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Method for rapidly synthesizinghierarchically porous HKUST-1 material with dual-functiontemplate method

A HKUST-1, template method technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, other chemical processes, etc., to achieve the effects of energy saving, stable structure, and mild conditions

Active Publication Date: 2017-06-13
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

According to people such as Stock [Stock N, Biswas S.ChemInformAbstract: Synthesis of Metal—Organic Frameworks (MOFs): Routes to Various MOFTopologies, Morphologies, and Composites [J].ChemInform, 2012,43(16):933-69.] According to the collation, the space-time yield of the hydrothermal synthesis of HKUST-1 reported in the literature is σ p =225(kg·m -3 d -1 ), the space-time yield can only reach σ by methods such as microwave-assisted heating p =225(kg·m -3 d -1 )

Method used

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  • Method for rapidly synthesizinghierarchically porous HKUST-1 material with dual-functiontemplate method
  • Method for rapidly synthesizinghierarchically porous HKUST-1 material with dual-functiontemplate method
  • Method for rapidly synthesizinghierarchically porous HKUST-1 material with dual-functiontemplate method

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1.093g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 15ml deionized water, 0.525g trimesic acid (H 3 BTC) was dissolved in 15ml methanol and stirred for 20 minutes respectively; Cu(NO 3 ) 2 ·3H 2 O aqueous solution was added to the methanol solution of trimesic acid to obtain a mixed solution, and the stirring was continued for 5 minutes; 1.12 g template agent N, N, N, N-tetramethylhexamethylenediamine (purchased from Bailingwei, the same below) was added to the mixed solution , and continued to stir for 30 s; the solution was filtered with suction, and the obtained solid was dried in a vacuum oven at 120°C for 12 hours to prepare a multi-level porous HKUST-1 material, labeled as sample A1.

Embodiment 2

[0031] 1.093g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 15ml deionized water, 0.576g trimesic acid (H 3 BTC) was dissolved in 15ml methanol and stirred for 15 minutes respectively; Cu(NO 3 ) 2 ·3H 2 O aqueous solution was added to the methanol solution of trimesic acid to obtain a mixed solution, and the stirring was continued for 10 minutes; 1.20 g template agent N, N, N, N-tetramethylhexamethylenediamine was added to the mixed solution, and the stirring was continued for 30 s; the solution After suction filtration, the obtained solid was dried in a vacuum oven at 120° C. for 16 hours to prepare a multi-level porous HKUST-1 material, labeled as sample A2.

Embodiment 3

[0033] 1.093g Cu(NO 3 ) 2 ·3H 2O was dissolved in 15ml deionized water, 0.479g trimesic acid (H 3 BTC) was dissolved in 15ml methanol and stirred for 18 minutes respectively; Cu(NO 3 ) 2 ·3H 2 O aqueous solution was added to the methanol solution of trimesic acid to obtain a mixed solution, and the stirring was continued for 8 minutes; 1.16 g of template agent N, N, N, N-tetramethylhexamethylenediamine was added to the mixed solution, and the stirring was continued for 30 s; After suction filtration, the obtained solid was dried in a vacuum oven at 120° C. for 14 hours to prepare a multi-level porous HKUST-1 material, labeled as sample A3. .

[0034] Taking the effect of the hierarchically porous HKUST-1 material prepared in Example 1 as a representative to analyze the effect of the present invention, the analytical results of the hierarchically porous HKUST-1 material prepared in other examples are basically the same as those in Example 1, so they are not one by one. s...

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Abstract

The inventiondiscloses a method for rapidly synthesizinga hierarchically porous HKUST-1 material with a dual-functiontemplate method. With the adoption of the method, the yield can be increased, and the synthesis time of the materialcan be shortened to 30 s. The method comprises steps as follows: Cu(NO3)2.3H2O is dissolved in deionized water, andtrimesic acid is dissolved in methanol and stirred; two solutions are mixed and stirred continuously; a template agent is added to a mixed solution and stirred, a product is subjected to suction filtration and then placed in a vacuum drying oven for drying, and the hierarchically porous HKUST-1 material is prepared. According to the method, N,N,N,N-tetramethylethylenediamineis taken as the template agent and adeprotonation agent simultaneously, the operation is simple, conditions are mild, and reaction time is very short; a synthetic product has a rich porous structure, is provided with micropores and mesoporessimultaneously, facilitates macromolecular diffusion and has better application prospect in the aspects of adsorption and separation of gas, catalysis, drug delivery and the like.

Description

technical field [0001] The invention belongs to the field of rapid preparation of hierarchical porous metal-organic framework materials, and in particular relates to a method for rapidly synthesizing a hierarchical porous HKUST-1 material by a dual-functional template method. Background technique [0002] Porous materials have applications in adsorption separation, gas storage, catalysis, drug delivery, etc. Metal-organic framework compounds MOFs (metal-organic frameworks, MOFs) are a coordination polymer with a single size and shape periodic network structure obtained by assembling organic ligands and metal ions or metal clusters. As a new type of porous material, MOFs have huge micropore volume, specific surface area and ultra-high porosity, and have extremely high application prospects. Traditional MOFs are mostly microporous structures, and in applications such as separation and catalysis involving macromolecules, micropores seriously hinder mass transfer and diffusion,...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08J9/28B01J20/22B01J20/30B01J31/22B01J35/10
CPCB01J20/226C08G83/008C08J9/28B01J20/3057B01J31/1691B01J31/2239B01J2531/0213B01J2531/16C08J2387/00B01J35/60
Inventor 奚红霞李非儿段崇雄李金清
Owner SOUTH CHINA UNIV OF TECH
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