Issue 8, 2020

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 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.

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

Supplementary files

Article information

Article type
Edge Article
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
Creative Commons BY license

Chem. Sci., 2020,11, 2141-2147

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. L. James, F. Duarte, P. A. Williams, K. D. M. Harris and T. Friščić, Chem. Sci., 2020, 11, 2141 DOI: 10.1039/C9SC05514B

This article is licensed under a Creative Commons Attribution 3.0 Unported Licence. You can use material from this article in other publications without requesting further permissions from the RSC, provided that the correct acknowledgement is given.

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