Manometric real-time studies of the mechanochemical synthesis of zeolitic imidazolate frameworks

Ivana Brekalo, Wenbing Yuan, Cristina Mottillo, Yuneng Lu, Yuancheng Zhang, Jose Casaban, K. Travis Holman, Stuart L. James, Frédéric Duarte, P. Andrew Williams, Kenneth D.M. Harris, Tomislav Friščić

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Abstract

We demonstrate a simple method for real-time monitoring of mechanochemical synthesis of metal–organic frameworks, by measuring changes in pressure of gas produced in the reaction. Using this manometric method to monitor the mechanosynthesis of the zeolitic imidazolate framework ZIF-8 from basic zinc carbonate reveals an intriguing feedback mechanism in which the initially formed ZIF-8 reacts with the CO2 byproduct to produce a complex metal carbonate phase, the structure of which is determined directly from powder X-ray diffraction data. We also show that the formation of the carbonate phase may be prevented by addition of excess ligand. The excess ligand can subsequently be removed by sublimation, and reused. This enables not only the synthesis but also the purification, as well as the activation of the MOF to be performed entirely without solvent.
Original languageEnglish
Number of pages8
JournalChemical Science
DOIs
Publication statusPublished - 02 Jan 2020

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Brekalo, I., Yuan, W., Mottillo, C., Lu, Y., Zhang, Y., Casaban, J., Holman, K. T., James, S. L., Duarte, F., Williams, P. A., Harris, K. D. M., & Friščić, T. (2020). Manometric real-time studies of the mechanochemical synthesis of zeolitic imidazolate frameworks. Chemical Science. https://doi.org/10.1039/C9SC05514B