Large scale fluorine-free synthesis of hierarchically porous iron(III) trimesate MIL-100(Fe) with a zeolite MTN topology

You Kyong Seo, Ji Woong Yoon, Ji Sun Lee, U. Hwang Lee, Young Kyu Hwang, Chul-Ho Jun, Patricia Horcajada, Christian Serre, Jong San Chang

Research output: Contribution to journalArticle

134 Citations (Scopus)

Abstract

The hierarchically mesoporous iron(III) trimesate MIL-100(Fe) with a zeolite-MTN topology is known as an advanced functional material that is biocompatible. In this work, the large scale synthesis of MIL-100(Fe) has been achieved by hydrothermal reactions using suitable conditions without HF for the large scale synthesis. Although such conditions are narrow, the concurrent change of iron precursor and increase in the concentration of reaction mixture give rise to a synergetic effect leading to an increase in the crystallinity of F-free MIL-100(Fe). This method, combined with two purification steps (solvent extraction and chemical treatment with NH 4F) leads to a highly porous F-free material obtained throughout a very high space-time-yield (>1700 kg/m 3 day). Possible formation mechanisms of MIL-100(Fe) under hydrothermal conditions have been proposed in terms of four steps such as hydrolysis, deprotonation, self-assembly, and polycondensation. The resulting material exhibits similar physicochemical properties to those of the one prepared in the presence of HF, except for a slight difference in sorption capacities of gases and liquid vapors corresponding to the difference of pore volume. Regardless of the use of HF, the purified MIL-100(Fe) possesses very high uptakes for both non-polar toluene and polar ethanol probe molecules due to the respective interactions with hydrophilic and hydrophobic sites in the framework. Finally, hydrophobicity measurements confirm that the dehydrated MIL-100(Fe) is more hydrophobic than conventional zeolite beta (SiO 2/Al 2O 3 = 25) and commercial iron trimesate (Basolite F300) from BASF SE.

Original languageEnglish
Pages (from-to)137-145
Number of pages9
JournalMicroporous and Mesoporous Materials
Volume157
DOIs
Publication statusPublished - 2012 Jul 15

Fingerprint

Zeolites
Fluorine
fluorine
topology
Iron
Topology
iron
synthesis
solvent extraction
Deprotonation
Functional materials
Solvent extraction
Polycondensation
Hydrophobicity
hydrophobicity
purification
sorption
Self assembly
Purification
Toluene

All Science Journal Classification (ASJC) codes

  • Chemistry(all)
  • Materials Science(all)
  • Condensed Matter Physics
  • Mechanics of Materials

Cite this

Seo, You Kyong ; Yoon, Ji Woong ; Lee, Ji Sun ; Lee, U. Hwang ; Hwang, Young Kyu ; Jun, Chul-Ho ; Horcajada, Patricia ; Serre, Christian ; Chang, Jong San. / Large scale fluorine-free synthesis of hierarchically porous iron(III) trimesate MIL-100(Fe) with a zeolite MTN topology. In: Microporous and Mesoporous Materials. 2012 ; Vol. 157. pp. 137-145.
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abstract = "The hierarchically mesoporous iron(III) trimesate MIL-100(Fe) with a zeolite-MTN topology is known as an advanced functional material that is biocompatible. In this work, the large scale synthesis of MIL-100(Fe) has been achieved by hydrothermal reactions using suitable conditions without HF for the large scale synthesis. Although such conditions are narrow, the concurrent change of iron precursor and increase in the concentration of reaction mixture give rise to a synergetic effect leading to an increase in the crystallinity of F-free MIL-100(Fe). This method, combined with two purification steps (solvent extraction and chemical treatment with NH 4F) leads to a highly porous F-free material obtained throughout a very high space-time-yield (>1700 kg/m 3 day). Possible formation mechanisms of MIL-100(Fe) under hydrothermal conditions have been proposed in terms of four steps such as hydrolysis, deprotonation, self-assembly, and polycondensation. The resulting material exhibits similar physicochemical properties to those of the one prepared in the presence of HF, except for a slight difference in sorption capacities of gases and liquid vapors corresponding to the difference of pore volume. Regardless of the use of HF, the purified MIL-100(Fe) possesses very high uptakes for both non-polar toluene and polar ethanol probe molecules due to the respective interactions with hydrophilic and hydrophobic sites in the framework. Finally, hydrophobicity measurements confirm that the dehydrated MIL-100(Fe) is more hydrophobic than conventional zeolite beta (SiO 2/Al 2O 3 = 25) and commercial iron trimesate (Basolite F300) from BASF SE.",
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Large scale fluorine-free synthesis of hierarchically porous iron(III) trimesate MIL-100(Fe) with a zeolite MTN topology. / Seo, You Kyong; Yoon, Ji Woong; Lee, Ji Sun; Lee, U. Hwang; Hwang, Young Kyu; Jun, Chul-Ho; Horcajada, Patricia; Serre, Christian; Chang, Jong San.

In: Microporous and Mesoporous Materials, Vol. 157, 15.07.2012, p. 137-145.

Research output: Contribution to journalArticle

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AU - Seo, You Kyong

AU - Yoon, Ji Woong

AU - Lee, Ji Sun

AU - Lee, U. Hwang

AU - Hwang, Young Kyu

AU - Jun, Chul-Ho

AU - Horcajada, Patricia

AU - Serre, Christian

AU - Chang, Jong San

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N2 - The hierarchically mesoporous iron(III) trimesate MIL-100(Fe) with a zeolite-MTN topology is known as an advanced functional material that is biocompatible. In this work, the large scale synthesis of MIL-100(Fe) has been achieved by hydrothermal reactions using suitable conditions without HF for the large scale synthesis. Although such conditions are narrow, the concurrent change of iron precursor and increase in the concentration of reaction mixture give rise to a synergetic effect leading to an increase in the crystallinity of F-free MIL-100(Fe). This method, combined with two purification steps (solvent extraction and chemical treatment with NH 4F) leads to a highly porous F-free material obtained throughout a very high space-time-yield (>1700 kg/m 3 day). Possible formation mechanisms of MIL-100(Fe) under hydrothermal conditions have been proposed in terms of four steps such as hydrolysis, deprotonation, self-assembly, and polycondensation. The resulting material exhibits similar physicochemical properties to those of the one prepared in the presence of HF, except for a slight difference in sorption capacities of gases and liquid vapors corresponding to the difference of pore volume. Regardless of the use of HF, the purified MIL-100(Fe) possesses very high uptakes for both non-polar toluene and polar ethanol probe molecules due to the respective interactions with hydrophilic and hydrophobic sites in the framework. Finally, hydrophobicity measurements confirm that the dehydrated MIL-100(Fe) is more hydrophobic than conventional zeolite beta (SiO 2/Al 2O 3 = 25) and commercial iron trimesate (Basolite F300) from BASF SE.

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