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High-fluoride-content graphite fluoride and preparation method thereof

A technology of fluorinated graphene and graphene, applied in the direction of graphene, fluorinated carbon, nano-carbon, etc., can solve the problems of fluorinated graphene with high fluorine content, low thermal stability, cumbersome process, etc., and achieve Increased fluorination degree, improved thermal stability, and easy diffusion effects

Active Publication Date: 2013-12-04
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The latter is to react graphene with a fluorinating agent, and the fluorinated graphene produced is only "0-10.5%" rich, and the corresponding thermal stability is also low, and both need to reduce graphene oxide to After graphene is fluorinated, the process is more cumbersome
Although the patent CN 1026107941 A discloses a method for directly fluorinating graphene to prepare fluorinated graphene, the maximum fluorine content in the resulting modified graphene is still only 30%, which cannot reach the high fluorine content of fluorinated graphene. Require

Method used

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  • High-fluoride-content graphite fluoride and preparation method thereof
  • High-fluoride-content graphite fluoride and preparation method thereof
  • High-fluoride-content graphite fluoride and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0036] Freeze the prepared graphene oxide aqueous dispersion in liquid nitrogen for 100s and then dry it with a freeze dryer to a water content of 1% to obtain honeycomb graphene oxide; place the graphene oxide in a closed vacuum reactor , replace the air in the reactor with nitrogen three times, then vacuumize, then fill with fluorine and nitrogen, and control the initial partial pressure of fluorine in the reactor to 3 KPa, and then raise the temperature to 200°C at a heating rate of 1°C / min And keep warm for 30 minutes, wait for the reactor to cool down to room temperature naturally, take out the fluorinated graphene.

[0037] It is measured that the massfraction of fluorine element in this graphene is 56%, and the massfraction of carbon element is 44%.

Embodiment 2

[0039] The prepared aqueous dispersion of graphene oxide was frozen in liquid nitrogen for 300s and then dried to a water content of 1% with a lyophilizer to obtain honeycomb graphene oxide; the graphene oxide was placed in a closed vacuum reactor , replace the air in the reactor with nitrogen three times, then vacuumize, then fill with fluorine and nitrogen, and control the initial partial pressure of fluorine in the reactor to 30 KPa, and then raise the temperature to 250°C at a heating rate of 5°C / min And keep warm for 10 minutes, wait for the reactor to cool down to room temperature naturally, take out the fluorinated graphene.

[0040] It is measured that the mass fraction of fluorine element in this graphene is 55%, and the mass fraction of carbon element is 45%.

Embodiment 3

[0042] The prepared graphene oxide aqueous dispersion was frozen in liquid nitrogen for 200s and then dried to a water content of 2% with a lyophilizer to obtain honeycomb graphene oxide; the graphene oxide was placed in a closed vacuum reactor , replace the air in the reactor with nitrogen for three times, then evacuate, then fill with fluorine, nitrogen and argon, and control the initial partial pressure of fluorine in the reactor to 50 KPa, then raise the temperature at a rate of 5 °C / min to 200°C and keep it warm for 120 minutes. After the reactor is naturally cooled to room temperature, the fluorinated graphene is taken out.

[0043] It is measured that the mass fraction of fluorine in the graphene is 64%, and the mass fraction of carbon is 36%.

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Abstract

The invention discloses high-fluoride-content graphite fluoride and a preparation method thereof. The method comprises the following steps: preparing aqueous dispersion liquid of graphite oxide with a conventional improved Hummers method, then freezing the aqueous dispersion liquid of graphite oxide in liquid nitrogen to be completely frozen into solid, and freezing and drying to obtain cellular graphite oxide; under a mixed atmosphere of inert gas and fluoride, warming the cellular graphite oxide for fluoridation, and cooling to room temperature. The fluoride content of the prepared high-fluoride-content graphite fluoride is 55-70 percent, fluorine atoms are bonded with carbon atoms in a covalent bond mode, weightlessness peak temperature is larger than 470 DEG C, the heat stability is good, and the resistance is larger than 1012 omega. The prepared graphite fluoride has the advantages of high fluoride content, good heat resistance of fluorine-containing groups, low cost, simple process, lower reaction temperature, high safety and energy saving, is suitable for mass production, and has a better application prospect.

Description

technical field [0001] The invention belongs to the technical field of fluorinated graphene and its preparation, and in particular relates to a high-fluorine-content fluorinated graphene and a preparation method thereof. Background technique [0002] As a derivative of graphene, graphene fluoride has attracted widespread attention due to its unique physical and chemical properties such as high energy storage, lubrication and barrier properties, and wide energy gap. In fluorinated graphene, the level of fluorine content affects the performance of fluorinated graphene in various aspects, such as its chemical stability, thermal stability, lamellar structure spacing, electrical properties, magnetic properties, adsorption properties, barrier properties and lubrication properties, etc. have a direct impact. Generally speaking, the performance of fluorinated graphene with high fluorine content is better than that of fluorinated graphene with low fluorine content. Therefore, accord...

Claims

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Application Information

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IPC IPC(8): C01B31/00C01B32/10C01B32/184
Inventor 刘向阳王旭高杰黄杰阳李保印范聪
Owner SICHUAN UNIV
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