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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 difficult to separate them from complex systems, resulting in waste of materials

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
Comparison scheme
Effect test

Embodiment 1

[0039] Embodiment 1, magnetic Fe 3 o 4 Preparation of UiO-66 material

[0040] (1) Magnetic Fe 3 o 4 Preparation of nanoparticles: 2.6g FeCl 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, and the mixture was magnetically stirred for 30min to obtain a dark brown viscous liquid, and then the liquid was transferred to a PTFE-lined stainless steel reaction In the kettle, the temperature was raised to 200°C in a constant temperature blast drying oven, and after 8 hours of reaction, it was naturally cooled to room temperature. The solution in the kettle was taken out, washed several times with absolute ethanol and deionized water, and vacuum-dried at 60°C to obtain a black powder. is Fe 3 o 4 Nanoparticles, the particle size is 600~700nm.

[0041] (2) Magnetic Fe 3 o 4 Particle surface thioglycolic acid modification: 200mg (0.864mmol) Fe 3 o 4 Dissolve in 40mL ethanol and ultrason...

Embodiment 2

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

[0046] (2) Magnetic Fe 3 o 4 Particle surface modification with thioglycolic acid: same as Example 1;

[0047] (3) Magnetic Fe 3 o 4 Preparation of UIO-66 material: Magnetic Fe modified with thioglycolic acid 3 o 4 Disperse the particles in 10mL of DMF, add triethylamine to adjust the pH=5, add 10mL of 34.3mM ZrCl dropwise under stirring 4 solution, stirred at 70°C for 30min, washed with DMF, 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 skeleton as the core. The above operation was repeated 3 times, and the obtained microspheres had a particle size of 630-760 nm and a shell thickness of 20-40 nm.

[0048] Fe prepared by cycling three times 3 o 4 UIO-66 has a saturation magnetization of 67 emug -1 . Fe wrapped with UIO-66 after three cycles 3 o 4 The magnetization...

Embodiment 3

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

[0051] (2) Magnetic Fe 3 o 4 Particle surface modification with thioglycolic acid: same as Example 1;

[0052] (3) Magnetic Fe 3 o 4 Preparation of UIO-66 material: Magnetic Fe modified with thioglycolic acid 3 o 4 Disperse the particles in 10mL of DMF, add triethylamine to adjust the pH=5, add 10mL of 34.3mM ZrCl dropwise under stirring 4 solution, stirred at 70°C for 30min, washed with DMF, 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 skeleton as the core. Continuously repeat the above operation 6 times, and the obtained microspheres have a particle size of 660-830 nm and a shell thickness of 40-80 nm.

[0053] Fe prepared by cycling 6 times 3 o 4 The saturation magnetization of UIO-66 is 52emug -1 . Fe after 6 cycles of wrapping UIO-66 3 o 4 The decreased magn...

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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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