Magnetic metal-organic framework material with core-shell structure and preparation method therefor

A technology of magnetic metals and organic frameworks, applied in the direction of microsphere preparation, alkali metal compounds, chemical instruments and methods, etc., can solve the problems of material waste and difficult separation, improve utilization efficiency, prevent agglomeration, and achieve reliable performance controlling effect

Inactive Publication Date: 2016-01-13
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The material can adsorb and enrich toxic and harmful substances, but it is di

Method used

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  • Magnetic metal-organic framework material with core-shell structure and preparation method therefor
  • Magnetic metal-organic framework material with core-shell structure and preparation method therefor
  • Magnetic metal-organic framework material with core-shell structure and preparation method therefor

Examples

Experimental program
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Example Embodiment

[0039] Example 1. Magnetic Fe 3 O 4 Preparation of UiO-66 material

[0040] (1) Magnetic Fe 3 O 4 Preparation of nanoparticles: 2.6gFeCl 3 ·6H 2 O was dissolved in 50mL of ethylene glycol solution and stirred vigorously to form a clear solution, then 5.75g of NaAc was added, the mixture was stirred magnetically for 30 minutes to obtain a dark brown viscous liquid, and then the changed liquid was transferred to the stainless steel lined with PTFE for reaction In the kettle, heat up to 200°C in a constant temperature blast drying box, and cool to room temperature naturally after 8 hours of reaction. Take out the solution in the kettle, wash it with absolute ethanol and deionized water several times, and dry it under vacuum at 60°C to obtain black powder. Is Fe 3 O 4 Nano particles, the particle size is 600~700nm.

[0041] (2) Magnetic Fe 3 O 4 Modification of particle surface with thioglycolic acid: add 200mg (0.864mmol) Fe 3 O 4 Dissolve in 40mL ethanol for ultrasonic dispersion, tr...

Example Embodiment

[0044] Example 2

[0045] (1) Magnetic Fe 3 O 4 Preparation of nanoparticles: same as Example 1;

[0046] (2) Magnetic Fe 3 O 4 Mercaptoacetic acid modification on particle surface: same as in Example 1;

[0047] (3) Magnetic Fe 3 O 4 UIO-66 material preparation: magnetic Fe modified with thioglycolic acid 3 O 4 Disperse the particles in 10mL DMF, add triethylamine to adjust pH=5, add 10mL 34.3mM ZrCl dropwise under stirring 4 The solution was stirred at 70°C for 30min, washed with DMF and dispersed in 20mL of 17.15mM terephthalic acid solution, and mechanically stirred at 70°C for 1h to obtain magnetic Fe 3 O 4 Magnetic microspheres with UiO-66 porous framework as the core and shell. Repeating the above operation three times, the particle size of the obtained microspheres is 630~760nm, and the thickness of the shell layer is 20~40nm.

[0048] Fe prepared in three cycles 3 O 4 The saturation magnetization of UIO-66 is 67emug -1 . Fe after wrapping UIO-66 three times 3 O 4 The magneti...

Example Embodiment

[0049] Example 3

[0050] (1) Magnetic Fe 3 O 4 Preparation of nanoparticles: same as Example 1;

[0051] (2) Magnetic Fe 3 O 4 Mercaptoacetic acid modification on particle surface: same as in Example 1;

[0052] (3) Magnetic Fe 3 O 4 UIO-66 material preparation: magnetic Fe modified with thioglycolic acid 3 O 4 Disperse the particles in 10mL DMF, add triethylamine to adjust pH=5, add 10mL 34.3mM ZrCl dropwise under stirring 4 The solution was stirred at 70°C for 30min, washed with DMF and dispersed in 20mL of 17.15mM terephthalic acid solution, and mechanically stirred at 70°C for 1h to obtain magnetic Fe 3 O 4 Magnetic microspheres with UiO-66 porous framework as the core and shell. The above operation is continuously repeated 6 times, and the particle size of the obtained microspheres is 660-830 nm, and the thickness of the shell layer is 40-80 nm.

[0053] Fe prepared in 6 cycles 3 O 4 The saturation magnetization of UIO-66 is 52emug -1 . Fe after 6 cycles of wrapping UIO-66 3 O ...

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Abstract

The invention provides a magnetic metal-organic framework material with a core-shell structure and belongs to the field of metal-organic framework materials. According to the material provided by the invention, magnetic microspheres, which take magnetic nano Fe3O4 as cores and take UiO-66 porous frameworks as shells, are prepared through carrying out functional modification on the surface of super-paramagnetic nano Fe3O4 firstly by thioglycollic acid, and then, respectively bonding metal zirconium (Zr) ions and a terephthalic acid ligand to the surface of paramagnetic nano Fe3O4 in a coordinating manner by a layer-by-layer self-assembly method, are regular in shape, have the particle size of 600-700nm, are uniform in particle size distribution and have superparamagnetism, thermal stability, chemical stability and solvent resistance. Due to superparamagnetism, the external magnetic field separation, washing purification, reuse and the like of UiO-66 can be achieved, so that the utilization efficiency of UiO-66 materials is greatly increased.

Description

technical field [0001] The invention belongs to the technical field of magnetic metal organic framework materials, and relates to a magnetic metal organic framework material with a core-shell structure and a preparation method thereof. Background technique [0002] Metal-organic frameworks (MOFs) are porous crystalline materials formed by the self-assembly process of oxygen or nitrogen-containing rigid organic ligands and inorganic metal ion clusters, which have a high specific surface area, regular pore structure, and adjustable pores. Skeletal structures of size and diversity. MOFs have both high crystallinity and strong metal-ligand interactions, and the presence of strong coordination bonds enhances their chemical and thermal stability. These properties make MOFs a new class of multifunctional materials. [0003] The quantum effects and surface effects produced by the small size and large specific surface area of ​​magnetic nanoparticles endow them with many special pr...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30B01J13/02
Inventor 霍淑慧刘萍周鹏鑫张哲喻菁雷自强
Owner NORTHWEST NORMAL UNIVERSITY
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