A kind of three-dimensional graphene macrobody and preparation method thereof

A graphene macro-body, graphene technology, applied in the field of graphene, can solve problems such as inability to carry out directional mass transfer or transmission

Active Publication Date: 2018-05-15
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing three-dimensional macroscopic body obtained based on the self-assembly process has a network structure of disordered connections inside, and neither the graphene matrix nor the spatial channel in the macroscopic body can perform directional mass transfer or transport.

Method used

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  • A kind of three-dimensional graphene macrobody and preparation method thereof
  • A kind of three-dimensional graphene macrobody and preparation method thereof
  • A kind of three-dimensional graphene macrobody and preparation method thereof

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preparation example Construction

[0032] The present invention also provides a preparation method of the above-mentioned three-dimensional graphene macrobody, comprising the following steps: S1) mixing and reacting graphene oxide with a reducing agent to obtain partially reduced graphene oxide; S2) oxidizing the partially reduced Graphene is subjected to sulfonation reaction to obtain sulfonated graphene oxide; S3) mixing and reacting the sulfonated graphene oxide with a reducing agent to obtain sulfonated graphene; S4) combining the sulfonated graphene with polyhydroxy The compounds are mixed for hydrothermal reaction, and then freeze-dried to obtain a three-dimensional graphene macrobody.

[0033] The present invention uses graphene oxide as a raw material, which can be self-made or commercially available without special limitations. The present invention is preferably graphene oxide prepared by the improved Hummers method, and is more preferably prepared according to the following steps:

[0034] A) graphit...

Embodiment 1

[0060] Configure 6mg / ml sulfonated graphene aqueous solution, add 1ml of 30mg / ml polyvinyl alcohol (PVA, MW is 75000 ~ 80000) to 5ml of sulfonated graphene solution, ultrasonic 10min to make it fully mixed; The mixed solution of acidified graphene and PVA was placed in a high-pressure reactor and sealed, and hydrothermally reacted at 180°C for 6 hours to form a hydrogel; then, a layered three-dimensional graphene macroscopic body was obtained by freeze-drying.

[0061] Utilize scanning electron microscope to analyze the three-dimensional graphene macrobody obtained in embodiment 1, obtain its SEM picture, as figure 1 shown. Depend on figure 1 It can be seen that the interlayer spacing of the three-dimensional graphene macroscopic body obtained in Example 1 is 5-10 μm.

Embodiment 2

[0063] Configure 6mg / ml sulfonated graphene aqueous solution, add 1ml of 15mg / ml polyvinyl alcohol (PVA, MW is 75000 ~ 80000) to 5ml of sulfonated graphene solution, ultrasonic 10min to make it fully mixed; The mixed solution of acidified graphene and PVA was placed in a high-pressure reactor and sealed, and hydrothermally reacted at 180°C for 6 hours to form a hydrogel; then, a layered three-dimensional graphene macroscopic body was obtained by freeze-drying.

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Abstract

The invention provides a three-dimensional graphene macro material and a preparation method thereof. The method comprises the following steps: S1, mixing graphene oxide with a reducing agent to react and obtain partially-reduced graphene oxide; S2, causing the partially-reduced graphene oxide to be subjected to a sulfonation reaction to obtain sulfated graphene oxide; S3, mixing the sulfated graphene oxide with the reducing agent to react and obtain sulfated graphene; and S4, mixing the sulfated graphene with a polyhydroxy compound to carry out a hydrothermal reaction and obtain the three-dimensional graphene macro material. Compared with the prior art, functional groups of different positions including the surface and the edge of a graphene oxide sheet layer are regulated, so that the functional groups have selectivity on cross-linking effect of a cross-linking agent and induce the graphene oxide sheet layer to present orientation in construction of a 3D macrostructure; meanwhile, the influence on the growth of ice crystals in the subsequent freeze drying process can be avoided; the three-dimensional graphene macrostructure with a sequential layered structure can be finally prepared.

Description

technical field [0001] The invention belongs to the technical field of graphene, in particular to a method for preparing a three-dimensional graphene macroscopic body. Background technique [0002] Graphene is a carbon atom with sp 2 The hybridized orbitals form a hexagonal planar film with a honeycomb lattice, a two-dimensional material with a thickness of only one carbon atom. Since its discovery in 2004, this unique material has attracted widespread attention due to its multiple excellent properties. Thanks to its good mechanical and electrical properties, three-dimensional macroscopic materials based on two-dimensional graphene materials also have broad application prospects. [0003] At present, the preparation methods of graphene three-dimensional macroscopic materials are mainly divided into two categories: template method and self-assembly method. Among them, the template method is mainly chemical vapor deposition (CVD), and the surface of the prepared graphene thr...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C01B32/184
CPCC01P2004/03C01P2004/30
Inventor方齐乐周旭峰刘兆平
OwnerNINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI