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Using supercritical CO2 in the preparation of metal-organic frameworks: Investigating effects on crystallisation

Elsegood, Mark R.J.; Doan, Huan V.; Cheng, Fei; Dyirakumunda, Thandeka; Elsegood, Mark; Chin, Jiamin; Rowe, Oliver; Redshaw, Carl; Ting, Valeska P.

Authors

Mark R.J. Elsegood

Huan V. Doan

Fei Cheng

Thandeka Dyirakumunda

Mark Elsegood

Jiamin Chin

Oliver Rowe

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Professor Carl Redshaw C.Redshaw@hull.ac.uk
Professor of Inorganic Materials Chemistry and REF Lead for Chemistry

Valeska P. Ting



Abstract

© 2019 by the authors. Licensee MDPI, Basel, Switzerland. In this report, we explore the use of supercritical CO2 (scCO2) in the synthesis of well-known metal-organic frameworks (MOFs) including Zn-MOF-74 and UiO-66, as well as on the preparation of [Cu24(OH-mBDC)24]n metal-organic polyhedra (MOPs) and two new MOF structures {[Zn2(L1)(DPE)]∙4H2O}n and {[Zn3(L1)3(4,4’-azopy)]∙7.5H2O}n, where BTC = benzene-1,3,5-tricarboxylate, BDC = benzene-1,4-dicarboxylate, L1 = 4-carboxy-phenylene-methyleneamino-4-benzoate, DPE = 1,2-di(4-pyridyl)ethylene, 4.4’-azopy = 4,4’- azopyridine, and compare the results versus traditional solvothermal preparations at low temperatures (i.e., 40 °Ϲ). The objective of the work was to see if the sames or different products would result from the ssCO2 route versus the solvothermal method. We were interested to see which method produced the highest yield, the cleanest product and what types of morphology resulted. While there was no evidence of additional meso- or macroporosity in these MOFs/MOPs nor any significant improvements in product yields through the addition of scCO2 to these systems, it was shown that the use of scCO2 can have an effect on crystallinity, crystal size and morphology.

Citation

Elsegood, M. R., Doan, H. V., Cheng, F., Dyirakumunda, T., Elsegood, M., Chin, J., …Ting, V. P. (2020). Using supercritical CO2 in the preparation of metal-organic frameworks: Investigating effects on crystallisation. Crystals, 10(1), Article 17. https://doi.org/10.3390/cryst10010017

Journal Article Type Article
Acceptance Date Dec 30, 2019
Online Publication Date Dec 31, 2019
Publication Date 2020-01
Deposit Date Jan 2, 2020
Publicly Available Date Jan 3, 2020
Journal Crystals
Electronic ISSN 2073-4352
Publisher MDPI
Peer Reviewed Peer Reviewed
Volume 10
Issue 1
Article Number 17
DOI https://doi.org/10.3390/cryst10010017
Keywords Metal-organic framework; Supercritical CO2; Crystallisation
Public URL https://hull-repository.worktribe.com/output/3340425
Publisher URL https://www.mdpi.com/2073-4352/10/1/17

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