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A method for the rapid synthesis of hierarchically porous hkust-1 materials by a dual-functional template method

A HKUST-1, hierarchical pore technology, applied in the field of rapid preparation of hierarchical porous metal-organic framework materials, achieves the effects of energy saving, stable structure, and mild conditions

Active Publication Date: 2020-06-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • A method for the rapid synthesis of hierarchically porous hkust-1 materials by a dual-functional template method
  • A method for the rapid synthesis of hierarchically porous hkust-1 materials by a dual-functional template method
  • A method for the rapid synthesis of hierarchically porous hkust-1 materials by a dual-functional template method

Examples

Experimental program
Comparison scheme
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 invention discloses a method for rapidly synthesizing hierarchical porous HKUST-1 materials using a dual-functional template method. This method can increase the yield and shorten the synthesis time of this material to 30 seconds. The method includes the following steps: converting Cu(NO 3 ) 2 •3H 2 Dissolve O in deionized water, dissolve trimesic acid in methanol, and stir; then mix the two solutions and continue stirring; add the template agent and stir, filter the product and put it into a vacuum drying box to dry. Grade hole HKUST‑1 material. This method only uses N, N, N, N-tetramethylhexanediamine as both template agent and deprotonating agent. It has simple operation, mild conditions and very short reaction time. The synthesized product has a rich pore structure, with both micropores and mesopores, which facilitates the diffusion of macromolecules and has good application prospects in gas adsorption and separation, catalysis, drug delivery, etc.

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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Patent Type & Authority Patents(China)
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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