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Method for rapidly preparing high specific surface area graphene oxide

A high specific surface area, graphene technology, applied in chemical instruments and methods, inorganic chemistry, carbon compounds, etc., can solve the problems of prolonging freeze-drying treatment time, lengthy preparation cycle, improving vacuum degree, etc., achieving environmental friendliness and simple process. , easy to operate effect

Inactive Publication Date: 2014-08-27
ZHANGJIAGANG DONGDA IND TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

As mentioned above, graphite oxide obtained by chemical oxidation methods such as Brodie method, Hummers method and Staudenmaier method has a large number of oxygen-containing groups such as hydroxyl, carboxyl and epoxy groups in its structure, and its compatibility with water is very good. , and can form a good interaction through hydrogen bonds and other methods. Therefore, when sublimating and removing water molecules, the vacuum degree has to be increased and the freeze-drying treatment time must be extended. It often takes more than 72 hours to dry completely, and the preparation cycle is too long.

Method used

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  • Method for rapidly preparing high specific surface area graphene oxide
  • Method for rapidly preparing high specific surface area graphene oxide
  • Method for rapidly preparing high specific surface area graphene oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Using the Brodie method, 2g of natural flake graphite (80 mesh sieve) is oxidized to obtain graphite oxide with a carbon-to-oxygen ratio (C / O)=4.2; configure tert-butanol / water mixing volume ratio of 0.3:1 for freeze-drying medium, and stir and disperse graphite oxide in tert-butanol / water mixed solvent to obtain a uniformly dispersed suspension. Place the graphite oxide suspension in the cold trap of a freeze dryer for rapid freezing at -55°C, then turn on the vacuum pump to keep the vacuum in the freezing chamber below 30Pa, and keep this state for 45 hours until the solvent is completely sublimated, and then you can get dry Sponge-like graphene oxide ( figure 1 ).

[0037] The observation of the morphology by scanning electron microscope found that the three-dimensional cross-linked structure of graphene oxide was intact without collapse, the carbon ring sheets were fully peeled off, and the structure was loose ( figure 2 ). Using the specific surface area and po...

Embodiment 2

[0039] Using the Hummers method, 5g of natural flake graphite (100 mesh sieve) is oxidized to obtain graphite oxide with a carbon-to-oxygen ratio (C / O)=3.6; configure tert-butanol / water mixing volume ratio of 1:1 for freeze-drying medium, and stir and disperse graphite oxide in tert-butanol / water mixed solvent to obtain a uniformly dispersed suspension. Place the graphite oxide suspension in the cold trap of a lyophilizer for rapid freezing at -40°C, then turn on the vacuum pump to keep the vacuum in the freezing chamber below 50 Pa, and keep this state for 37 hours until the solvent is completely sublimated, and then you can get dry Sponge-like graphene oxide.

[0040] The observation of the morphology by scanning electron microscope found that a large number of irregular cross-linked holes run through the three-dimensional structure of graphene oxide, and the cross-linked structure is intact without collapse. Using the specific surface area and porosity analyzer, the BET sp...

Embodiment 3

[0042] Using the Staudenmaier method, 3g of artificial graphite powder (200 mesh sieve) is oxidized to obtain graphite oxide with a carbon-to-oxygen ratio (C / O)=4.1; configure tert-butanol / water mixing volume ratio of 4:1 for freeze-drying medium, and stir and disperse graphite oxide in tert-butanol / water mixed solvent to obtain a uniformly dispersed milky mixed solution. Put the graphite oxide emulsion in the cold trap of the lyophilizer for rapid freezing at -15°C, then turn on the vacuum pump to keep the vacuum in the freezing chamber below 50Pa, and keep this state for 46 hours until the solvent is completely sublimated, and the dry sponge can be obtained graphene oxide.

[0043] The observation of the morphology by scanning electron microscope found that the graphene oxide product maintained a good three-dimensional stacked structure hole, and the cross-linked structure was intact without collapse. Using the specific surface area and porosity analyzer, the BET specific s...

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Abstract

The invention discloses a method for rapidly preparing high specific surface area graphene oxide. The method comprises the following steps: (1) preparing a graphene oxide precursor by utilizing a chemical oxidation method; (2) preparing a tertiary butanol and water mixed medium; (3) dispersing the graphene oxide precursor in the tertiary butanol and water mixed medium, and preparing uniformly dispersed suspension or emulsion; and (4) performing vacuum freeze-drying treatment on the graphene oxide suspension or emulsion, thus obtaining the graphene oxide of which the superficial area is increased. The relative ratio of the tertiary butanol / water mixed medium is regulated, so that the freeze-drying period and stripping degree of the graphene oxide can be regulated. According to the preparation method, due to introduction of the tertiary butanol, the preparation period is effectively shortened, the production cost is reduced, the production process is simplified, the structural properties of the graphene oxide product are improved, and the specific surface area is increased.

Description

technical field [0001] The invention relates to the synthesis of functional materials in the technical field of chemistry and chemical engineering, in particular to a rapid preparation method for shortening the preparation period and increasing the specific surface area of ​​graphene oxide. Background technique [0002] Graphene has a series of excellent functional properties and is an outstanding representative in the field of functional materials. Since Professor Geim of the United Kingdom won the 2010 Nobel Prize for discovering graphene, the synthesis and application of graphene has aroused people's great interest. big concern. Traditional crystalline materials are all three-dimensional structures. The emergence of graphene has changed the long-standing view that two-dimensional crystals cannot exist stably. The ultra-high specific surface area of ​​two-dimensional crystals makes them have obvious advantages in the fields of catalyst supports, flexible electrodes, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/198
Inventor 王继刚丁滔黄珊
Owner ZHANGJIAGANG DONGDA IND TECH RES INST
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