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Preparation method of MOFs/graphene adsorption material

An adsorption material, graphene technology, applied in the direction of chemical instruments and methods, other chemical processes, etc., can solve the problems that cannot be widely applied, and achieve the effect of improving porosity and thermal stability, enhancing stability and mechanical strength

Inactive Publication Date: 2016-11-02
NANJING UNIV OF POSTS & TELECOMM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The patent document with the application publication number CN103432997A discloses a Cu-based organic framework-graphene oxide composite material, which uses mechanochemical methods to promote the chemical reaction between metal ions and organic ligands, but its preparation method is only for certain Organic ligands and certain metal salt particles are not widely applicable

Method used

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  • Preparation method of MOFs/graphene adsorption material
  • Preparation method of MOFs/graphene adsorption material
  • Preparation method of MOFs/graphene adsorption material

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Preparation of pre-oxidized graphite

[0024] Add 5g of 300um expandable flake graphite to 250ml of 98% concentrated H 2 SO 4 In the solution, after stirring and dispersing evenly, slowly add 50mL of fuming nitric acid, then stir in an ice bath for 24h, then pour into 1000mL of water for dilution, cool to room temperature, filter and wash with water, dry at 60°C for 24h, and then expand with 1000W microwave for one minute to obtain expanded graphite . Take 5g of expanded graphite, add it to 300mL of concentrated sulfuric acid with a mass fraction of 98%, stir and disperse evenly, and slowly add 4.2g of K 2 S 2 o 8 and 6.2gP 2 o 5 , stirred at 80°C for 5h, then poured into 2L of water for dilution, cooled, filtered, washed with water, and dried at room temperature for 48h to obtain pre-oxidized graphite.

[0025] (2) Preparation of graphene oxide dispersion

[0026] Get 5g of pre-oxidized graphite and add it to 200mL of concentrated sulfuric acid, then add 15...

Embodiment 2

[0034](1) Preparation of pre-oxidized graphite

[0035] Add 4g of 300um expandable flake graphite to 100ml of 98% concentrated H 2 SO 4 In the solution, after stirring and dispersing evenly, slowly add 40mL fuming nitric acid, then stir in an ice bath for 24h, then pour into 1000mL water for dilution, cool to room temperature, filter and wash with water, dry at 60°C for 12h, and then expand with 1000W microwave for one minute to obtain expanded graphite ; Get 2g expanded graphite, join in the concentrated sulfuric acid that 100mL mass fraction is 98%, slowly add 1.8g K after stirring and dispersing 2 S 2 o 8 and 2.1gP 2 o 5 , stirred at 80°C for 5h, then poured into 2L of water for dilution, cooled, filtered, washed with water, and dried at room temperature for 48h to obtain pre-oxidized graphite.

[0036] (2) Preparation of graphene oxide dispersion

[0037] Take 1g of pre-oxidized graphite and add it to 50mL of concentrated sulfuric acid, then add 3g of KMnO 4 Add sl...

Embodiment 3

[0041] (1) preparation of preoxidized graphite: with embodiment 2

[0042] (2) Preparation of graphene oxide dispersion: different from Example 2, KMnO 4 The mass is 2g.

[0043] (3) Preparation of MOFs / graphene gel

[0044] Using 1,2,4-benzenetricarboxylic acid as the organic ligand, CuCl 2 as a metal salt. Weigh CuCl 2 (24mg, 0.18mmol) and 1,2,4-benzenetricarboxylic acid (14mg, 0.67mmol) were dissolved in 10mL of deionized water, stirred and dispersed for 5min; 4mL of 25mg / mL graphene oxide aqueous dispersion was taken, dispersed in 6mL In dimethylacetamide (DMAC) and 6mL of dimethylformamide (DMF), stir for 5min, then mix the two into a 40mL reactor, add 10mL of methanol in the reactor and stir for 5min, the reaction The kettle was placed in an oven at 80°C for 6h, and then heated to 180°C for 6h to obtain Cu-MOFs / graphene gel.

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Abstract

The invention discloses a preparation method of a MOFs / graphene adsorption material. The method consists of: firstly preparing a graphene oxide dispersion solution, then letting the graphene oxide dispersion solution and an organic ligand to form coordination bond simultaneously with metal ions, and performing self-assembly to obtain gel. Specifically, the organic ligand comprises 1, 3, 5-benzenetricarboxylic acid, 1, 2, 4-benzenetricarboxylic acid or phthalic acid, and the metal salt includes Cu(NO3)2 3H2O, CuCl2, or ZnCl2. Graphene not only can participate in MOFs material formation by physical blending, but also forms the MOFs / graphene composite material in the form of chemical bond. The added graphene oxide not only enhances the stability and mechanical strength of the material, but also endows MOFs materials with some unique properties of graphene, and effectively improves the porosity and thermal stability of MOFs materials.

Description

technical field [0001] The invention relates to the field of preparation of metal organic framework materials, in particular to a preparation method of MOFs / graphene adsorption materials. Background technique [0002] In recent years, due to more and more polluting gases emitted through the combustion of fossil fuels, the phenomenon of global warming has become more and more serious. Among them, carbon dioxide is the main greenhouse gas. People began to explore the absorption of carbon dioxide gas while looking for less environmental pollution. Clean energy, among which hydrogen is a clean and efficient energy carrier. However, hydrogen also has its drawbacks, that is, it is not only difficult to produce, but also difficult to store in high capacity. A material for the capture and storage of gases is being actively researched, but the research in this area has not made outstanding progress. [0003] Metal-organic framework materials (MOFs) are a type of coordination polyme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30
CPCB01J20/226B01J20/20B01J2220/46
Inventor 闵永刚冯亚飞马寸亮肖壮青
Owner NANJING UNIV OF POSTS & TELECOMM