Preparation method of graphene oxide

A graphene and graphite technology, applied in the field of preparation of graphene oxide, can solve the problems of destroying the structural integrity of reduced GO, reducing the yield of GO exfoliation, prolonging the reaction time, etc., and achieving high exfoliation yield suitable for large-scale industrial production. , the effect of low reaction temperature

Pending Publication Date: 2022-04-15
无锡漆好环保新材料研究有限公司
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  • Claims
  • Application Information

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Problems solved by technology

However, when water is added, especially at higher temperatures, prolonged reaction times lead to some disadvantages
For example, cracks and holes appear in the GO layer, which leads to the fracture of GO due to excessive oxidation
In addition, water-enhanced oxidation usually produces a large number of irreparable defects at the edges, which seriously damages the structural integrity of reduced GO (rGO)
However, if no water is added during the reaction, the stripping yield of GO will be reduced.

Method used

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  • Preparation method of graphene oxide
  • Preparation method of graphene oxide

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Embodiment 1

[0041] As a method for preparing graphene oxide according to an embodiment of the present invention, the method comprises the following steps: (1) sputtering a certain amount of flake graphite in a plasma cleaning machine with air plasma for 30 minutes to obtain modified flake graphite; (2) In an ice bath, 25mL of concentrated sulfuric acid is added to a beaker, and slowly add 3g of potassium permanganate under magnetic stirring to form a dark green solution; (3) slowly add 1g of modified flake graphite; (4) transfer it to In a water bath at 35 degrees Celsius, react for 4 hours at a stirring speed of 350 rpm; (5) pour the mixture into 50 mL of ice water, then add 3 mL of 30% hydrogen peroxide, and stir fully with a glass rod; (6) add water to wash, and the flaky crystals naturally settle, After there is a clear boundary, pour out the supernatant, add water and wash it several times until it is neutral, and then graphene oxide is obtained. The exfoliation yield of GO was 96%. ...

Embodiment 2

[0043]As a method for preparing graphene oxide according to an embodiment of the present invention, the method comprises the following steps: (1) sputtering a certain amount of flake graphite in a plasma cleaning machine with air plasma for 30 minutes to obtain modified flake graphite; (2) In an ice bath, 40mL of concentrated sulfuric acid is added to a beaker, and slowly add 4g of potassium permanganate under magnetic stirring to form a dark green solution; (3) slowly add 1g of modified flake graphite; (4) transfer it to In a water bath at 35 degrees Celsius, react for 4 hours at a stirring speed of 350 rpm; (5) pour the mixture into 80 mL of ice water, then add 6 mL of 30% hydrogen peroxide, and stir thoroughly with a glass rod; (6) add water to wash, and the flaky crystals naturally settle, After there is a clear boundary, pour out the supernatant, add water and wash it several times until it is neutral, and then graphene oxide is obtained. The exfoliation yield of GO was 9...

Embodiment 3

[0045] As a method for preparing graphene oxide according to an embodiment of the present invention, the method comprises the following steps: (1) sputtering a certain amount of flake graphite in a plasma cleaning machine with air plasma for 30 minutes to obtain modified flake graphite; (2) In an ice bath, 50mL of concentrated sulfuric acid is added to a beaker, and slowly add 5g of potassium permanganate under magnetic stirring to form a dark green solution; (3) slowly add 1g of modified flake graphite; (4) transfer it to In a water bath at 35 degrees Celsius, react for 4 hours at a stirring speed of 350 rpm; (5) pour the mixture into 100 mL of ice water, then add 8 mL of 30% hydrogen peroxide, and stir fully with a glass rod; (6) add water to wash, and the flaky crystals naturally settle, After there is a clear boundary, pour out the supernatant, add water and wash it several times until it is neutral, and then graphene oxide is obtained. The exfoliation yield of GO was 99%....

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Abstract

The invention provides a preparation method of graphene oxide, and belongs to the field of material preparation. The method comprises the following steps: (1) carrying out plasma sputtering on graphite to obtain modified graphite; (2) adding potassium permanganate into concentrated sulfuric acid, and uniformly mixing to obtain a mixture A; (3) adding the modified graphite in the step (1) into the mixture A to obtain a mixture B; (4) reacting the mixture B at 25-60 DEG C for 2-6 hours to obtain a mixture C; (5) adding the mixture C into ice water, adding hydrogen peroxide, and uniformly mixing; and (6) adding water into the product obtained in the step (5), and washing until the product is neutral, thereby obtaining the precipitate, namely the graphene oxide. The stripping yield of the graphene oxide reaches up to 95% or above, and the dosage of concentrated sulfuric acid and potassium permanganate is effectively reduced. The method is high in stripping yield, low in cost, small in danger, rapid and simple in reaction process and very suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a preparation method of graphene oxide. Background technique [0002] In the past ten years, two-dimensional materials such as graphene, molybdenum disulfide, and black scale have attracted extensive attention because of their excellent optical, electrical, magnetic, and thermal properties. At present, many literatures at home and abroad have reported that two-dimensional materials have great application potential in the fields of catalysis, energy storage, heat conduction, and metal corrosion protection. For large-scale application, the most fundamental problem is to solve the problem of low-cost preparation of two-dimensional materials. [0003] Since single-layer graphene was produced by tape tearing method in 2004, inspired by this, many researchers have developed many methods for producing two-dimensional nanosheets: such as ion exchange stripping method, liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198
CPCC01B32/198
Inventor 顾林丰景朱野
Owner 无锡漆好环保新材料研究有限公司
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