Removal of Confined Ionic Liquid from a Metal Organic Framework by Extraction with Molecular Solvents

Manish P. Singh, Nilesh R. Dhumal, Hyung J Kim, Johannes Kiefer, James A. Anderson

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Abstract

Hybrid materials of ionic liquids (IL) 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 non-porous structure that presents itself as non-uniformly agglomerated micro-rods 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.
Original languageEnglish
Pages (from-to)10577–10586
Number of pages10
JournalThe Journal of Physical Chemistry C
Volume121
Issue number19
Early online date25 Apr 2017
DOIs
Publication statusPublished - 2017

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Ionic Liquids
Ionic liquids
2-Propanol
Metals
Acetone
acetone
Methanol
methyl alcohol
liquids
metals
Water
water
Vibrational spectroscopy
solvent extraction
Hybrid materials
Solvent extraction
energy storage
X ray powder diffraction
Energy storage
Diffraction patterns

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Removal of Confined Ionic Liquid from a Metal Organic Framework by Extraction with Molecular Solvents. / Singh, Manish P.; Dhumal, Nilesh R.; Kim, Hyung J; Kiefer, Johannes; Anderson, James A.

In: The Journal of Physical Chemistry C, Vol. 121, No. 19, 2017, p. 10577–10586.

Research output: Contribution to journalArticle

Singh, Manish P. ; Dhumal, Nilesh R. ; Kim, Hyung J ; Kiefer, Johannes ; Anderson, James A. / Removal of Confined Ionic Liquid from a Metal Organic Framework by Extraction with Molecular Solvents. In: The Journal of Physical Chemistry C. 2017 ; Vol. 121, No. 19. pp. 10577–10586.
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title = "Removal of Confined Ionic Liquid from a Metal Organic Framework by Extraction with Molecular Solvents",
abstract = "Hybrid materials of ionic liquids (IL) 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 non-porous structure that presents itself as non-uniformly agglomerated micro-rods 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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AU - Anderson, James A.

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N2 - Hybrid materials of ionic liquids (IL) 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 non-porous structure that presents itself as non-uniformly agglomerated micro-rods 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.

AB - Hybrid materials of ionic liquids (IL) 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 non-porous structure that presents itself as non-uniformly agglomerated micro-rods 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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