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
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[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...
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[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...
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[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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