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Macroscopic-quantity preparation method of fluorinated graphene

A technology of fluorinated graphene and fluorinated graphite is applied in the field of macro-scale preparation of fluorinated graphene, and can solve the problems of inability to prepare fluorinated graphene on a large scale, high requirements for reaction atmosphere and equipment, and difficulty in realizing industrialization. , to achieve the effect of short cycle, low cost and few preparation steps

Inactive Publication Date: 2019-01-08
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former is based on graphene, F 2 or XeF 2 As a fluorinating reagent, graphene was exposed to F 2 or XeF 2 The fluorination reaction occurs in an atmosphere, because this method has high requirements on the reaction atmosphere and equipment, is expensive, the reaction is difficult to control and is prone to danger, and the fluorination agent is highly toxic, so it is difficult to realize industrialization; the second method is based on Fluorinated graphite is used as a raw material, and fluorinated graphene is obtained by exfoliating it by various means. Withers’ research group exfoliates fluorinated graphite to obtain fluorinated graphene by mechanical exfoliation. Obviously, this method cannot be used for large-scale preparation of fluorinated graphene. fluorinated graphene, Zboril research group uses very polar sulfolane as a solvent liquid-phase ultrasonic exfoliation of fluorinated graphite to obtain fluorinated graphene, the disadvantage of this method is the use of highly toxic sulfolane

Method used

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  • Macroscopic-quantity preparation method of fluorinated graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 0.2g of cetyltrimethylammonium bromide in a 100mL beaker, add 20mL of isopropanol, and stir at room temperature for 10min to obtain a mixed solution;

[0026] Take 0.2g of fluorinated graphite powder, add 50mL of N-methylpyrrolidone, after stirring, add the above cetyltrimethylammonium bromide mixed solution, and keep in a constant temperature water bath at 50°C for 2h;

[0027] After cooling naturally at room temperature, place it in an ultrasonic vibration cleaner, and ultrasonicate for 2 hours with a power of 150W;

[0028] Centrifuge the fluorinated graphene dispersion obtained after ultrasonic stripping, centrifuge at 12000rmp for 15min, collect the supernatant, filter, wash with ethanol multiple times, and freeze-dry to obtain the target product fluorinated graphene.

[0029] figure 1 TEM of the fluorinated graphene prepared for this example.

Embodiment 2

[0031] Put 0.3g of tetradecyldimethylpyridinium bromide in a 100mL beaker, add 50mL of dichloromethane, and stir at room temperature for 10min;

[0032] Take 0.5g of fluorinated graphite powder, add 100mL of N-methylpyrrolidone, after stirring, add a mixed solution of tetradecyldimethylpyridinium bromide, and keep in a constant temperature water bath at 30°C for 2h;

[0033] After cooling naturally at room temperature, place it in an ultrasonic vibration cleaner, and ultrasonicate for 6 hours with a power of 150W;

[0034] Centrifuge the fluorinated graphene dispersion obtained after ultrasonic stripping, centrifuge at 12000rmp for 10min, collect the supernatant, filter, wash with ethanol multiple times, and freeze-dry to obtain the target product fluorinated graphene.

Embodiment 3

[0036] Put 0.4g of cetyltrimethylammonium bromide in a 100mL beaker, add 30mL of ethanol, and stir at room temperature for 10min;

[0037] Take 0.1g of fluorinated graphite powder, add 50mL of N,N-dimethylacetamide, add cetyltrimethylammonium bromide mixed solution after stirring, and keep in constant temperature water bath at 60°C for 2h;

[0038] After natural cooling at room temperature, place it in an ultrasonic vibration cleaner, 200W power ultrasonic 4h;

[0039] Centrifuge the fluorinated graphene dispersion obtained after ultrasonic stripping, centrifuge at 10000rmp for 15min, collect the supernatant, filter, wash with ethanol multiple times, and freeze-dry to obtain the target product fluorinated graphene.

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Abstract

The invention provides a macroscopic-quantity preparation method of fluorinated grapheme. According to the preparation method, with cheap fluorinated graphite as a raw material, after treatment by a cationic surfactant and an organic intercalator and ultrasonic stripping, single-layer or few-layer fluorinated grapheme can be obtained. According to the preparation method, a technology is simple, the reaction is mild, control is easy, the raw material is cheap and easy to obtain, and the yield is high; the preparation method is applicable to large-scale macroscopic-quantity industrial production.

Description

technical field [0001] The invention belongs to the field of new materials and relates to a macro-preparation method of fluorinated graphene. Background technique [0002] As a new derivative of graphene materials, graphene fluoride not only maintains the high-strength properties of graphene, but also brings novel interfaces and properties such as reduced surface energy, enhanced hydrophobicity, and widened bandgap due to the introduction of fluorine atoms. Physical and chemical properties. Especially compared with zero-bandgap graphene, the controllable introduction of fluorine realizes the transition and transformation of its electronic structure from conductor, semiconductor to insulator, and the widening of the bandgap makes fluorinated graphene exhibit more excellent optoelectronic properties and greater practical application possibilities. These excellent properties of fluorinated graphene make it have great application potential in lubricants, electronic optical dev...

Claims

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Application Information

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IPC IPC(8): C01B32/19C01B32/10
CPCC01B32/10C01B32/19
Inventor 何丹农胡丹童琴赵昆峰代卫国金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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