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

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posted on 07.01.2020, 14:25 by Huan Doan, Fei Cheng, Thandeka Dyirakumunda, Mark Elsegood, Jiamin Chin, Oliver Rowe, Carl Redshaw, Valeska P. Ting
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.

Funding

UK Engineering and Physical Sciences Research Council (EP/R01650X/1 and EP/R023816/1)

History

School

  • Science

Department

  • Chemistry

Published in

Crystals

Volume

10

Issue

1

Publisher

MDPI AG

Version

VoR (Version of Record)

Rights holder

© The Authors

Publisher statement

This is an Open Access Article. It is published by MDPI under the Creative Commons Attribution 4.0 Unported Licence (CC BY). Full details of this licence are available at: http://creativecommons.org/licenses/by/4.0/

Acceptance date

30/12/2019

Publication date

2019-12-31

Copyright date

2020

eISSN

2073-4352

Language

en

Depositor

Dr Mark Elsegood. Deposit date: 2 January 2020

Article number

17

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