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Preparation method for metal-organic framework nanoparticle material with mesoporous structure

A technology of organic framework and mesoporous structure is applied in the field of preparation of metal-organic framework nanoparticle materials, which can solve the problems of difficult preparation of mesoporous structure and large particle size of materials, and achieve the effect of high specific surface area and large adsorption capacity.

Inactive Publication Date: 2014-07-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method for preparing nano-scale metal-organic framework materials with mesoporous structures under mild conditions for the problems that the mesoporous structure of existing metal-organic framework materials is difficult to prepare and the material particle size is large

Method used

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  • Preparation method for metal-organic framework nanoparticle material with mesoporous structure
  • Preparation method for metal-organic framework nanoparticle material with mesoporous structure
  • Preparation method for metal-organic framework nanoparticle material with mesoporous structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Dissolve 0.0081g of CTAB and 0.0018g of CA mixture (the molar ratio of CTAB and CA is 2.3) in 25mL of N,N-dimethylformamide, sonicate for 10min to fully dissolve.

[0029] 2. Slowly add 0.6758g of ferric chloride hexahydrate and 0.4150g of 1,4-terephthalic acid into the above solution, and continue to sonicate until a uniform and transparent solution is obtained. (The ratio of soluble metal inorganic salts, organic ligand molecules and organic solvents is 1:1:129).

[0030] 3. Put the transparent solution obtained in 2 into the hydrothermal reaction kettle, and react at 75°C for 96h.

[0031] 4. After the reaction, centrifuge the reaction solution to remove the N,N-dimethylformamide reaction solution.

[0032] 5. The crude product was then washed twice with N,N-dimethylformamide to remove unreacted raw materials.

[0033] 6. Use 1M ammonium nitrate in ethanol / water (V / V=1:2) solution to ion-exchange the solid obtained in 5 at 60°C for 24 hours to remove the templat...

Embodiment 2

[0036] 1. Dissolve 0.0081g of CTAB and 0.0021g of CA mixture (the molar ratio of CTAB and CA is 2.03) in 25mL of N,N-dimethylformamide, sonicate for 10min to fully dissolve.

[0037]2. Slowly add 0.6758g of ferric chloride hexahydrate and 0.4150g of 1,4-terephthalic acid into the above solution, and continue to sonicate until a uniform and transparent solution is obtained.

[0038] 3. Put the transparent solution obtained in 2 into the hydrothermal reaction kettle, and react at 75°C for 96h.

[0039] 4. After the reaction, centrifuge the reaction solution to remove the N,N-dimethylformamide reaction solution.

[0040] 5. The crude product was then washed twice with N,N-dimethylformamide to remove unreacted raw materials.

[0041] 6. Use 1M ammonium nitrate in ethanol / water (V / V=1:2) solution to ion-exchange the solid obtained in 5 at 60°C for 24 hours to remove the template agent.

[0042] 7. Finally, wash the product removed from the template agent in 6 with ethanol / water s...

Embodiment 3

[0044] 1. Dissolve 0.0081g of CTAB and 0.0040g of CA mixture (the molar ratio of CTAB and CA is 1.15) in 25mL of N,N-dimethylformamide, sonicate for 10min to fully dissolve.

[0045] 2. Slowly add 0.6758g of ferric chloride hexahydrate and 0.4150g of 1,4-terephthalic acid into the above solution, and continue to sonicate until a uniform and transparent solution is obtained.

[0046] 3. Put the transparent solution obtained in 2 into the hydrothermal reaction kettle, and react at 75°C for 96h.

[0047] 4. After the reaction, centrifuge the reaction solution to remove the N,N-dimethylformamide reaction solution.

[0048] 5. The crude product was then washed twice with N,N-dimethylformamide to remove unreacted raw materials.

[0049] 6. Use 1M ammonium nitrate in ethanol / water (V / V=1:2) solution to ion-exchange the solid obtained in 5 at 60°C for 24 hours to remove the template agent.

[0050] 7. Finally, wash the product removed from the template agent in 6 with ethanol / water ...

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Abstract

The invention relates to a preparation method for a metal-organic framework nanoparticle material with a mesoporous structure. The method comprises the steps of: dissolving a cationic template molecule and an anionic ligand molecule able to undergo electrostatic pairing with the cationic template molecule in an organic solvent, adding a soluble metal inorganic salt and a micromolecular organic-ligand molecule able to achieve coordination bonding with the metal ion so as to undergo solvothermal reaction under a proper temperature, thus obtaining the metal-organic framework nanoparticle with a mesoporous structure. The metal-organic framework nano-material prepared by the invention has an aperture in a mesoporous range, has high specific surface area and large adsorption capacity, and can be used in drug delivery systems, bioanalysis and detection, film fixation and other fields.

Description

technical field [0001] The invention belongs to the field of metal-organic framework materials, and in particular relates to a preparation method of metal-organic framework nanoparticle materials with mesoporous structures. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs) are a class of materials with an infinite network structure formed by the self-assembly of metal ions or metal ion clusters and organic ligand molecules. This type of material has diverse and easily functionalized structures, large specific surface area and porosity, and has shown superiority in the fields of gas storage, adsorption separation, molecular recognition, photoelectromagnetic catalysis, ion exchange, imaging and drug delivery systems. application prospects. [0003] However, most of the metal-organic framework materials synthesized now have a microporous structure, and the pore size is generally less than 2 nanometers (J.Am.Chem.Soc.2006, 128, 16474). Alt...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30A61K47/12
Inventor 吴仁安刘荣徐桂菊
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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