 24 hours, centrifuge, remove the supernatant, and then wash with absolute ethanol and deionized water several times to completely remove unreacted trimethylchlorosilane, and make the washing Liquid to neutral, obtain silane-modified graphene oxide;

[0032]Step 2: Disperse the above-mentioned silane-modified graphene oxide in 100ml of absolute ethanol and sonicate it for 1 hour to become a uniform and stable modified graphene oxide dispersion, then add 1g of hydrazine hydrate and reduce it at 60°C for 24 hours, Then the reaction solution was suction filtered, and the obtained filter cake...

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Abstract

The invention provides a preparation method of dispersible silane functionalized graphene. The method comprises the steps of: conducting ultrasonic dispersion to graphene oxide in absolute ethyl alcohol so as to form a uniform graphene oxide dispersion solution, then adjusting the pH value to 3-4, or under the protection of an inert atmosphere, adding silane into the dispersing solution for modification, with silane and graphene oxide in a mass ratio of 0.1:1-5:1, continuing the reaction for 12h-48h at a temperature ranging from normal temperature to 78DEG C, carrying out centrifugation, then adding hydrazine hydrate to the obtained solid, performing heating reduction, and filtering the reaction solution, then washing and drying the filter cake, thus obtaining dispersible silane functionalized grapheme. The method of the invention is simple and practicable, and the obtained silane functionalized grapheme has good dispersibility in solvents like absolute ethyl alcohol, acetone, toluene, ethyl acetate, butyl acetate, and tetrahydrofuran (THF), etc.

Description

technical field [0001] The invention relates to the preparation of graphene, in particular to a preparation method of dispersible silane functionalized graphene. Background technique [0002] Graphene is a carbonaceous material with a single-layer two-dimensional honeycomb structure formed by densely packed carbon atoms. It can be regarded as the basic structural unit for the construction of fullerenes, carbon nanotubes, and graphite. Graphene has extremely high Young's modulus (about 1100Gpa), thermal conductivity (about 5000J / (m·K·s)), room temperature carrier mobility (2×10 5 cm 2 / (V s)) and specific surface area (theoretical calculation value 2630m 2 / g), also has quantum Hall effect and quantum tunneling effect, etc., and is expected to be widely used in nanocomposite materials, liquid crystal materials and energy storage materials. However, graphene is neither hydrophilic nor lipophilic, and its chemical reaction is inert, which hinders its research and applicatio...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 马文石时镜镜汪双凤
Owner SOUTH CHINA UNIV OF TECH
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