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

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Department of Mechanical Engineering, University of Bristol, Bristol BS8 1TR, UK
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Department of Oil Refining and Petrochemistry, Faculty of Oil and Gas, Hanoi University of Mining and Geology, Duc Thang, Bac Tu Liem, Hanoi 10000, Vietnam
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Department of Chemistry & Biochemistry, University of Hull, Cottingham Rd, Hull HU6 7RX, UK
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Chemistry Department, Loughborough University, Loughborough, Leicestershire LE11 3TU, UK
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Department of Physical Chemistry, Faculty of Chemistry, University of Vienna, 1090 Vienna, Austria
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Energy Materials Laboratory, School of Chemistry, University of East Anglia, Norwich NR4 7TJ, UK
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Authors to whom correspondence should be addressed.
Crystals 2020, 10(1), 17; https://doi.org/10.3390/cryst10010017
Received: 3 December 2019 / Revised: 26 December 2019 / Accepted: 30 December 2019 / Published: 31 December 2019
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 °C). The objective of the work was to see if the same or different products would result from the scCO2 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. View Full-Text
Keywords: metal-organic framework; supercritical CO2; crystallisation metal-organic framework; supercritical CO2; crystallisation
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Doan, H.V.; Cheng, F.; Dyirakumunda, T.; Elsegood, M.R.J.; Chin, J.; Rowe, O.; Redshaw, C.; Ting, V.P. Using Supercritical CO2 in the Preparation of Metal-Organic Frameworks: Investigating Effects on Crystallisation. Crystals 2020, 10, 17.

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