High yield synthesis of Ni-BTC metal–organic framework with ultrasonic irradiation: Role of polar aprotic DMF solvent

• Published in: Ultrasonics sonochemistry 2016-07, Vol.31, p.93-101
• Main Authors: Israr, Farrukh, Chun, Daye, Kim, Yeongmin, Kim, Duk Kyung
• Format: Article
• Language: English
• Subjects: Ni-BTC MOF; Polar aprotic solvent; Power effect; Temperatures effect; Ultrasonic treatment
• ISSN: 1350-4177; 1873-2828
• DOI: 10.1016/j.ultsonch.2015.12.007

•Ultrasonic synthesis of Ni-MOF and the choice of correct solvent during treatment.•Effect of varying ultrasonic power along with probe temperature upon MOF yield has been determined.•80% ultrasonic power with 60°C probe temperature has proved to be the optimum process parameter. Nickel based porous solid was synthesized with 20kHz 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 750W) 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 960–1000m2/g.