LNNU-2-series nano-MOF (metal organic framework) type hierarchical porous material and preparation method thereof
A multi-level pore and nanotechnology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of rare distribution of mesopores and small volume of mesopores
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[0024] The preparation method of the LNNU-1 series nano-MOF type hierarchical porous material of the present invention, the steps are as follows:
[0025] ⑴. Select the reaction material: Al(NO 3 ) 3 ×9H 2 O, Tribenzoic acid (BTC), solvent, the molar ratio of each component is as follows:
[0026] Al(NO 3 ) 3 ×9H 2 O: Tribenzoic acid (BTC): solvent = 1.5: 1.0: 200~250;
[0027] The solvent is absolute ethanol or a mixed solvent; the mixed solvent is absolute ethanol + N,N-dimethylformamide (DMF), and the ratio is absolute ethanol and N,N-dimethylformamide The volume ratio of formamide (DMF) is 15:0-3;
[0028] (2) After mixing and stirring the reaction materials, heat the reaction in an oven, the reaction temperature is controlled between 100-120 °C, and the time is 24-168 hours; or microwave heating, the reaction temperature is controlled between 100-120 °C , the time is 1 to 3 minutes;
[0029] (3) After the reaction is completed, cool to room temperature, filter th...
Embodiment 1
[0037] Hierarchical porous material LNNU-2A preparation method:
[0038] 0.60 g (1.6 mmol) Al(NO 3 ) 3 9H 2 O and 0.126 g (0.6 mmol) of BTC were dissolved in 15 mL of absolute ethanol with stirring at room temperature, then transferred to a 30 mL polytetrafluoroethylene reactor and sealed at 120 °C for 24 hours. After cooling to room temperature, the gummy mass was filtered, washed with hot alcohol and dried. The resulting solid material yield is about 96%, MIL-110 (Al) (Fig. 1, X-ray powder map) nanoparticle size is about 10 nm (Fig. 2, SEM), microporous (1.6 nm) and mesoporous (4 nm )(N 2 gas adsorption isotherm and pore size distribution, Fig. 3).
Embodiment 2
[0040] Preparation method of hierarchical porous material LNNU-2B:
[0041] 0.450 g (1.2 mmol) Al(NO 3 ) 3 9H 2 O and 0.095 g (0.45 mmol) of BTC were dissolved in 15 mL of absolute ethanol, stirred at room temperature and then added with 0.439 g (7.5 mmol) of sodium chloride nanoparticles (particle size 300 nm) for ultrasonic mixing. Transfer to 30 milliliters capacity polytetrafluoroethylene reactors airtightly afterward and react at 120 DEG C for 24 hours. After cooling to room temperature, the colloidal substance was dried at room temperature, washed with deionized water to remove NaCl and then washed with absolute ethanol and dried. The resulting MIL-110 (Fig. 4, SEM).
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