Preparation method of metal-organic framework compound with hierarchical pore structure

An organic framework, multi-level hole technology, applied in the direction of zinc organic compounds, copper organic compounds, etc., can solve problems such as the collapse of the overall structure, and achieve the effect of ensuring stability

Inactive Publication Date: 2014-11-19
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the removal of surfactants often leads to the collapse of the overall

Method used

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  • Preparation method of metal-organic framework compound with hierarchical pore structure
  • Preparation method of metal-organic framework compound with hierarchical pore structure
  • Preparation method of metal-organic framework compound with hierarchical pore structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1. Preparation of hierarchically porous ZIF-8.

[0032] (1) Add 10ml (2mg / ml) polymer nanowire solution, 15ml methanol, and 25ml Zn(NO 3 ) 2 (250mM) methanol solution, 50ml 2-methylimidazole (250mM) methanol solution. Shake well and let stand at room temperature. After 24 hours, a white precipitate was obtained, which was collected by centrifugation, washed twice with methanol, and dried overnight in a vacuum oven to obtain 0.1238 g of a white solid.

[0033] (2) The product was put into a muffle furnace and calcined at 350° C. for 4 hours to obtain 0.0915 g of a yellow solid. Field emission scanning electron microscopy, high resolution transmission electron microscopy, nitrogen adsorption and desorption experiment results are as follows: figure 1 , 2 , 3.

Embodiment 2

[0034] Example 2. Preparation of hierarchically porous ZIF-8.

[0035] (1) Add 2ml polymer nanowire (2mg / ml) solution, 83ml methanol, and 5ml Zn(NO 3 ) 2 · 6H 2 O (250mM) methanol solution, 10ml 2-methylimidazole (250mM) methanol solution. Shake well and let stand at room temperature. After 24 hours, a white flocculent precipitate was obtained, which was collected by centrifugation, washed twice with methanol, and dried overnight in a vacuum oven to obtain 0.0727 g of a white solid.

[0036] (2) The product was put into a muffle furnace, and calcined at 350° C. for 4 hours to obtain 0.0504 g of a yellow solid.

Embodiment 3

[0037] Example 3. Preparation of hierarchically porous ZIF-7.

[0038] (1) Add 10ml (2mg / ml) polymer nanowire solution, 15ml methanol, and 25ml Zn(NO 3 ) 2 · 6H 2 O (250mM) methanol solution, 50ml benzimidazole (250mM) methanol solution. Shake well and let stand at room temperature. After 3 days, a white precipitate was obtained, which was collected by centrifugation, washed twice with methanol, and dried overnight in a vacuum oven to obtain 0.3216 g of a white solid.

[0039] (2) The product was put into a muffle furnace and calcined at 400°C for 3 hours to obtain 0.2852 g of a white solid. The field emission scanning electron microscope of the product, the high resolution transmission electron microscope experiment results are as follows Figure 4 .

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Abstract

The invention belongs to the technical field of nanocomposite materials and in particular relates to a preparation method of a metal-organic framework compound with a hierarchical pore structure. The preparation method comprises the following steps: firstly, self-assembling a diblock copolymer in a solvent to form a flexible polymer nanowire with a core-shell structure, and cross-linking cores to obtain a polymer nanowire with a stable solvent; adding metal ions and organic ligands into a nanowire solution to form a mixed solution; crystallizing at the room temperature to obtain a metal-organic framework/core-shell structure polymer nanowire compound; calcining to remove the polymer nanowire to obtain a hierarchical pore material with MOFs (metal-organic frameworks) micropores, small mesopores formed after calcination of a shell layer of the polymer nanowire and large mesopores formed after calcinations of a core layer. According to the MOFs material with the hierarchical pore structure, the advantages of the micropores and the micropores are combined, the mass transfer speed of the MOFs material is improved, relatively large molecules can conveniently enter the MOFs material, and the application potential of the MOFs material in the field of catalysis, adsorption and the like is improved.

Description

technical field [0001] The invention belongs to the technical field of nanocomposite materials, and in particular relates to a preparation method of a metal organic framework compound with a hierarchical porous structure. Background technique [0002] Porous materials, such as molecular sieves, mesoporous silicon, and activated carbon, are a very important class of materials. Due to their huge specific surface area, they are widely used in catalysis, gas adsorption, ion exchange and so on. Metal-organic frameworks (MOFs), a newly emerging organic-inorganic porous material, have attracted extensive attention due to their excellent properties and the controllability of structure and function. MOFs are a class of crystalline materials composed of metal ions and organic ligands. The structures and functions of MOsFs can be obtained according to the selection of metal ions and the synthesis of different organic ligands. It can be applied in the fields of gas storage, separatio...

Claims

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Application Information

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IPC IPC(8): C07F3/06C07F1/08
Inventor 陈道勇易俊琦
Owner FUDAN UNIV
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