A kind of medium and micro double hole hkust-1 material and its preparation method and application

A HKUST-1, medium and micro-double hole technology, applied in chemical instruments and methods, other chemical processes, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of the wide application and synthesis cost of the long-ligand method increase and decrease of pore size, etc., to achieve the effect of rich micropore and mesopore structure, good crystal structure and good repeatability

Inactive Publication Date: 2016-07-06
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, although the use of long ligands can introduce mesopores in MOFs, this approach often leads to the interconnection of the framework after removal of the guest solvent, resulting in a decrease in pore size.
At the same time, the price of long ligands is relatively expensive, which also increases the cost of synthesis. These problems limit the wide application of long ligand methods.

Method used

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  • A kind of medium and micro double hole hkust-1 material and its preparation method and application
  • A kind of medium and micro double hole hkust-1 material and its preparation method and application
  • A kind of medium and micro double hole hkust-1 material and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0039] Weigh 1.068gCu(NO 3 ) 2 .3H 2 O was dissolved in a solvent formed by mixing 8mlDMF, 8ml ethanol and 8ml water, and stirred until completely dissolved to obtain a clear solution A; another 0.46gH 3 BTC was dissolved in the same solvent formed by mixing 8mlDMF, 8ml ethanol and 8ml water, and stirred until it was completely dissolved to obtain a clear solution B; the clear solution B was added to the clear solution A, and stirred evenly to obtain a mixed solution; 0.197g3- APS was added to the mixed solution, and then stirred for 30 min; the mixed solution was transferred into a stainless steel autoclave for hydrothermal synthesis, and heated at 110 °C for 12 h; after cooling to room temperature, the product was filtered and vacuum-dried at 150 °C for 8 h; ℃ and soaked with ethanol for 4 times, each time for 12 hours; the product was filtered and vacuum-dried at 150 ℃ for 12 hours to prepare the sample B1 of medium and micro-porous HKUST-1 material.

Embodiment 2

[0041] Weigh 1.068gCu(NO 3 ) 2 .3H 2 O was dissolved in a solvent formed by mixing 8.5ml DMF, 8.5ml ethanol and 8.5ml water, and stirred until completely dissolved to obtain a clear solution A; another 0.50gH 3 BTC was dissolved in the same solution formed by mixing 8.5mlDMF, 8.5ml ethanol and 8.5ml water, and stirred until completely dissolved to obtain a clear solution B; the clear solution B was added to the clear solution A, and stirred evenly to obtain a mixed solution; Add 0.16g of 3-APS into the mixed solution, and then stir for 60min; transfer the mixed solution into a stainless steel autoclave for hydrothermal synthesis, and heat at 120°C for 8h; after cooling to room temperature, the product is filtered and vacuum-dried at 120°C for 15h; The product was soaked with ethanol at 150°C for 3 times, each time for 14h; the product was filtered and vacuum-dried at 140°C for 8h to prepare the sample B2 of medium-micro-porous HKUST-1 material.

Embodiment 3

[0043] Weigh 1.068gCu(NO 3 ) 2 .3H 2 O was dissolved in a solvent formed by mixing 8.5ml DMF, 8.5ml ethanol and 8.5ml water, and stirred until completely dissolved to obtain a clear solution A; another 0.45gH 3 BTC was dissolved in the same solvent formed by mixing 8.5mlDMF, 8.5ml ethanol and 8.5ml water, and stirred until completely dissolved to obtain a clear solution B; the clear solution B was added to the clear solution A and stirred evenly to obtain a mixed solution; Add 0.32g of 3-APS into the mixed solution, and then stir for 50 minutes; transfer the mixed solution into a stainless steel autoclave for hydrothermal synthesis, and heat at 110°C for 10h; after cooling to room temperature, the product is filtered and vacuum-dried at 140°C for 15h; The product was soaked with ethanol at 120°C for 5 times, each time for 8h; the product was filtered and vacuum-dried at 120°C for 15h to prepare the sample B3 of medium-micro-porous HKUST-1 material.

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Abstract

The invention belongs to the field of metal-skeleton organic matter preparation, and discloses a medium-micro-double-porous HKUST-1 material, a preparation method and application thereof. The method is to combine Cu(NO 3 ) 2 .3H 2 O and H 3 Dissolve BTC in a mixed solution of DMF, ethanol and water, and stir to obtain clear solution A and clear solution B; add clear solution A to clear solution B, mix well; add 3-aminopropyltrimethoxysilane, and stir; The obtained mixed solution was transferred into a stainless steel high-pressure reaction kettle, and the temperature was raised; the reaction kettle was cooled to room temperature, the product was filtered, and vacuum-dried; the obtained product was washed 4 times with ethanol to obtain a medium-micro-double-porous HKUST-1 material; the product of the present invention With a single mesoporous and microporous crystal structure, it overcomes the mass transfer resistance in the reaction and improves the mass transfer efficiency, especially in the fields of catalysis, adsorption and separation involving macromolecules.

Description

technical field [0001] The invention belongs to the field of metal-skeleton organic matter preparation, in particular to a medium-micro-double-porous HKUST-1 material and its preparation method and application, specifically HKUST-1 metal-skeleton organic matter containing multi-level channels of micropores and mesopores And its preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs) are obtained by hybridization of organic ligands (organic ligands containing single or multiple carboxylic acids or organic ligands containing nitrogen and oxygen atoms) with metal ions or metal clusters. Coordination polymers with a periodic network structure of a single size and shape are therefore also called porous coordination polymers (porous coordination polymers, PCPs). MOFs have been widely used in sensing, gas separation, adsorption, biopharmaceutical carriers, gas storage, and catalysis due to their excellent properties such as well-developed ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F1/08B01J31/22B01J20/22
Inventor 郑丽明奚红霞柳泽伟朱智洪李彦彦
Owner SOUTH CHINA UNIV OF TECH
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