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Method for preparing graphene oxide according to Fenton oxidation method

A Fenton oxidation and graphite technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of environmental pollution, non-recyclability, hindering the mass production of graphene oxide, etc., without special protection, change Expensive, changing the effect of difficult separation and purification

Inactive Publication Date: 2017-05-17
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • Method for preparing graphene oxide according to Fenton oxidation method
  • Method for preparing graphene oxide according to Fenton oxidation method

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Embodiment 1

[0029] Expanded graphite was prepared by 98wt% concentrated sulfuric acid and 30wt% hydrogen peroxide oxidative intercalation. In this example, 0.3g of natural flake graphite with a size of 180 μm and a carbon content of 90% was added to 10 mL H 2 SO 4 , 2 mL H 2 o 2 After stirring for 30 min and then standing at room temperature for 8 h, the flake graphite undergoes natural and gentle intercalation expansion, and the expansion volume is 30 mL. The pre-expanded graphite is vacuum filtered to collect the waste liquid for repeated use. Add 3mL of 1mol / L Fenton’s reagent and 9mL of 10% hydrogen peroxide to 0.3g of the pre-expanded graphite product. At this time, because the pre-expanded graphite has not been treated and the liquid environment is acidic, the graphite oxide product is obtained by hydrothermal reaction at 180°C for 6 hours, and then used Wash with deionized water repeatedly until the pH of the water phase is 7, then add 300mL of deionized water for 800W ultrasoni...

Embodiment 2

[0031] Adopt the method of the concentrated sulfuric acid of 98wt%, the hydrogen peroxide oxidative intercalation of 30wt% to prepare expanded graphite, in this embodiment, at first 3 g size is 23 μm carbon content and is 95% natural flake graphite and is added to 25 mL H 2 SO 4 , 2.5 mL H 2 o 2 After stirring for 10 min and then standing at room temperature for 4 h, the flake graphite undergoes natural and gentle intercalation expansion, and the expansion volume is 50 mL. The pre-expanded graphite is vacuum filtered, and the collected waste liquid is reused. Add 3mL of 3mol / L Fenton's reagent and 15mL of 30% hydrogen peroxide to 0.3g of the pre-expanded graphite product. At this time, because the pre-expanded graphite has not been treated and the liquid environment is acidic, the graphite oxide product is obtained by hydrothermal reaction at 100°C for 8 hours, and then used Repeated washing with deionized water until the pH of the water phase = 7, and then adding 800W ultr...

Embodiment 3

[0033] Adopt 98wt% concentrated sulfuric acid, the method for oxidative intercalation of 30wt% hydrogen peroxide to prepare expanded graphite, in the present embodiment, at first 20 g size is 270 μm and carbon content is 99% natural flake graphite is added to 50 mL H 2 SO 4 , 8 mL H 2 o 2After stirring for 20 min and then standing at room temperature for 3 h, the flake graphite undergoes natural and gentle intercalation expansion, and the expansion volume is 240 mL. The pre-expanded graphite is vacuum filtered, and the collected waste liquid is reused. Add 3mL of 2mol / L Fenton’s reagent and 24mL of 20% hydrogen peroxide to 0.3g of the pre-expanded graphite product. At this time, because the pre-expanded graphite has not been treated and the liquid environment is acidic, the graphite oxide product is obtained by hydrothermal reaction at 160°C for 10 hours, and then used Wash with deionized water repeatedly until the pH of the water phase is 7, then add 300mL of ethanol and w...

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Abstract

The invention discloses a method for preparing graphene oxide according to the Fenton oxidation method. The method disclosed by the invention comprises the following steps: taking natural crystalline flake graphite as a raw material, performing pre-expansion to increase the interlayer space of the graphite, and stimulating hydroxyl radical decomposed by hydrogen peroxide by a Fenton reagent under the hydrothermal condition to perform deep oxidation to prepare a graphite oxide product; cleaning the prepared graphite oxide and performing ultrasonic preparation in a solvent to obtain graphene oxide dispersion liquid; drying the graphene oxide dispersion liquid to obtain the graphene oxide powder. Strong acid and heavy metal oxidant are not needed in the preparation process, the aftertreatment process is simple and environmentally friendly, and the raw material is low in cost; furthermore, and the preparation process is simple, and the method is expected to prepare the graphene oxide in a large scale.

Description

technical field [0001] The invention relates to a method for preparing graphene oxide by a Fenton oxidation method. Background technique [0002] Since the concept of 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 many literature reviews at ...

Claims

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Application Information

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IPC IPC(8): C01B32/198
CPCC01P2002/82C01P2004/03
Inventor 阎兴斌杨娟
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI