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Using Supercritical CO2 in the Preparation of Metal-Organic Frameworks: Investigating Effects on Crystallisation

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

Authors

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

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 same 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.

Journal Article Type Article
Journal Crystals
Print ISSN 2073-4352
Publisher MDPI
Peer Reviewed Peer Reviewed
Volume 10
Issue 1
Article Number 17
APA6 Citation Doan, H. V., Cheng, F., Dyirakumunda, T., Elsegood, M., Chin, J., Rowe, O., …Ting, V. P. (in press). Using Supercritical CO2 in the Preparation of Metal-Organic Frameworks: Investigating Effects on Crystallisation. Crystals, 10(1), https://doi.org/10.3390/cryst10010017
DOI https://doi.org/10.3390/cryst10010017
Keywords Inorganic Chemistry; General Materials Science; General Chemical Engineering; Condensed Matter Physics

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