jp7b02289_si_001.pdf (1.83 MB)
Removal of Confined Ionic Liquid from a Metal Organic Framework by Extraction with Molecular Solvents
journal contribution
posted on 2017-04-25, 00:00 authored by Manish
P. Singh, Nilesh R. Dhumal, Hyung J. Kim, Johannes Kiefer, James A. AndersonHybrid
materials of ionic liquids (ILs) confined in metal organic
frameworks (MOF) are promising materials for energy storage. The effects
of exposing or treating such composite materials with molecular solvents,
e.g., with the aim to extract and replace the IL, have not been studied
to date. In this study, acetone, isopropanol, methanol, and water
were used to remove the IL 1-ethyl-3-methylimidazolium ethyl sulfate
confined in a Cu-based metal–organic framework (CuBTC). The
consequences of the solvent extraction process were analyzed using
vibrational spectroscopy (FTIR), powder X-ray diffraction (PXRD),
N2 adsorption, scanning electron microscopy (SEM), and
transmission electron microscopy (TEM). Methanol was identified as
the best solvent for IL removal as it shows high extraction efficiency
without affecting the porous geometry and crystal structure of the
MOF. On the other hand, acetone and isopropanol were not able to completely
remove the IL from CuBTC under the conditions employed. Water effectively
removed the IL, but it has a significant detrimental effect on the
CuBTC structure. This impact manifests as changes in the infrared
spectra and the PXRD patterns as well as in the electron micrographs.
The degraded CuBTC exhibits a nonporous structure that presents itself
as nonuniformly agglomerated microrods along with very few hexagonal/amorphous
phases. The confinement of acetone, isopropanol, and methanol in the
MOF was also investigated. The results show that CuBTC is stable in
acetone, isopropanol, and methanol but unstable in water.
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Keywords
vibrational spectroscopyIL removalresults showPXRD patternsIL 1- ethyl -3-methylimidazolium ethyl sulfateacetoneMolecular Solvents Hybrid materialselectron micrographsnonuniformly agglomerated microrodsMOFFTIRCuBTC structureTEMSEMimpact manifestsscanning electron microscopyenergy storagetransmission electron microscopyCuBTC exhibitsextraction processisopropanolMetal Organic Frameworkcrystal structuremethanolextraction efficiency
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