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Preparation method of fluorinated graphene

A technology of fluorinated graphene and graphene, which is applied in the field of preparation of fluorinated graphene materials, can solve problems such as the inability to realize the regulation of fluorine content, large production safety hazards, and high price

Active Publication Date: 2014-12-17
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, high-quality graphene itself is difficult to mass-produce and expensive
Moreover, using the F 2 or XeF 2 Both are extremely corrosive and highly toxic gases, which pose a great potential safety hazard in production
The second is to physically exfoliate (micromechanical or solvent-assisted ultrasound) fluorinated graphite to obtain monolayer or few-layer fluorinated graphene (Zboril, R.; Karlicky, F.; Bourlinos, A.B.; Steriotis, T.A. ; Stubos,A.K.;Georgakilas,V.;Safarova,K.;Jancik,D.;Trapalis,C.;Otyepka,M.Small2010,6,2885.), but the efficiency is extremely low, and the regulation of fluorine content cannot be achieved

Method used

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  • Preparation method of fluorinated graphene

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[0131] Preparation of fluorinated graphene

[0132] The invention provides a kind of preparation method of fluorinated graphene, described method comprises:

[0133] Use fluorinating reagent to react with graphene oxide to obtain fluorinated graphene.

[0134] In another preferred example, the mass ratio of fluorinating reagent to graphene oxide is: fluorinating reagent: graphene oxide = 0.001-500:1, preferably fluorinating reagent: graphene oxide = 0.1-100:1.

[0135] Preferably, after the reaction is completed, a quenching agent can be optionally added to quench the reaction system. The quenching agents include (but are not limited to): alcohols, thiols, amines, ketones, amides, water, or combinations thereof.

[0136] In another preferred embodiment, the quencher is selected from the group consisting of methanol, ethanol, isopropanol, or combinations thereof.

[0137] The reaction can be carried out in an inert solvent. Preferably, the inert solvent is selected from the ...

Embodiment 1

[0158] Weigh 120 mg of graphene oxide and disperse it in 120 mL of tetrahydrofuran, add 2 mL of diethylaminosulfur trifluoride (DAST), stir at room temperature for 3 days, then add 50 mL of methanol to the reaction system to quench the reaction. Then the reaction system was filtered through a 0.22-micron polytetrafluoroethylene membrane, the filter cake was washed with a solvent, the filter cake was collected and vacuum-dried to obtain a black powder product, the fluorine content was determined to be 3.1% by elemental analysis.

Embodiment 2

[0160] The preparation method is basically the same as in Example 1, except that the solvent used is pyridine, and the fluorine content of the obtained product is determined to be 5.2% by elemental analysis.

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Abstract

The invention relates to a mild preparation method of fluorinated graphene. The method adopts cheap and easily available graphene oxide and a liquid or solid fluorinating reagent as raw materials, and by changing the reaction solvent, time, pressure and other conditions, fluorinated graphene with an adjustable fluorine content can be obtained at room temperature. According to the invention, the filtration washing means is also utilized to remove the excess reaction reagents, solvents and other impurities during solution method preparation, thus obtaining a pure fluorinated graphene product.

Description

technical field [0001] The invention relates to the field of fluorinated materials, in particular, the invention relates to a preparation method of a fluorinated graphene material. Background technique [0002] Graphene is a new type of two-dimensional carbon single-substance nanomaterial discovered after fullerene and carbon nanotubes. It has many special physical properties (such as zero band gap, room temperature quantum Hall effect) and extraordinary electrical and thermal conductivity. , optical and mechanical properties, and has great potential application prospects in electronics, structural materials, energy storage materials, catalytic materials, sensing materials, etc. Graphene fluoride is a derivative material of graphene, which is part or all of graphene sp 2 Carbon is converted to sp by addition of F atom 3 The structure is C-F, but the morphology still maintains the lamellar structure. Perfluorinated graphene, also known as perfluorinated graphane, is a tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 李维实陈庆云赵福刚赵刚李柏力王金土葛从伍梅崇余
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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