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

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

*Corresponding author for this work

Research output: Contribution to journalArticle (Academic Journal)

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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 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.

Original languageEnglish
Article number17
Number of pages28
JournalCrystals
Volume10
Issue number1
DOIs
Publication statusPublished - 31 Dec 2019

Keywords

  • metal-organic framework
  • Supercritical CO<inf>2</inf>
  • crystallisation

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