Synthesis of hydrophobic MIL-53(Al) nanoparticles in low molecular weight alcohols: systematic investigation of solvent effects

Warfsman, Jan; Tokay, Begum; Champness, Neil

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). When methanol is employed in the synthesis of MIL-53(Al), termed MIL 53(MeOH), several unique properties are observed. 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 without the requirement for an energy-consuming activation process. 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.

Citation

Warfsman, J., Tokay, B., & Champness, N. (2018). Synthesis of hydrophobic MIL-53(Al) nanoparticles in low molecular weight alcohols: systematic investigation of solvent effects. CrystEngComm, 20(32), 4666-4675. https://doi.org/10.1039/C8CE00913A

• Journal Article Type: Article
• Acceptance Date: Jul 5, 2018
• Online Publication Date: Jul 9, 2018
• Publication Date: Aug 28, 2018
• Deposit Date: Oct 18, 2018
• Publicly Available Date: Jul 10, 2019
• Electronic ISSN: 1466-8033
• Publisher: Royal Society of Chemistry
• Peer Reviewed: Peer Reviewed
• Volume: 20
• Issue: 32
• Pages: 4666-4675
• DOI: https://doi.org/10.1039/C8CE00913A
• Public URL: https://nottingham-repository.worktribe.com/output/1175322
• Publisher URL: https://pubs.rsc.org/en/Content/ArticleLanding/2018/CE/C8CE00913A#!divAbstract
• Contract Date: Oct 22, 2018