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Synthesis of Hydrophobic MIL-53(Al)-nanoparticles in Low Weight Alcohols: Systematic Investigation of Solvent Effects

Abstract

The effects of using low-weight alcohols, methanol and ethanol, for the synthesis of MIL-53(Al) are investigated and the results directly compared with analogous synthesis in water and N,N-dimethylformamide (DMF). We have successfully synthesised MIL-53(Al), termed MIL 53(MeOH), using MeOH as solvent and employing a reaction temperature of 150oC, lower than that typically used for analogous water or DMF-based reactions. Several unique properties are observed for MIL 53(MeOH). The breathing phenomenon which is known for MIL-53(Al) derivatives, prepared using water or DMF as reaction solvent, is not observed for samples prepared from methanol and the framework adopts, and remains in, the large-pore form. Thus, measurement of N2-isotherms and calculation of internal surface areas have verified that the synthesis of MIL-53(MeOH) leads to a product which is highly porous with only minimal or no activation required. Furthermore, X-ray diffraction measurements and scanning electron microscopy at different humidity levels reveal a reversible loss of crystallinity at high humidity levels for MIL-53(MeOH) which was not observed previously for any other known MIL-53 derivative. In contrast the synthesis of MIL-53(Al) in ethanol leads of a product with low crystallinity.

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Publication details

The article was received on 01 Jun 2018, accepted on 05 Jul 2018 and first published on 09 Jul 2018


Article type: Paper
DOI: 10.1039/C8CE00913A
Citation: CrystEngComm, 2018, Accepted Manuscript
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    Synthesis of Hydrophobic MIL-53(Al)-nanoparticles in Low Weight Alcohols: Systematic Investigation of Solvent Effects

    J. Warfsmann, B. Tokay and N. R. Champness, CrystEngComm, 2018, Accepted Manuscript , DOI: 10.1039/C8CE00913A

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