Method for preparing size-controlled graphene oxide by clean oxidation technology

A technology of graphene and graphene dispersion liquid, which is applied in the field of graphene oxide, can solve the problems that hinder the mass production of graphene oxide, waste of water resources and energy, and non-recyclable utilization, so as to change the difficulty of separation and purification and make the process safe and controllable , changing the costly effect

Active Publication Date: 2016-12-07
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, the preparation of graphene oxide in the above preparation methods requires the introduction of a large amount of acid solution and strong oxidant, resulting in a serious waste of water resources and energy in order to remove a large amount of acid solution and strong oxidant in the purification stage. , and these strong oxidants all have heavy metal ions, which cannot be recycled, causing irreversible serious pollution to the environment, thus hindering the mass production of graphene oxide

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  • Method for preparing size-controlled graphene oxide by clean oxidation technology
  • Method for preparing size-controlled graphene oxide by clean oxidation technology
  • Method for preparing size-controlled graphene oxide by clean oxidation technology

Examples

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Embodiment 1

[0026] Using 98wt% concentrated sulfuric acid and potassium permanganate as the oxidation intercalation method to prepare expandable graphite, in this example, 10 g of natural flake graphite with a size of 23 μm was added to 50 mL H 2 SO 4 , 2g KMnO 4 The mixture was stirred for 30 min and then allowed to stand at room temperature for 1 h to prepare expandable graphite. After cleaning the expandable graphite, take out 0.3g, add 0.5mL of 28% ammonia water and 10mL of 30% hydrogen peroxide, then add water to dilute to 30mL, and react in water at 180°C for 6h to obtain the graphite oxide product, then wash the graphite oxide product with deionized water until the water Phase pH = 7, then add 300mL deionized water and 800W ultrasonic dispersion to obtain graphene oxide aqueous dispersion; freeze-dry to prepare graphene oxide powder.

Embodiment 2

[0028] Using 98wt% concentrated sulfuric acid and potassium permanganate as an oxidation intercalation method to prepare expandable graphite, in this example, 10 g of natural flake graphite with a size of 80 μm was first added to 50 mL H 2 SO 4 , 2g KMnO 4 The mixture was stirred for 30 min and then allowed to stand at room temperature for 1 h to prepare expandable graphite. After cleaning the expandable graphite, take out 1g, add 1mL of 28% ammonia water and 5mL of 30% hydrogen peroxide, then add water to dilute to 30mL, and react in water at 100°C for 8h to obtain the graphite oxide product, then wash the graphite oxide product with deionized water until the pH of the water phase =7, then add 800W ultrasonic dispersion in 300mL DMF to obtain graphene oxide aqueous dispersion; spray drying to prepare graphene oxide powder.

Embodiment 3

[0030] Using 98wt% concentrated sulfuric acid and potassium permanganate as an oxidation intercalation method to prepare expandable graphite, in this example, 10 g of natural flake graphite with a size of 75 μm was added to 50 mL H 2 SO 4 , 2g KMnO 4The mixture was stirred for 30 min and then allowed to stand at room temperature for 1 h to prepare expandable graphite. After cleaning the expandable graphite, take out 1g, add 1mL of 28% ammonia water and 8mL of 30% hydrogen peroxide, and then add water to dilute to 60mL. At this time, because the pre-expanded graphite has not been treated, the liquid environment is acidic, and the hydrothermal reaction at 160°C for 10h produces graphite oxide. Afterwards, the graphite oxide product was washed with deionized water until the pH of the water phase was 7, and then 800W ultrasonic dispersion was added to a mixture of 300mL ethanol and water to obtain a graphene oxide water dispersion; spray drying was used to prepare a graphene oxid...

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Abstract

The invention discloses a method for preparing size-controlled graphene oxide by a clean oxidation technology. The method comprises the following steps: performing pre-oxidization on natural flake graphite serving as a raw material to increase a gap between graphite layers and add an oxidization functional group on the edge, enabling ammonium hydroxide and hydrogen peroxide to act jointly under a hydrothermal condition to protect a flake graphite layer from being sheared too small, and performing deep oxidization by a hydroxyl radical produced by hydrogen peroxide excitation to prepare a graphite oxide product; cleaning the prepared graphite oxide, and performing ultrasonic treatment in a solvent to prepare a graphene oxide dispersing solution; drying the graphene oxide dispersing solution to obtain graphene oxide powder. In the preparation process, no strong acid and no heavy metal oxidant are needed; the post-treatment process is simple and environment-friendly; the raw materials are low in cost; furthermore, the preparation process is simple, and the method is a method expected to be used for preparing the graphene oxide in a large scale.

Description

technical field [0001] The invention relates to a method for preparing size-controllable graphene oxide by clean oxidation technology. Background technique [0002] Since the concept of graphene (Graphene) was proposed by the research group led by A.K. Geim of the University of Manchester in 2004, graphene, as another bright star in the carbon family, has been highly valued by physics, chemistry and materials scientists. Therefore, graphite Graphene has become another "universal material" that shines after carbon nanotubes (Science 2004, 306:666.). Compared with carbon nanotubes, graphene has a perfect hybrid structure, and has attracted much attention for its ultra-high electrical conductivity, extremely fast electron transport speed, high hardness, high specific surface area, and room temperature quantum Hall effect (Nat. Mater . 2007, 6, 183; Science 2009, 324, 1530.). So far, researchers have conducted extensive research on the preparation of graphene, and there are ma...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01P2002/82C01P2004/03
Inventor 阎兴斌杨娟
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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