Preparation method and applications of multi-level pore structure metal organic framework material

A metal-organic framework and metal-organic framework technology, which is applied in the field of preparation of metal-organic framework materials with a hierarchical porous structure, can solve the problems of unstable performance of metal-organic framework materials, and the preparation method is not universal, and achieves mild conditions, Simple preparation process and controllable pore size

Active Publication Date: 2019-09-20
WUHAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of this, the present invention aims to propose a method for preparing a metal-organic framework material with a hierarchical porous structure, so as to solve the problem that the existing method for preparing metal-organic framework materials is not universal, and the properties of the prepared metal-organic framework materials are not stable. The problem

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  • Preparation method and applications of multi-level pore structure metal organic framework material
  • Preparation method and applications of multi-level pore structure metal organic framework material
  • Preparation method and applications of multi-level pore structure metal organic framework material

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Embodiment 1

[0033] A method for preparing a metal-organic framework material with a hierarchical porous structure, specifically comprising the following steps:

[0034] 160mg hafnium chloride (0.5mmol), 83mg terephthalic acid (0.5mmol), 18ml N,N-dimethylformamide (0.234mol), 1ml formic acid (0.026mol) and 3ml deionized water (0.167mol) Add it into the reaction kettle, stir it evenly with ultrasonic, then conduct a hydrothermal reaction at a reaction temperature of 123°C for 48 hours. After the hydrothermal reaction is completed, cool it to room temperature at a cooling rate of 2°C / min, and then centrifuge to obtain multi-stage pores For the crude metal organic framework material, at this cooling rate, the unreacted ligand can be crystallized in the form of a uniform octahedron, which is convenient for the subsequent purification of the product;

[0035] Soak the crude metal-organic framework material with a hierarchical porous structure in methanol and dichloromethane for three days, cent...

Embodiment 2

[0037] A method for preparing a metal-organic framework material with a hierarchical porous structure, specifically comprising the following steps:

[0038] 160mg hafnium chloride (0.5mmol), 83mg terephthalic acid (0.5mmol), 18ml N,N-dimethylformamide (0.234mol), 1m acetic acid (0.017mol) and 1ml deionized water (0.055mol) Add it into the reaction kettle, stir it evenly with ultrasonic, then conduct a hydrothermal reaction at a reaction temperature of 123°C for 48 hours. After the hydrothermal reaction is completed, cool it to room temperature at a cooling rate of 2°C / min, and then centrifuge to obtain multi-stage pores For the crude metal organic framework material, at this cooling rate, the unreacted ligand can be crystallized in the form of a uniform octahedron, which is convenient for the subsequent purification of the product;

[0039] Soak the crude metal-organic framework material with a hierarchical porous structure in methanol and dichloromethane for three days, centr...

Embodiment 3

[0041] A method for preparing a metal-organic framework material with a hierarchical porous structure, specifically comprising the following steps:

[0042]160mg hafnium chloride (0.5mmol), 83mg terephthalic acid (0.5mmol), 18ml N,N-dimethylformamide (0.234mol), 1m acetic acid (0.017mol) and 3ml deionized water (0.167mol) Add it into the reaction kettle, stir it evenly with ultrasonic, then conduct a hydrothermal reaction at a reaction temperature of 123°C for 48 hours. After the hydrothermal reaction is completed, cool it to room temperature at a cooling rate of 2°C / min, and then centrifuge to obtain multi-stage pores For the crude metal organic framework material, at this cooling rate, the unreacted ligand can be crystallized in the form of a uniform octahedron, which is convenient for the subsequent purification of the product;

[0043] Soak the crude metal-organic framework material with a hierarchical porous structure in methanol and dichloromethane for three days, centri...

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Abstract

The invention provides a preparation method and applications of a multi-level pore structure metal organic framework material. The preparation method comprises: mixing a metal salt, an organic ligand, N,N-dimethylformamide, water and carboxylic acid, uniformly stirring, carrying out a hydrothermal reaction, cooling to a room temperature after completing the hydrothermal reaction, carrying out centrifugation, and purifying to prepare the multi-level pore structure metal organic framework material. According to the present invention, the prepared multi-level pore structure metal organic framework material has characteristics of stable performance and controlled and uniform pore size; and phosphotungstic acid is loaded in the mesoporous channel of the metal organic framework material through an in-situ synthesis method, the original framework structure can be remained after the loading, and the presence of the mesopores allows the contact between the large substrate molecule and the active site so as to extend the application range of the multi-level pore structure metal organic framework material.

Description

technical field [0001] The invention relates to the technical field of catalytic materials, in particular to a preparation method and application of a metal-organic framework material with a hierarchical porous structure. Background technique [0002] Porous materials have been one of the research hotspots and are considered to be powerful tools for many important applications due to their ability to interact with atoms, ions, molecules, and even larger guests both in the internal pore system and external surfaces. Metal-organic framework (MOF) is a crystalline porous material formed by the self-assembly of metal ions (or clusters) and organic ligands. Due to its large specific surface area, porosity, adjustable channels, and designable structure, it has huge potential applications in gas storage, separation, catalysis and sensing. [0003] 99% of the currently researched MOF materials are microporous materials. The controllability of the channels is mainly adjustable in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J31/22B01J35/10C07C41/03C07C43/13
CPCC08G83/008B01J31/1691B01J31/2213B01J31/2239B01J35/1004C07C41/03C07C43/13B01J2531/48B01J2531/49
Inventor 常刚刚李嘉昕阳晓宇
Owner WUHAN UNIV OF TECH
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