Nickel based porous solid was synthesized with 20 kHz ultrasonic irradiation. The reaction of Ni(II) nitrate hexahydrate with 1,3,5-benzene tricarboxylic acid in N,N-Dimethylformamide (DMF) as the sole solvent under ultrasonic radiation produced porous Ni-BTC MOF. Choice of correct solvent for the ultrasonic treatment was proven important. The effect of varying ultrasonic powers (40%, 60% and 80% of 750 W) along with different temperature conditions (50 °C, 60 °C, 70 °C and 80 °C) influenced the respective yield. A very high yield of 88% Ni-BTC MOF was obtained from 80% ultrasonic power at 60 °C. BET surface areas of the MOF crystals measured by N2 gas adsorption isotherms were in the range of 960-1000 m(2)/g.
Cu-BTC (BTC=1,3,5-benzenetricarboxylate) metal organic framework (MOF) was synthesized using different solvent conditions with ultrasonic treatment. Solvent mixtures of water/N,N-dimethylformamide (DMF), water/ethanol were used for the reactions with or without a variety of bases under 20 kHz ultrasonically treated conditions. Prepared crystals were purified through 30 min of sonication to remove unreacted chemicals. Treatment time and ultrasonic power effects were compared to get optimum synthetic condition. The characterization of MOF powders was performed by scanning electron microscopy, X-ray powder diffraction, infrared-spectroscopy, thermo-gravimetric analysis and specific surface determination using the BET method. Isolated crystal yields varied with different solvent and applied ultrasonic power conditions. A high isolated crystal yield of 86% was obtained from water/ethanol/DMF solvent system after 120 min of ultrasonic treatment at 40% power of 750 W. Different solvent conditions led to the formation of Cu-BTC with different surface area, and an extremely high surface area of 1430 m(2)/g was obtained from the crystals taken with the solvent condition of water:DMF=70:30.
Ni-BTC (BTC = 1,3,5-benzene tricarboxylate) metal organic framework (MOF) was synthesized using different solvent conditions. Solvent mixtures of water/N,N-dimethylformamide (DMF), water/ethanol, and water/ethanol/DMF were used for the reactions with or without a variety of bases at 160 °C for 48 hours. Even with same green crystals, prepared MOFs show all different BET surface areas and different XRD patterns. The highest BET surface area of the crystals was 850 m 2 /g obtained from water/DMF solvent with NH 4 OH as a base. The measured surface areas of the crystals follows the order of Ni-BTC (water/DMF-NH4OH) > Ni-BTC (water/DMF-TMA) > Ni-BTC (water/DMF) > Ni-BTC (water/DMF-Pyridine) > Ni-BTC (water/ethanol) > Ni-BTC (water/DMF-aniline) > Ni-BTC (water/DMF-NaOH) .
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