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Preparation method of nano graphite sheet

A technology of nano-graphite sheets and expanded graphite, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems affecting the application of nano-graphite sheets, endangering the health of producers, and high production costs, and achieves short running time, The effect of high peeling degree and good thermal conductivity

Active Publication Date: 2013-12-25
西大(常熟)研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Usually, concentrated strong protic acid is used to prepare graphite intercalation compounds, such as nitric acid and sulfuric acid as intercalation agents for intercalation reaction, and then washed with water, dried, and expanded at high temperature. 2 , SO 3 、H 2 S. NO x Escaping in the form of other gases, forming a large amount of nitrogen and sulfur oxides, causing serious environmental pollution and endangering the health of producers
In addition, when sulfuric acid is used as an intercalation agent, a considerable part of sulfur remains in the expanded graphite worms in the form of compounds, and most of the sulfur content is above 1%, which affects the application of nano-graphite sheets.
In addition, the thermal expansion of graphite intercalation compounds is usually produced by heating in conventional high-temperature furnaces that are energy-intensive, thus causing considerable production costs

Method used

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  • Preparation method of nano graphite sheet
  • Preparation method of nano graphite sheet
  • Preparation method of nano graphite sheet

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 1g of natural fine flake graphite, 1.4g of perchloric acid, 0.8g of glacial acetic acid and 0.4g of potassium permanganate, and put the weighed materials into a dry three-necked flask equipped with a thermometer and a magnetic stirring rotor. The mixture was continuously mixed and reacted with magnetic stirring at 45° C. for 60 min, then filtered, washed with deionized water until neutral, and dried at 60° C. for 1 h to obtain intercalated expandable graphite. Put the dried intercalated expandable graphite into a microwave oven for rapid heating. The microwave output power is 500W. During the heating process, a bright flame can be observed. When the flame disappears, the heating stops and the heating time is 10s to obtain expanded graphite. Next, 1 g of expanded graphite was initially mixed with 80 ml of absolute ethanol solution with a stirring bar, and then the mixture was irradiated with ultrasonic waves at a power of 600 W for 2 hours. After that, remove the r...

Embodiment 2

[0036] Weigh 1.1g of natural fine flake graphite, 1.54g of perchloric acid, 0.88g of glacial acetic acid and 0.44g of potassium permanganate, and put the weighed materials into a dry three-necked flask equipped with a thermometer and a magnetic stirring rotor. The mixture was continuously mixed and reacted with magnetic stirring at 40°C for 65min, then filtered, washed with deionized water until neutral, and dried at 55°C for 1.5h to obtain intercalated expandable graphite. Put the dried intercalated expandable graphite into a microwave oven for rapid heating. The microwave output power is 550W. During the heating process, a bright flame can be observed. When the flame disappears, the heating stops and the heating time is 8s to obtain expanded graphite. Next, 2 g of expanded graphite was initially mixed with 80 ml of absolute ethanol solution with a stirring bar, and then the mixture was irradiated with ultrasonic waves at a power of 800 W for 1.5 hours. After that, remove the...

Embodiment 3

[0038] Weigh 1.2g of natural fine flake graphite, 1.68g of perchloric acid, 0.96g of glacial acetic acid and 0.48g of potassium permanganate, and put the weighed materials into a dry three-necked flask equipped with a thermometer and a magnetic stirring rotor. The mixture was continuously mixed and reacted with magnetic stirring at 45°C for 70min, then filtered, washed with deionized water until neutral, and dried at 50°C for 2h to obtain intercalated expandable graphite. Put the dried intercalated expandable graphite into a microwave oven for rapid heating. The microwave output power is 600W. During the heating process, a bright flame can be observed. When the flame disappears, the heating stops and the heating time is 7s to obtain expanded graphite. Next, 3 g of expanded graphite was initially mixed with 80 ml of absolute ethanol solution with a stirring bar, and then the mixture was irradiated with ultrasonic waves at a power of 800 W for 1.5 hours. Afterwards, remove the r...

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Abstract

The invention discloses a preparation method of a nano graphite sheet. Natural flake graphite is taken as a raw material; oxidation intercalation treatment is performed on the natural flake graphite by adopting an oxidizing agent and an intercalation agent so as to form intercalated expansible graphite; puffing is performed on the intercalated expansible graphite through a microwave heating method so as to form expansible graphite; the expansible graphite is stripped into nano graphite sheets by adopting ultrasonic irradiation in an organic solvent. The preparation method provided by the invention is simple in operation, high in efficiency, excellent in safety and uniform in expansion; the nano graphite sheet prepared through the preparation method is 0.5 to 20 Mum in diameter, 0.35 to 50 nm in thickness and 35 nm in average thickness, the degree of stripping is high, and the nano graphite sheet can be made into different shapes such as a winding drum shape, a curly S shape and a concave-convex block mass shape, and has an excellent heat-conducting property, and can be easily dispersed in the organic solvent.

Description

technical field [0001] The invention belongs to the field of nano-graphite materials, and in particular relates to a preparation method of nano-graphite sheets. Background technique [0002] Due to abundant sources, low price, extremely high corrosion resistance and chemical stability, and good electrical and thermal conductivity, nanographite sheets can be widely used. For example: as a conductive filler in polymers to improve the conductivity of polymer composites, as an additive in heat transfer oil or phase change thermal energy storage materials to improve thermal conductivity, as an electrode component in lithium-ion batteries, in hydrogen storage materials Nano-graphite flakes are also introduced to enhance its hydrogen storage performance. [0003] The preparation and synthesis methods of nano-graphite can be divided into two categories: one is the physical preparation method of crushing natural flake graphite, mainly including mechanical ball milling, detonation ...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y30/00C01B32/225
Inventor 黄金肖俊兵祝盼盼
Owner 西大(常熟)研究院有限公司
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