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A kind of preparation method of graphene

A technology of graphene and graphite, which is applied in the field of graphene, can solve problems such as application limitations and the influence of graphene physical properties, and achieve the effects of reduced equipment requirements, unaffected physical properties, and reduced graphite content

Active Publication Date: 2016-02-03
JIANGSU SIDIKE NEW MATERIALS SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can produce graphene on a large scale, but the addition of polymer dispersant will affect the physical properties of graphene, which limits its application in many aspects

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The present embodiment provides a kind of preparation method of graphene, is to make through the following steps:

[0024] 1) Dispersing graphite in an azodicarbonamide foaming agent solution, stirring at a constant temperature for 30 minutes, and ultrasonically oscillating for 30 minutes, the ratio of graphite (g) to organic foaming agent (g) in parts by mass is 1:0.05;

[0025] 2) Keep the product of 1) in an oil bath at 280°C for 30 minutes at a constant temperature;

[0026] 3) After the product of 2) is cooled to normal temperature, it is added to a mixed solution of ethanol and concentrated nitric acid with a volume ratio of 30:1 to form a uniformly dispersed suspension with a concentration of 0.003g / mL. Under hydrothermal reaction for 48 hours, the suspension was cooled, filtered, precipitated, washed, and vacuum-dried at 60°C for 24 hours;

[0027] 4) Add the product of 3) into the sodium hydroxide solution with pH=7.5, stir at 180° C. for 1 h, and the stirring...

Embodiment 2

[0030] The present embodiment provides a kind of preparation method of graphene, is to make through the following steps:

[0031] 1) Dispersing graphite in azodicarbonamide foaming agent solution, stirring at constant temperature for 1 hour, and ultrasonically vibrating for 10 minutes, the ratio of graphite (g) to organic foaming agent (g) in parts by mass is 1:0.2;

[0032] 2) Keep the product of 1) in an oil bath at 150°C for 30 minutes at a constant temperature;

[0033] 3) After the product of 2) is cooled to normal temperature, it is added to a mixed solution of ethanol and concentrated nitric acid with a volume ratio of 5:1 to form a uniformly dispersed suspension with a concentration of 0.05g / mL, and the suspension is heated at 160°C Under hydrothermal reaction for 6 hours, the suspension was cooled, filtered, precipitated, washed, and vacuum-dried at 100°C for 12 hours;

[0034] 4) Add the product of 3) into the sodium hydroxide solution with pH=11, stir at 260° C. fo...

Embodiment 3

[0037] The present embodiment provides a kind of preparation method of graphene, is to make through the following steps:

[0038] 1) Dispersing graphite in an azodicarbonamide foaming agent solution, stirring at a constant temperature for 40 minutes, and ultrasonically oscillating for 15 minutes, the ratio of graphite (g) to organic foaming agent (g) in parts by mass is 1:0.1;

[0039] 2) Keep the product of 1) in an oil bath at 180°C for 1.5 hours at a constant temperature;

[0040] 3) After the product of 2) is cooled to normal temperature, it is added to a mixed solution of ethanol and concentrated nitric acid with a volume ratio of 10:1 to form a uniformly dispersed suspension, which is hydrothermally reacted at 90°C for 12 hours, and the suspended Liquid cooling, filtration, precipitation, washing, and vacuum drying at 70°C for 14 hours;

[0041] 4) Add the product of 3) into the sodium hydroxide solution with pH=8, stir at 190° C. for 40 min, and the stirring speed is 3...

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Abstract

The invention discloses a preparation method of graphene, which comprises the following steps: 1) dispersing graphite in an organic foaming agent solution, stirring at constant temperature for 30 minutes-1 hour, and carrying out ultrasonic oscillation for 10-30 minutes; 2) keeping the product in the step 1) at constant temperature in a 150-280-DEG C oil bath for 30 minutes-5 hours; 3) cooling the product in the step 2) to normal temperature, adding into a mixed solution of ethanol and concentrated nitric acid in a volume ratio of 30:1-50:10 to form a uniformly-dispersed 0.003-0.05g / mL suspension, carrying out hydrothermal reaction on the suspension at 80-160 DEG C for 6-48 hours, cooling the suspension, filtering, precipitating, washing, and drying; and 4) adding the product in the step 3) into a sodium hydroxide solution with the pH value of 7.5-11, and stirring at 180-260 DEG C for 30 minutes-1 hour. The preparation method disclosed by the invention greatly enhances the graphene yield.

Description

technical field [0001] The invention relates to the technical field of graphene, in particular to a preparation method of graphene. Background technique [0002] Many methods of preparing graphene have been explored, namely: [0003] Mechanical peeling method, the mechanical peeling method is to use the method of layer peeling to peel off the graphite sheet, because the graphite with a single layer structure is graphene, and the layers in the graphite structure are combined by π bonds. When the peeling force is greater than the π bond When the force is applied, the graphite flakes peel off. The mechanical exfoliation method is to separate the graphite into smaller fragments, and then select the thinner graphite flakes from the fragments, and then stick the two sides of the flakes with special plastic tape, tear the tape, and the flakes are divided into two. By repeating this process, thinner and thinner graphite flakes are obtained, and finally graphene, which is composed ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 金闯杨晓明
Owner JIANGSU SIDIKE NEW MATERIALS SCI & TECH CO LTD
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