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Small and medium dual-hole HKUST-1 material and preparation method and application thereof

A kind of HKUST-1, medium and micro double-pore technology, applied in chemical instruments and methods, other chemical processes, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of increased synthesis cost, reduced pore size, long-term limit Ligand method is widely used to achieve the effect of good crystal structure, good repeatability, rich micropore and mesopore structure

Inactive Publication Date: 2014-12-10
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Small and medium dual-hole HKUST-1 material and preparation method and application thereof
  • Small and medium dual-hole HKUST-1 material and preparation method and application thereof
  • Small and medium dual-hole HKUST-1 material and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Weigh 1.068g Cu(NO 3 ) 2 .3H 2 O was dissolved in a solvent formed by mixing 8ml DMF, 8ml ethanol and 8ml water, and stirred until completely dissolved to obtain a clear solution A; another 0.46g H 3 BTC was dissolved in the same solvent formed by mixing 8ml DMF, 8ml ethanol and 8ml water, and stirred until completely dissolved to obtain a clear solution B; add the clear solution B to the clear solution A, and stir evenly to obtain a mixed solution; 0.197g3 -APS was added to the mixed solution, and then stirred for 30 minutes; the mixed solution was transferred into a stainless steel autoclave for hydrothermal synthesis, and heated at 110°C for 12h; after cooling to room temperature, the product was filtered and vacuum-dried at 150°C for 8h; Soak and wash with ethanol 4 times at 100°C for 12 hours each time; filter the product and dry it in vacuum at 150°C for 12 hours to prepare sample B1 of medium-micro-porous HKUST-1 material.

Embodiment 2

[0041] Weigh 1.068g Cu(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 0.50g H 3 Dissolve BTC in the same solution formed by mixing 8.5ml of DMF, 8.5ml of ethanol and 8.5ml of water, and stir until completely dissolved to obtain a clear solution B; add the clear solution B to the clear solution A, and stir evenly to obtain a mixed solution; Add 0.16g of 3-APS into the mixed solution, and 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 14 hours; the product was filtered and vacuum-dried at 140° C. for 8 hours to obtain a sample B2 of medium-micro-porous HKUST-1 material.

Embodiment 3

[0043] Weigh 1.068g Cu(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 0.45g H 3 Dissolve BTC in the same solvent formed by mixing 8.5ml DMF, 8.5ml ethanol and 8.5ml water, stir until completely dissolved to obtain clear solution B; add clear solution B to clear solution A, stir evenly to obtain a mixed solution; Add 0.32g of 3-APS into the mixed solution, and 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 obtain a sample B3 of medium-micro-porous HKUST-1 material.

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Abstract

The invention belongs to the field of preparation of metal-skeleton organic matters and discloses a small and medium dual-hole HKUST-1 material and a preparation method and application thereof. The method comprises the following steps: respectively dissolving Cu(NO3)2.3H2O and H3BTC into a mixed solution of DMF, ethyl alcohol and water; stirring to obtain a clear solution A and a clear solution B; adding the clear solution A to the clear solution B and mixing evenly; adding 3-aminopropyltrimethoxysilane and stirring; transferring the obtained mixed solution to a stainless steel high-pressure reaction kettle, and carrying out temperature programming; cooling the reaction kettle to room temperature, filtering the product, and drying the product in vacuum; and washing the obtained product with ethyl alcohol for four times, thus obtaining the small and medium dual-hole HKUST-1 material. The product has a single mesoporous and microporous crystal structure, the mass transfer resistance is overcome in reaction, the mass transfer efficiency is improved, and particularly, the product has a relatively good application prospect in the fields of catalysis, adsorption, separation and the like 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 single size and shape are also called 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 pore structure, surface modification, and ...

Claims

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Application Information

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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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