Preparation method of hollow metal organic framework material
A metal-organic framework and organic framework technology are applied in the field of preparation of hollow metal-organic framework materials, which can solve the problems of easy formation of mixtures, lack of universality, and difficulty in controlling the shape, so as to reduce operation steps, avoid framework collapse, and reduce costs. Effect
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[0029] The preparation method of the above-mentioned hollow metal organic framework material comprises the following steps:
[0030] (1) adding the metal and the organic ligand into an organic solvent to dissolve, and mixing and stirring the two solutions, then centrifuging, washing, and drying to obtain a metal-organic framework material precursor; the stirring reaction time is 24 hours; drying temperature is 60℃-120℃.
[0031] Preferably, the metal is a transition metal zinc (Zn 2+ ) ions, metallic cobalt (Co 2+ ) ions and metallic iron ions (Fe 3 + ); preferably, the metal ion compound is a soluble inorganic salt of transition metal ion, more preferably nitrate and chloride.
[0032] The organic ligands are nitrogen heterocyclic ligands and carboxylic acid ligands, and the nitrogen heterocyclic ligands are 2-methylimidazole.
[0033] The organic solvents were N,N-dimethylformamide (DMF), methanol (MeOH) and ethanol (EtOH).
[0034] (2) ultrasonically dispersing the me...
Embodiment 1
[0040] Example 1 A preparation method of a hollow metal organic framework material, (1) Weigh 2.38 grams of zinc nitrate hexahydrate, add 36 milliliters of DMF, 12 milliliters of methanol and 12 milliliters of ethanol, stir and dissolve to obtain solution A. Weigh 4 g of 2-methylimidazole, add 12 ml of DMF and 8 ml of methanol, stir and dissolve to obtain solution B. The B solution was added to the A solution, and the reaction was stirred at room temperature for 24 hours, centrifuged, washed with methanol, and dried at 80° C. to obtain the metal-organic framework material ZIF-8.
[0041](2) Weigh 250 mg of ZIF-8, add 10.68 ml of deionized water, and dissolve by ultrasonic. Add 45 microliters of pyrrole, stir at low temperature for 30 minutes at 0°C, then dropwise add 0.675 ml (concentration of 80 mg / ml) aqueous ammonium persulfate solution, continue to stir at low temperature for 2 hours at 0°C, then stir at room temperature for 8 hours, centrifuge , washed with methanol, and...
Embodiment 2
[0042] Embodiment 2 A kind of preparation method of hollow metal organic framework material,
[0043] (1) Weigh 5.82 g of cobalt nitrate hexahydrate, add 200 mL of methanol, stir and dissolve to obtain solution A. Weigh 6.56 g of 2-methylimidazole, add 200 mL of methanol, stir and dissolve to obtain solution B. Add solution B to solution A, sonicate for 30 min, stand at room temperature for 24 h, centrifuge, wash with methanol, and dry at 80°C to obtain metal-organic framework material ZIF-67.
[0044] (2) Weigh 250 mg of ZIF-67, add 16.5 ml of deionized water, and dissolve by ultrasonic. Add 100 microliters of pyrrole, stir at low temperature for 30 minutes at 0 °C, then add 1.5 ml (concentration of 80 mg / ml) ammonium persulfate dropwise, continue to stir at low temperature at 0 °C for 2 hours, then stir at room temperature for 8 hours, centrifuge, methanol Washed and freeze-dried to obtain hollow ZIF-67 metal-organic framework material.
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