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CuBTC type mesopore and micropore metal organic framework material and method for preparing same

A metal-organic framework, meso-micro double-hole technology, applied in the direction of copper organic compounds, etc., can solve the problems of fast framework collapse and limited application, and achieve the effects of simplified synthesis steps, good repeatability and simple process

Inactive Publication Date: 2015-12-16
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The apertures in the three vertical directions are However, the use of long ligands is easy to form multiple networks, and the prepared MOFs will collapse faster after removing the guest molecules, and the long ligands are generally more expensive, which limits the application of the long ligand method.
Therefore, how to conveniently and rapidly synthesize mesoporous biporous MOFs is still a great challenge.

Method used

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  • CuBTC type mesopore and micropore metal organic framework material and method for preparing same
  • CuBTC type mesopore and micropore metal organic framework material and method for preparing same
  • CuBTC type mesopore and micropore metal organic framework material and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) 1.094gCu(NO 3 ) 2 ·3H 2 O was dissolved in a mixed solution of 5ml of water and 10ml of ethanol, stirred at 30-40°C for 15min to obtain a clear solution;

[0034] (2) Add 0.525gH 3 Dissolve BTC (trimesic acid) in 15ml of ethanol, stir at 30-40°C for 15min to obtain a clear solution;

[0035] (3) Add the solution of step (1) to the solution of step (2), stir at 30-40°C for 15 minutes and mix well;

[0036](4) Add 1ml of dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride to the solution in step (3), stir at 30-40°C for 30min and mix evenly to obtain a mixed solution ;

[0037] (5) Place the mixed solution of step (4) in a 100ml stainless steel autoclave, and react at a temperature of 120°C for 12h;

[0038] (6) Cool the reaction product of step (5) to room temperature in a natural state, successively undergo suction filtration, dry at 100° C. for 3 hours in a blast drying oven, soak in ethanol at 100° C. for 4 times, each time for 8 hours, suction fil...

Embodiment 2

[0040] (1) 1.094gCu(NO 3 ) 2 ·3H 2 O was dissolved in a mixed solution of 5ml of water and 10ml of ethanol, stirred at 30-40°C for 15min to obtain a clear solution;

[0041] (2) Add 0.567gH 3 Dissolve BTC (trimesic acid) in 15ml of ethanol, stir at 30-40°C for 15min to obtain a clear solution;

[0042] (3) Add the solution of step (1) to the solution of step (2), stir at 30-40°C for 15 minutes and mix well;

[0043] (4) Add 2ml of dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride to the solution in step (3), stir at 30-40°C for 30min and mix evenly to obtain a mixed solution ;

[0044] (5) Place the mixed solution of step (4) in a 100ml stainless steel autoclave, and react at a temperature of 120°C for 12h;

[0045] (6) Cool the reaction product of step (5) to room temperature in a natural state, successively undergo suction filtration, dry at 100° C. for 3 hours in a blast drying oven, soak in ethanol at 100° C. for 4 times, each time for 8 hours, suction fi...

Embodiment 3

[0047] (1) 1.094gCu(NO 3 ) 2 ·3H 2 Dissolve O in a mixed solution of 5ml water and 10ml ethanol, stir at 30-40°C for 30min to obtain a clear solution;

[0048] (2) Add 0.525gH 3 Dissolve BTC (trimesic acid) in 15ml of ethanol, stir at 30-40°C for 30min to obtain a clear solution;

[0049] (3) Add the solution of step (1) to the solution of step (2), stir at 30-40°C for 30 minutes and mix well;

[0050] (4) Add 1ml of dimethyloctadecyl[3-(trimethoxysilyl)propyl]ammonium chloride to the solution in step (3), stir at 30-40°C for 60min and mix evenly to obtain a mixed solution ;

[0051] (5) Place the mixed solution of step (4) in a 100ml stainless steel autoclave, and react at a temperature of 110°C for 16h;

[0052] (6) Cool the reaction product of step (5) to room temperature in a natural state, successively undergo suction filtration, dry at 120° C. for 6 hours in a blast drying oven, and soak in ethanol at 120° C. for 5 times, each time for 12 hours, suction filtration ...

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Abstract

The invention belongs to the technical field of metal organic framework materials, and discloses a CuBTC type mesopore and micropore metal organic framework material and a method for preparing the same. The method includes dissolving Cu(NO<3>)<2><3>H<2>O in water and ethyl alcohol mixed solution and stirring the Cu(NO<3>)<2><3>H<2>O and the water and ethyl alcohol mixed solution to obtain first clear solution; dissolving H<3>BTC in ethyl alcohol and stirring the H<3>BTC and the ethyl alcohol to obtain second clear solution; uniformly stirring and mixing the first clear solution and the second clear solution with each other to obtain mixed solution, then adding dimethyl octadecyl [3-(trimethoxy silicon substrate) propyl] ammonium chloride into the mixed solution, and carrying out hydrothermal synthesis reaction under certain conditions to obtain reaction products; sequentially carrying out pumping filtration, forced-air drying, washing, pumping filtration and vacuum drying on the reaction products to obtain the CuBTC type mesopore and micropore metal organic framework material. The CuBTC type mesopore and micropore metal organic framework material and the method have the advantages that mesopore is successfully formed in the traditional micropore metal organic framework material CuBTC, products have large specific surface areas and pore volumes, and accordingly the CuBTC type mesopore and micropore metal organic framework material and the method have excellent application prospects in the aspects of macromolecular catalysis, adsorption, separation and the like.

Description

technical field [0001] The invention belongs to the technical field of metal-organic framework materials, and in particular relates to a CuBTC-type medium-micro-double-porous metal-organic framework material and a preparation method. Background technique [0002] Metal-organic frameworks (MOFs) are crystalline materials with a periodic network structure formed by self-assembly of inorganic metal ions and organic ligands. It has high specific surface area, designable structure and function, and adjustable pore size. It shows great application potential in adsorption, separation, catalysis and hydrogen storage. However, most of the currently reported MOFs materials are microporous (<2nm). On the one hand, too small pores prevent macromolecules such as adsorbates and reactants from entering the pores, and on the other hand, they lead to large mass transfer resistance, which is not conducive to molecular Fast diffusion, slow reaction. Therefore, in recent years, research on...

Claims

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Application Information

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IPC IPC(8): C07F1/08
Inventor 李彦彦奚红霞柳泽伟段崇雄
Owner SOUTH CHINA UNIV OF TECH
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