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A method for large-scale preparation of graphene

A graphene and graphite technology, applied in the field of large-scale graphene preparation, can solve the problems that functional groups cannot be successfully peeled off, graphene performance is not ideal, and the oxidation degree of graphite oxide is high, so as to avoid damage to the graphene sheet structure, and easy to scale. The effect of chemical production and less structural defects

Active Publication Date: 2020-05-08
GUANGDONG JUSHI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN102107870A discloses a method for rapidly preparing graphene using microwaves. First, graphite oxide is ground into fine powder, and then microwave radiation is carried out in a high vacuum state to obtain graphene. However, the method has a lengthy preparation process and requires high vacuum conditions, The disadvantages of high equipment requirements and high equipment preparation cost cannot be widely used; the paper "Preparation of functionalized graphene by microwave solid phase exfoliation method and its electrochemical capacitance performance" (Journal of Inorganic Chemistry, 2010, 26(8): 1375 ~1381)" also discloses a method for preparing graphene using microwaves. First, graphene oxide is prepared by the Hummers method, and then graphene is prepared by heating in a microwave oven. Therefore, many functional groups cannot be successfully stripped during stripping, resulting in unsatisfactory performance of the prepared graphene

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A method for large-scale preparation of graphene, comprising the following steps:

[0039] 1) 5g of graphite, 5g of potassium permanganate and 100mL of sulfuric acid with a mass fraction of 70% were mixed evenly, stirred and reacted at 70°C for 60min, then 100mL of deionized water and 10mL of hydrogen peroxide solution with a mass fraction of 10% were added, and stirred for 5min. Centrifuge at 8000r / min for 5min to obtain intercalated graphite;

[0040] 2) Disperse the intercalated graphite with 15 mL of deionized water (the moisture content of the intercalated graphite after water dispersion is 75%), then place it in a microwave reactor, fill it with nitrogen protection, irradiate with 800W microwave for 5 minutes, and filter to obtain graphene.

[0041] After testing, the electrical conductivity of the graphene prepared in this embodiment>1250S / cm, its TEM figure is as follows figure 1 shown.

Embodiment 2

[0043] A method for large-scale preparation of graphene, comprising the following steps:

[0044] 1) 5g of graphite, 5g of potassium permanganate and 80mL of sulfuric acid with a mass fraction of 90% were mixed uniformly, stirred and reacted at 50°C for 100min, then 100mL of deionized water and 10mL of hydrogen peroxide solution with a mass fraction of 10% were added, and stirred for 5min. Centrifuge at 8000r / min for 5min to obtain intercalated graphite;

[0045] 2) Disperse the intercalated graphite with 20mL of deionized water (the moisture content of the intercalated graphite after dispersing with water is 80%), then place it in a microwave reactor, fill it with nitrogen protection, irradiate with 1000W microwave for 5min, and filter to obtain graphene.

[0046] After testing, the electrical conductivity of the graphene prepared in this example is >1300 S / cm.

Embodiment 3

[0048] A method for large-scale preparation of graphene, comprising the following steps:

[0049] 1) 5g of graphite, 5g of potassium permanganate and 150mL of sulfuric acid with a mass fraction of 50% were mixed evenly, stirred and reacted at 90°C for 120min, then 75mL of deionized water and 15mL of hydrogen peroxide solution with a mass fraction of 10% were added, and stirred for 5min. Centrifuge at 8000r / min for 5min to obtain intercalated graphite;

[0050] 2) Disperse the intercalated graphite with 30 mL of deionized water (the moisture content of the intercalated graphite after dispersing with water is 85%), then place it in a microwave reactor, fill it with nitrogen protection, irradiate with 1000W microwave for 8 minutes, and filter to obtain graphene.

[0051] After testing, the electrical conductivity of the graphene prepared in this example is >1100 S / cm.

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Abstract

The invention discloses a method for large-scale preparation of graphene. The method comprises the following steps that 1, graphite, potassium permanganate and sulfuric acid are mixed to be uniform, astirring reaction is performed under the temperature of 0-100 DEG C for 10-120 min, water and a hydrogen peroxide solution are added, a stirring reaction is performed for 1-15 min, and solid-liquid separation is performed to obtain intercalation graphite; 2, the intercalation graphite is dispersed by water and then placed into a microwave reactor, shielding gas is introduced, the microwave reaction is performed for 1-15 min, and solid-liquid separation is performed to obtain graphite. The method is simple in technology, short in flow path, mild in reaction condition and low in cost, and facilitates large-scale production, the prepared graphene is excellent in performance and has few structural defects, the quality stability of different batches is good, and the wide application prospect in multiple fields is achieved.

Description

technical field [0001] The invention relates to a method for large-scale preparation of graphene. Background technique [0002] Graphene is a honeycomb planar film formed by sp2 hybridization of carbon atoms. It has a unique two-dimensional nanostructure and has the advantages of high electron transfer rate, good electrical conductivity, and high thermal conductivity. Nanomaterials, which are the thinnest but hardest and have the best electrical and thermal conductivity, have good application prospects in physics, materials science, electronic information, computers, aerospace and other fields. [0003] At present, the preparation methods of graphene mainly include: mechanical exfoliation method, vapor phase deposition method, liquid phase exfoliation method and redox method, etc. Among them, the oxidation-reduction method is currently recognized as a method for obtaining graphene in large quantities at low cost. The preparation of graphene by redox method includes two pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/19
CPCC01B2204/22C01P2004/04
Inventor 梁亚涛陈钢杨正高朱红芳
Owner GUANGDONG JUSHI CHEM CO LTD
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