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Manometric Real-Time Studies of the Mechanochemical Synthesis of Zeolitic Imidazolate Frameworks

preprint
submitted on 26.07.2019 and posted on 29.07.2019 by 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 Friscic
We demonstrate a 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 from powder X-ray diffraction data. Formation of the carbonate phase may be prevented by using excess ligand, leading to quantitative formation of ZIF-8. This reaction was performed on a 90 g scale, with the excess ligand removed by sublimation.

Funding

DMR-1610882

I2IPJ 485231-2015

RGPIN-2017-06467

History

Email Address of Submitting Author

ib308@georgetown.edu

Institution

Georgetown University

Country

United States

ORCID For Submitting Author

0000-0002-0309-5610

Declaration of Conflict of Interest

No conflict of interest

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