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Method for preparing graphene/MOF (metal-organic framework) porous composite material aquagel and graphene/MOF porous composite material aerogel

A porous composite material and graphene technology, which is applied in the field of preparation of graphene/metal organic framework compound porous composite hydrogel and aerogel, can solve the problem of long time-consuming stirring and mixing, weak interaction force and uncontrollable product shape And other issues

Active Publication Date: 2017-09-29
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

Disadvantages: The morphology of the obtained product is uncontrollable and graphene is easy to agglomerate; the synthesis reaction temperature is high and the pressure is high, and large-scale preparation has potential safety hazards; although the CVD method can be used to construct a three-dimensional graphene network to avoid the agglomeration of graphene, its preparation Harsh conditions and high energy consumption
This method is simple and convenient, but has similar disadvantages with the above-mentioned solvothermal method: (1) graphene is easy to agglomerate, resulting in uneven distribution of each component of the composite and poor conductivity; Good microscopic morphology and pore structure; (3) Stirring and mixing takes a long time; (4) The interaction between graphene and MOFs is weak, and MOFs crystals are easy to fall off from the graphene surface during post-processing (such as washing, centrifugation) , making it difficult to control the morphology and component ratio of the final product
Although this method is simple, it is limited by the types of elements that can be applied by atomic layer deposition technology, and the types of composites that can be prepared are limited.
In addition, the atomic layer deposition method requires special equipment, which is expensive and difficult to scale production

Method used

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  • Method for preparing graphene/MOF (metal-organic framework) porous composite material aquagel and graphene/MOF porous composite material aerogel
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  • Method for preparing graphene/MOF (metal-organic framework) porous composite material aquagel and graphene/MOF porous composite material aerogel

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Experimental program
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Effect test

Embodiment 1～6

[0041] 1. Sample preparation

[0042] (1) The preparation of embodiment 1 sample is carried out as follows:

[0043] Configure a 250mL reaction bottle in an ice bath, add 96mL of concentrated sulfuric acid, add 2g of graphite powder and 1g of sodium nitrate (>99%) solid mixture under magnetic stirring, then slowly add 6g of potassium permanganate (>99.6%), Control the reaction temperature not to exceed 10°C, take it out after reacting in an ice bath for 2h, and stir in a water bath at 35°C for 18h. As the reaction progressed, the reactant finally turned into a brown slurry, and then slowly added a 5% sulfuric acid solution to it for dilution. After adding 240mL of sulfuric acid solution, 5mL of hydrogen peroxide with a mass fraction of 30% was added thereto, and the solution turned bright yellow as the bubbles burst out. After continuous stirring for 2 hours, filter, and then wash with 10% hydrochloric acid solution and deionized water several times until the solution is neu...

Embodiment 6

[0059] (5) FTIR spectral analysis

Embodiment 1

[0062] The surface morphology of the pure GO airgel obtained in Example 1 is as follows: figure 2 (a,b). figure 2 (a) shows the overall morphology of the airgel. It can be seen that the three-dimensional framework is made of a large number of overlapping GO sheets, and countless micron-scale channels are constructed. figure 2 (b) is figure 2 (a) Partial enlarged view. From (b), it can be clearly seen that the GO sheets are transparent, indicating that the GO sheets have not agglomerated, which further proves that this self-supporting porous structure is constructed by a large number of single-layer GO sheets. figure 2 (c, d) are SEM images of the Fe-MOF crystal powder obtained in Example 2. It can be seen from figure (d) that the obtained Fe-MOF crystal is a polygonal spindle with a lateral dimension of several hundred nanometers.

[0063] Figure 4 with Figure 5 (a, b) are SEM images of the GO / Fe-MOF composite airgel obtained in Examples 3-6, respectively. It can b...

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Abstract

The invention discloses a method for preparing a graphene / MOF (metal-organic framework) porous composite material aquagel and a graphene / MOF porous composite material aerogel. The method comprises the following steps: taking a clean container, adding a graphene or graphene oxide dispersion solution into the container, adding MOFs crystal powder into the container until the mass ratio of the MOFs crystal powder to the graphene or graphene oxide is (1:100)-(100:1), sealing the container, and performing oscillation or stirring to promote the formation of a graphene or graphene oxide self-assembled three-dimensional framework structure and the uniform compounding between the MOFs crystals and graphene sheets or graphene oxide sheets, thereby obtaining the graphene / MOF porous composite material aquagel; and finally, performing freeze-drying to obtain the graphene / MOF porous composite material aerogel. The graphene / MOF porous composite material aerogel has a self-supporting porous structure, and maintains the structural integrity of the graphene or graphene oxide and MOFs. The preparation method is mild in conditions and simple to operate, and can effectively prevent the graphene sheets or graphene oxide sheets and the MOFs crystals from aggregation.

Description

technical field [0001] The invention relates to a method for preparing graphene / metal organic framework compound (graphene / MOF) porous composite hydrogel and aerogel. Background technique [0002] Graphene is a carbon atom with sp 2 A single-layer sheet-like structure material with a hexagonal honeycomb lattice composed of hybrid methods (see appendix figure 1 ). In 2004, Geim et al. successfully isolated graphene, thus confirming that it can exist alone. Graphene has many unique properties such as excellent electrical properties, thermal conductivity and mechanical strength due to its unique structure, so it is widely used in the preparation of nanocomposites and electronic devices, energy storage, catalysis, biosensors and other fields. It shows the great application potential of graphene. Graphene oxide is a solution-dispersed form of graphene. The existence of epoxy groups, hydroxyl groups and carboxyl groups on the surface and edge of graphene oxide can not only fu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/194C01B32/184
CPCC01P2002/01C01P2002/72C01P2002/80C01P2002/82C01P2004/03
Inventor 曹澥宏徐喜连徐立新
Owner ZHEJIANG UNIV OF TECH
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