High-efficiency catalysis macroscopic quantity preparation method for graphene oxide or compound thereof reduced and peeled based on microwaves

A technology of graphene and composites, which is applied in the field of high-efficiency catalytic macro-preparation, can solve the problems that have not been reported, long time of microwave irradiation of graphite oxide, unsatisfactory peeling effect, etc., and achieve good peeling effect

Inactive Publication Date: 2017-05-10
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the reaction time of microwave-irradiated graphite oxide without a catalytic system is relatively long, and the stripping effect in the air atmosphere is not ideal. The efficient catalytic macro-preparation method based on this has not yet been reported.

Method used

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  • High-efficiency catalysis macroscopic quantity preparation method for graphene oxide or compound thereof reduced and peeled based on microwaves
  • High-efficiency catalysis macroscopic quantity preparation method for graphene oxide or compound thereof reduced and peeled based on microwaves
  • High-efficiency catalysis macroscopic quantity preparation method for graphene oxide or compound thereof reduced and peeled based on microwaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Take ordinary graphite powder and apply the improved Hummers method, that is, take a small amount (about 300 mesh) and add 0.5-5 g of sodium nitrate powder and 30-120 ml of concentrated sulfuric acid, and slowly add 1-9 g of potassium permanganate in a cold water bath. Stir and react in a water bath between 40~45 °C for 1~4 h, then add a small amount of water, continue to react for 10~50 min, then add a large amount of water above 100 ml, react for 5~20 min, add an appropriate amount of hydrogen peroxide until the solution turns golden yellow.

[0037] After the solution was left to settle, discard the supernatant, add an appropriate amount of 5% to 20% hydrochloric acid, divide it into centrifuge tubes and centrifuge at a high speed (10000~15000 r / min), discard the supernatant, and then centrifuge and wash with water until neutral. , collect the product after washing with water, add an appropriate amount of deionized water for ultrasonic dispersion, and then centrifuge...

Embodiment 2

[0040] Obtain the freeze-dried GO product according to the method in the above-mentioned Example 1, put it into a beaker, sprinkle a trace amount (3.11 mg) of flake graphite powder (200 mesh) on its surface, and put it into a microwave oven for microwave irradiation (500~1000 W), under the catalysis of graphite flakes, the reaction started about 2 s after turning on the microwave, accompanied by a strong plasma arc, the reaction was completed in about 9 s, and a large number of microwave-assisted reduction and exfoliation graphene flocs (MEGO) were obtained. Raman and high-resolution transmission electron microscope characterization results prove that the product is high-quality graphene.

Embodiment 3

[0042]Obtain the freeze-dried GO product according to the method in the above-mentioned Example 1, put it into a beaker, sprinkle a trace amount (1.27mg) of flake graphite powder (325 mesh) on its surface, and put it into a microwave oven for microwave irradiation (500~1000 W), under the catalysis of flake graphite, the reaction starts instantly after turning on the microwave (the time interval is less than 1 s), accompanied by a strong plasma arc, the reaction is completed in about 6 s, and the microwave-assisted reduction and exfoliation of graphene flocs (MEGO) is obtained , but the amount is relatively small compared with the previous example, because the smaller the particle size, the stronger the ability to induce plasma, and the resulting local high-energy environment leads to the loss of part of the generated graphene due to the reaction with oxygen. Raman and high-resolution transmission electron microscope characterization results prove that the product is high-qualit...

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Abstract

The invention belongs to the technical field of preparation of graphene and particularly relates to a high-efficiency catalysis macroscopic quantity preparation method for graphene oxide or a compound thereof reduced and peeled based on microwaves. Aiming at solving the problems in a process of reducing the graphene oxide by the microwaves that the reaction time is long (30min or more under a 700W air atmosphere and about 15min under a W air atmosphere) and the peeling effect is not ideal, the method adopts flake graphite powder (with the size of 80-120 meshes) which is cheap and easy to obtain, and trace flake graphite powder is added into a microwave reduction system of the graphene oxide or the compound thereof; a partial ultrahigh-energy environment is realized by utilizing plasmas generated under a microwave environment, and the graphene oxide or the compound thereof is reduced and peeled instantly; and meanwhile, the method has a good quasi-single-layer peeling effect. The method has the advantages that the preparation is simple, raw materials are cheap and easy to obtain, no pollution is caused, and the efficiency is high, so that the method has large-scale industrial production values.

Description

technical field [0001] The invention belongs to the technical field of graphene preparation, in particular to a method for efficient catalytic macro-preparation of graphene oxide (GO) or its composites based on microwave reduction reduction. Background technique [0002] Graphene refers to sp 2 A two-dimensional atomic crystal material composed of carbon atoms, it has excellent electrical, thermal and mechanical properties, and has a unique two-dimensional macromolecular structure; this makes graphene the choice of solar cells, light-emitting diodes, ITO and FTO transparent electrodes, Methanol fuel cells, biomimetic oxidation catalysts, and supercapacitors have broad application prospects. [0003] Macroscopically speaking, synthetic graphene is mainly divided into two types of synthesis ideas: bottom-up and top-down. The bottom-up method mainly includes epitaxial growth method and chemical vapor deposition (CVD), and the top-down method mainly includes Including ultrason...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/192
CPCC01B2204/04C01B2204/30C01P2002/82C01P2004/03
Inventor 徐宇曦刘润泽宁振兼刘晶晶张宇姜天才卜凡兴杨阳
Owner FUDAN UNIV
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