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Preparation method of high fluorine content nano fluorinated graphene

A technology of fluorinated graphene and fluorine content, which is applied in the field of nanomaterials, can solve the problems that it is impossible to reach the nanometer level and has no practical significance, and achieve the effect of increasing the reaction contact area and reducing the particle size

Active Publication Date: 2018-09-11
厦门中科希弗科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process has no practical significance. The traditional so-called nano-graphite is prepared by mechanical grinding, and it is impossible to reach the nanometer level. The micron level is already the limit that grinding can achieve.

Method used

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  • Preparation method of high fluorine content nano fluorinated graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1: Put 50g of graphene into the fluorination equipment, pass in fluorine gas, keep the pressure at 95KPa, and react at 450-500°C for 12h.

[0020] Step 2: Weigh 100g of fluorinated graphene with low fluorine content prepared in step 1, add 500mL of N-methylpyrrolidone, transfer to the ball milling tank of planetary ball mill, and ball mill for 5h at a speed of 600r / min to obtain fluorinated graphene slurry.

[0021] Step 3: Transfer the fluorinated graphene slurry prepared in step 2 to a plastic bottle, then add 200mL N-methylpyrrolidone, and perform ultrasonic separation at 50kHz for 24h to obtain a fluorinated graphene dispersion, which is then spray-dried. The nanometer fluorinated graphene powder with low fluorine content is obtained.

[0022] Step 4: Put 50g of nano-fluorinated graphene powder with low fluorine content prepared in step 3 into the fluorination equipment, pass in a mixed gas containing 20% ​​fluorine gas, keep the pressure at 100-120KPa, at 650...

Embodiment 2

[0030] Step 1: Put 50g of graphene into the fluorination equipment, feed fluorine gas, keep the pressure at 80KPa, and react at 450°C for 8h.

[0031] Step 2: Weigh 100g of nano-fluorinated graphene with low fluorine content obtained in step 1, mix nano-fluorinated graphene with low fluorine content and 500mL liquid phase solvent, and transfer to planetary ball mill for ball milling after uniform mixing In the tank, the fluorinated graphene slurry was obtained at a rotating speed of 300r / min and a ball milling time of 2h.

[0032] Step 3. Transfer the fluorinated graphene slurry obtained in step 2 to a plastic bottle, add a liquid phase solvent to mix, and after mixing evenly, transfer to an ultrasonic separator, and perform ultrasonic treatment for 1 hour at an ultrasonic frequency of 20 kHz to obtain The fluorinated graphene dispersion liquid is spray-dried to obtain the fluorinated graphene nanometer powder with low fluorine content.

[0033] Step 4. Weigh 50g of the low-f...

Embodiment 3

[0036] Step 1: Put 50g of graphene into the fluorination equipment, pass in fluorine gas, keep the pressure at 90KPa, and react at 485°C for 12h.

[0037] Step 2: Weigh 100g of nano-fluorinated graphene with low fluorine content obtained in step 1, mix nano-fluorinated graphene with low fluorine content and 2000mL liquid phase solvent, and transfer to planetary ball mill for ball milling after mixing evenly In the tank, the fluorinated graphene slurry was obtained at a rotating speed of 500r / min and a ball milling time of 12h.

[0038] Step 3: Transfer the fluorinated graphene slurry obtained in step 2 to a plastic bottle, add a liquid phase solvent to mix, and after mixing evenly, transfer to an ultrasonic separator, and perform ultrasonic treatment for 12 hours at an ultrasonic frequency of 60 kHz to obtain The fluorinated graphene dispersion liquid is spray-dried to obtain the fluorinated graphene nanometer powder with low fluorine content.

[0039] Step 4: Weigh 50g of na...

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Abstract

The invention relates to the technical field of nano materials, and discloses a preparation method of high fluorine content nano fluorinated graphene. Firstly, fluorine gas is used as a fluorine source through step 1, the fluorine gas has strong reaction activity and can perform etching on the graphene, thereby achieving chemical crushing and reducing the particle size of the graphene, and nano-sized low fluoride content nano fluorinated graphene is effectively prepared, secondly, the particle size of the fluorinated graphene is further reduced through ultrasonic dispersion and high-energy ball milling in steps 2 and 3, and finally through the high temperature fluorination reaction of the fluorine-containing gas in step 4, the fluorine content in high fluorine content nano fluorinated graphene powder is guaranteed; after reasonably designed reaction steps, the finally prepared high fluorine content nano-fluorinated graphene powder with nanometre particle diameter has a structural sizeof 100 nanometre or less.

Description

technical field [0001] The invention relates to the technical field of nanometer materials, in particular to a method for preparing nanometer fluorinated graphene with high fluorine content. Background technique [0002] As a new derivative of graphene, fluorinated graphene not only maintains the high-strength performance of graphene, but also brings novel interface and physical and chemical properties such as reduced surface energy, enhanced hydrophobicity and widened band gap due to the introduction of fluorine atoms. . At the same time, fluorinated graphene is resistant to high temperature and has stable chemical properties, showing properties similar to polytetrafluoroethylene, and is called "two-dimensional Teflon". The surface energy of fluorinated graphene is reduced, the hydrophobicity is enhanced, and it also has the characteristics of high temperature resistance and stable chemical properties. It can be used as a tunnel barrier or as a high-quality insulator or ba...

Claims

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Application Information

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IPC IPC(8): C01B32/194B82Y40/00
CPCB82Y40/00C01B32/194C01B2204/32
Inventor 叶荣森
Owner 厦门中科希弗科技有限公司
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