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

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 using excess ligand, enabling the rational development of first design leading to completely solvent-free and quantitative mechanochemical formation of ZIF-8 on a 90 gram scale, with excess ligand removed by sublimation.

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Article information


Submitted
04 Nov 2019
Accepted
26 Dec 2019
First published
02 Jan 2020

This article is Open Access
All publication charges for this article have been paid for by the Royal Society of Chemistry

Chem. Sci., 2020, Accepted Manuscript
Article type
Edge Article

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

I. Brekalo, W. Yuan, C. Mottillo, Y. Lu, Y. Zhang, J. Casaban, K. T. Holman, S. James, F. Duarte, A. Williams, K. D. M. Harris and T. Friščić, Chem. Sci., 2020, Accepted Manuscript , DOI: 10.1039/C9SC05514B

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