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Graphene oxide preparation method with controllable inter-layer spacing

A graphene, interlayer spacing technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long reaction time, small interlayer spacing, complex processing, etc., to achieve short experimental period, large interlayer spacing, experimental simple conditional effect

Active Publication Date: 2019-04-12
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem to be solved by the present invention is to provide a method for preparing graphene oxide with controllable layer spacing, which overcomes the disadvantages of the existing Hummers method Tours method for preparing graphene oxide, either the layer spacing is small, or the pretreatment is complicated, dangerous, long reaction time

Method used

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  • Graphene oxide preparation method with controllable inter-layer spacing
  • Graphene oxide preparation method with controllable inter-layer spacing
  • Graphene oxide preparation method with controllable inter-layer spacing

Examples

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Effect test

Embodiment 1

[0024] The specific steps of the preparation method of graphene oxide in the present embodiment are as follows:

[0025] (1) Add 1 mL of concentrated H 2 SO 4 , 0.2gK 2 S 2 o 8 and 1gNaNO 3 Add it to a 50mL flask, stir vigorously in an ice-water bath for 1h, add 2g of graphite powder, stir for 0.2h until the color of the mixture turns black, raise the temperature to 80°C and continue the reaction for 0.2h, stop stirring, cool to room temperature, and use Diluted with ionized water, filtered to obtain a solid, washed to neutral, and dried for later use;

[0026] (2) All the solids obtained in the previous step were added to a 250mL flask, and then 10mL of concentrated H 2 SO 4 , slowly add 1gKMnO 4 , keep at 20°C for 1h, raise the temperature to 30°C for 1h, slowly add 100mL deionized water to the mixture, raise the temperature to 95°C, continue stirring for 15 minutes; cool to room temperature, add 1mL 30wt% H 2 o 2 , stirred for a while to obtain a mixed solution; ...

Embodiment 2

[0029] The specific steps of the chemical preparation method of graphene oxide in the present embodiment are as follows:

[0030] (1) Add 1 mL of concentrated H 2 SO 4 , 1gK 2 S 2 o 4 and 0.2g NaNO 3 Add it to a 50mL flask, stir vigorously in an ice-water bath for 0.2h, add 5g of graphite powder, and stir for 0.2h until the color of the mixture turns black, raise the temperature to 60°C and continue the reaction for 1h, stop stirring, cool to room temperature, and use Diluted with ionized water, filtered to obtain a solid, washed to neutral, and dried for later use;

[0031] (2) All the solids obtained in the previous step were added to a 250mL flask, and then 45mL of concentrated H 2 SO 4 , slowly add 6gKMnO 4 , keep at 10°C for 0.2h, raise the temperature to 40°C for 2h, slowly add 100mL of deionized water to the mixture, raise the temperature to 100°C, continue stirring for 5 minutes; cool to room temperature, add 6mL of 30wt% H 2 o 2 , stirred for a while to obta...

Embodiment 3

[0034] The specific steps of the chemical preparation method of graphene oxide in the present embodiment are as follows:

[0035] (1) Dissolve 5 mL of concentrated H 2 SO 4 , 1gK 2 S2 o 4 and 1gNaNO 3 Add it into a 50mL flask, stir vigorously in an ice-water bath for 1h, add 2g of graphite powder, and stir for 1h until the color of the mixture turns black, raise the temperature to 80°C and continue the reaction for 0.2h, stop stirring, cool to room temperature, and use a deionized Dilute with water, filter to obtain a solid, wash until neutral, and dry for later use;

[0036] (2) All the solids obtained in the previous step were added to a 250mL flask, and then 45mL of concentrated H 2 SO 4 , slowly add 6gKMnO 4 , keep at 10°C for 1h, raise the temperature to 30°C for 15h, slowly add 150mL of deionized water to the mixture, raise the temperature to 95°C, continue stirring for 15 minutes; cool to room temperature, add 6mL of 30wt% H 2 o 2 , stirred for a while to obtai...

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Abstract

The invention relates to a graphene oxide preparation method with controllable inter-layer spacing. The preparation method includes the following steps that 1, graphene powder is pre-oxidized in a concentrate-sulfuric acid environment, and solids are washed to be neutral and aired for usage; 2, a pre-oxidation product is increased in temperature through multiple steps for secondary oxidation underthe effects of potassium permanganate and concentrated sulfuric acid strong oxidant; 3, centrifugal separation is conducted, and freeze drying is conducted to obtain graphene oxide. The method has the advantages that the inter-layer spacing of the prepared graphene oxide is large; by changing experimental conditions, graphene oxides with kinds of inter-layer spacing are prepared under control. Agood microenvironment is provided for preparation of an organic-inorganic intercalation compound, and the graphene oxide has broad application prospects in the fields of preparation of compound materials, ocean corrosion prevention, fouling prevention and others.

Description

technical field [0001] The invention belongs to the technical field of graphene oxide preparation, and relates to a method for preparing graphene oxide with controllable interlayer spacing by a two-step oxidation method. Background technique [0002] Graphene is a single-atom-thick self-supporting two-dimensional crystal composed of carbon atoms with SP 2 The honeycomb planar film formed by hybridization, due to its special structure, graphene exhibits some excellent properties, including high electrical conductivity, high thermal conductivity, high optical properties and high mechanical strength, and has become a popular choice in materials science, physics, chemistry and one of the research hotspots in the field of nanotechnology. Graphene oxide is the product of chemical oxidation and exfoliation of graphite powder. It is characterized by rich surface functional groups, which improves its water solubility, wettability and surface activity, making graphene oxide more effe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/198
CPCC01B2204/20C01B32/198
Inventor 郑豪程昱升陈建芳
Owner ZHEJIANG UNIV
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