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Preparation method of MOFs (Metal-Organic Frameworks)-graphene composite material

A composite material and graphene technology, applied in the field of porous materials and nanomaterials, can solve the problems of platinum particle loss, high temperature requirements, low porosity, etc., and achieve the effect of mild reaction, less dosage and short time

Active Publication Date: 2017-02-22
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. When using the traditional chemical reduction method to prepare graphene, hydrazine is usually used as the reducing agent, which is extremely toxic
[0007] 2. If graphene is directly used in the fuel cell oxygen reduction catalyst, graphene is extremely easy to reunite. At this time, the electrolyte cannot fully contact the active sites on graphene, which reduces its catalytic activity.
[0008] 3. In the traditional synthesis of MOFs materials, people generally use high-boiling point solvent DMF, which requires a high temperature for the reaction system, which is not conducive to saving energy; in addition, the solvent molecules need to be removed in the subsequent steps of the reaction, resulting in a waste of raw materials
[0009] 4. In the prior art, when preparing composite materials of graphene and MOFs, graphene oxide prepared by traditional chemical reduction method is mostly used as the composite raw material, and the sheets of graphene oxide are easy to agglomerate and carbon remains between layers Too many oxygen-containing functional groups such as hydroxyl (-OH) and epoxy (-C-O-C), resulting in weak conductivity and low porosity of the composite
[0010] 5. In the traditional proton exchange membrane fuel cell, Pt / C (platinum carbon catalyst) is often used as the cathode redox catalyst. Although the catalyst particles are small, the specific surface area of ​​the material is large, and platinum is used as the metal center, the reactivity is high, but as With the increase of ionic liquid flow and use time, platinum particles are easily lost from the carbon support, resulting in catalyst deactivation
The poor durability and high production cost of this Pt / C catalyst hinder its commercial development

Method used

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  • Preparation method of MOFs (Metal-Organic Frameworks)-graphene composite material
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  • Preparation method of MOFs (Metal-Organic Frameworks)-graphene composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] To prepare graphite oxide, the specific steps are as follows:

[0039] Add 2.5g NaNO 3 and 120ml concentrated sulfuric acid, stir evenly, then add 5g graphite powder, after stirring for 30min, slowly add 15gKMnO 4 Powder, control the system temperature at 0-5°C, and react at low temperature for 2 hours. Transfer the beaker to a water bath, stir at 35°C for 2h, then add 420mL of deionized water, raise the temperature of the system to 98°C for 30min, add 40mL of H 2 o 2 , and then washed with deionized water, centrifuged, and freeze-dried to obtain solid powdered graphite oxide.

Embodiment 2

[0041] Prepare reduced graphene oxide (rGO), the specific steps are as follows:

[0042] Taking THF as the reaction medium, the graphite oxide obtained in Example 1 is used as a raw material to prepare reduced graphene oxide (rGO), and the specific steps are as follows:

[0043] Get 0.4g graphite oxide (made by embodiment 1), be placed in 40mL THF and ultrasonically disperse 30min to obtain graphene oxide dispersion liquid; 4 Dissolve in 10ml of methanol, and add it dropwise to the graphene oxide dispersion with a constant pressure dropping funnel, react in an ice-water bath at 5°C for 4h, then raise the temperature of the system to 60°C for 1h, wash with a small amount of deionized water and methanol centrifuge, Obtained reduced graphene oxide (in the form of a slightly wet solid powder).

[0044] The reduced graphene oxide prepared in this example was vacuum-dried at 60° C. for 20 hours and then weighed to 0.2 g, thus measuring: the quality of the product reduced graphene o...

Embodiment 3

[0046] Preparation of rGO@MOF-Ni composite material (graphene / Ni-organic framework composite material), the specific steps are as follows:

[0047] 1) prepare graphene: concrete steps are the same as embodiment 2, just change the consumption of raw material graphite oxide into 0.6g, make reduced graphene oxide (being slightly wet solid powder).

[0048] 2) Mix the reduced graphene oxide prepared in step 1) with 0.582g (2mmol) Ni(NO 3 ) 2 ·6H 2 O, 0.332g (2mmol) H 2 Add BDC and 0.224g (1mmol) DABCO to 20mL THF / H 2 O / CH 3 OH (volume ratio: 3:1:1) mixed solution, ultrasonically stirred for 1 h, and then reacted at 110 °C for 72 h in the reactor, then heated with THF, slightly heated CH 3 OH was washed three times each, and vacuum-dried at 90°C for 20 h to obtain rGO@MOF-Ni (mark this sample as rGO@MOF-Ni-1).

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Abstract

The invention relates to a preparation method of a MOFs (Metal-Organic Frameworks) graphene composite material, comprising the following steps: (1) preparing graphene by taking graphite oxide as a raw material, THF (tetrahydrofuran) as a reaction medium and NaBH4 as a reducing agent; (2) adding graphene, metal salt, H2BDC (1,4-benzenedicarboxylic acid) and DABCO (1,4-diazabicyclooctane triethylenediamine) into a THF / H2O / CH3OH mixed solution, ultrasonically stirring, reacting for 12-72 h at 80-180 DEG C, and purifying to obtain the MOFs-graphene composite material. According to the preparation method, in the step (1), the experimental condition for preparing a graphene precursor is mild, the time is short, the number of layers of the prepared graphene is small, the use level of the reducing agent is reduced as THF is used as a solvent, high temperature is not needed, complex washing and drying processes are eliminated, and the environment pollution is less; in the step (2), the THF is used as an organic solvent for synthesis of the metal organic frameworks, the utilization rate of the raw material is increased, the THF solvent is low in boiling point and low in usage requirement on equipment, and an after-treatment process is simple and easy to operate. The MOFs-graphene composite material prepared by the method can be widely applied to energy devices such as a fuel-cell catalyst, a super-capacitor, and an anode material and an adsorbing material of a lithium ion battery.

Description

technical field [0001] The invention relates to the field of porous materials and nanometer materials, in particular to a method for preparing MOFs-graphene composite materials. Background technique [0002] Metal-organic frameworks (MOFs) are also called porous coordination polymers (PCPs). The chemical synthesis mechanism of this emerging crystalline microporous material has been widely accepted and has attracted great attention in the scientific research community. This three-dimensional geometric structure is formed by linking organic ligands and inorganic metal ions, and their structures can be designed according to different performances. The most unique properties of MOFs are their ultra-high porosity and relatively high internal specific surface area. Therefore, it plays an important role in functional devices, especially for energy storage, adsorption, sensing, proton conduction, and drug delivery. In general, the micropores and size lengths of MOFs can be tuned ...

Claims

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Application Information

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IPC IPC(8): C01B32/184H01M4/90
CPCH01M4/9083Y02E60/50
Inventor 涂文懋严琼
Owner WUHAN UNIV OF TECH
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