Method for preparing high-quality reduced graphene through high-energy-pulse microwave rapid recovery

A high-energy pulse and graphene technology, applied in the graphene field, can solve the problems of many graphene defects and long processing time, and achieve the effect of simple operation, complete sheet structure and high quality

Inactive Publication Date: 2019-10-18
徐州宇帆机电科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the processing time of these methods is long, and some by-products are produced, and the graphene produced has many defects, which limits the further expansion of the graphene product market

Method used

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  • Method for preparing high-quality reduced graphene through high-energy-pulse microwave rapid recovery
  • Method for preparing high-quality reduced graphene through high-energy-pulse microwave rapid recovery
  • Method for preparing high-quality reduced graphene through high-energy-pulse microwave rapid recovery

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Add 1g of flake graphite to 20mL of fuming nitric acid in an ice-water bath, then add 2mL of 30% hydrogen peroxide while stirring, react for 40min, wash with water, dry, and expand in a tube microwave oven with a power of 800w for 10s , to obtain expanded graphite.

[0027] Place a beaker containing 120ml of concentrated sulfuric acid with a mass fraction of 98% and 12ml of phosphoric acid with a mass fraction ≥ 50% in a low-temperature water bath at 0°C, add 1g of the obtained expanded graphite into the mixed acid solution, and stir magnetically for 30 minutes ; Secondly, according to the speed of 1g / h, 6g of potassium permanganate is slowly added to the above-mentioned mixed system, and the temperature of the reaction system is maintained at no more than 20°C (the addition of potassium permanganate should not be too fast, and can be added in small amounts and many times. ), continue the reaction at 0°C for 48h; then slowly add 400ml of dilute sulfuric acid at 0°C with...

Embodiment 2

[0034] Add 1g of flake graphite to 25mL of fuming nitric acid in an ice-water bath, then add 2mL of 30% hydrogen peroxide while stirring, react for 60min, wash with water, dry, and expand in a tube microwave oven with a power of 500w for 30s , to obtain expanded graphite.

[0035]Place a beaker containing 110ml of concentrated sulfuric acid with a mass fraction of 98% and 12ml of phosphoric acid with a mass fraction ≥ 50% in a low-temperature water bath at 0°C, add 1g of the obtained expanded graphite into the mixed acid solution, and stir magnetically for 45 minutes ; Secondly, according to the speed of 1g / h, 5g of potassium permanganate is slowly added to the above-mentioned mixed system, and the temperature of the reaction system is maintained at no more than 20°C (the addition of potassium permanganate should not be too fast, and can be added in small amounts and many times. ), continue the reaction at 0°C for 48h; then slowly add 400ml of dilute sulfuric acid at 0°C with ...

Embodiment 3

[0039] Add 1g of flake graphite to 25mL of fuming nitric acid in an ice-water bath, then add 2mL of 30% hydrogen peroxide while stirring, react for 60min, wash with water, dry, and expand for 15s in a tube microwave oven with a power of 800w , to obtain expanded graphite.

[0040] Place a beaker containing 90ml of concentrated sulfuric acid with a mass fraction of 98% and 12ml of phosphoric acid with a mass fraction ≥ 50% in a low-temperature water bath at 0°C, add 1g of the obtained expanded graphite into the mixed acid solution, and stir magnetically for 10 minutes ; Secondly, according to the speed of 1g / h, 4g of potassium permanganate is slowly added to the above-mentioned mixed system, and the temperature of the reaction system is maintained at no more than 10°C (the addition of potassium permanganate should not be too fast, and can be added in small amounts and multiple times. ), continue the reaction at 0°C for 48 hours; then slowly add 270ml of ice-dilute sulfuric acid...

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Abstract

The invention provides a method for preparing high-quality reduced graphene through high-energy-pulse microwave rapid recovery. The method comprises the main steps that crystalline flake graphite is added into fuming nitric acid under ice-water bath, hydrogen peroxide is added for a reaction for a certain time, washing and drying are conducted, and expanded graphite is obtained through microwave puffing; the expanded graphite and potassium permanganate are sequentially added in a mixed-acid system of 0-DEG C concentrated sulfuric acid and phosphoric acid, the strong oxidizing performance of the potassium permanganate is used, and the graphene is oxidized into graphene oxide under the low temperature of 0 DEG C; the graphene oxide is placed in a tube furnace to be subjected to insulation treatment, and pre-reduced graphene oxide powder is obtained; and finally, the pre-reduced graphene oxide powder is placed in a high-energy-pulse microwave cavity, microwave is opened, and a high-quality reduced graphene product is obtained. According to the high-quality reduced graphene prepared through the method, the lamellar structure is complete, the reduced graphene finally obtained through high-energy-pulse microwave rapid recovery is high in quality, and a good foundation is provided for preparation of graphene oxide, and graphene-based nanocomposite materials.

Description

technical field [0001] The invention belongs to the technical field of graphene, and in particular relates to a method for preparing high-quality reduced graphene by rapid reduction of high-energy pulsed microwaves. Background technique [0002] Graphene oxide is the product of graphite powder after chemical oxidation and exfoliation. It is also called functionalized graphene. It is an oxide of graphene and a precursor for low-cost and large-scale preparation of graphene. Compared with expensive carbon nanotubes, graphene oxide is cheap and easy to prepare. The traditional Hummers method to prepare graphene oxide has three steps, low-temperature edge oxidation, medium-temperature deep oxidation and high-temperature hydrolysis. However, due to medium-temperature strong oxidation and high-temperature hydrolysis, it is very easy to cause irreversible effects on the sheet structure of graphite, resulting in the loss of carbon atoms, which affects the performance and application...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B32/184
Inventor 刘秉国宇文超李华健张利波
Owner 徐州宇帆机电科技有限公司
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