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Large Scale Fluorine-Free Synthesis of Hierarchically Porous Iron(III) Trimesate MIL-100(Fe) with a Zeolite MTN Topology
Summary:
The authors fromKorea Research Institute of Chemical Technology (KRICT), Yonsei University, and Université de Versailles developed afluorine-free, hierarchically porous iron(III) trimesate MIL-100(Fe) with zeolite MTN topology, achievinghigh space-time yield (>1700 kg/m³·day) and superior adsorption performance for non-polar (toluene) and polar (ethanol) molecules.


Background:
1.Previous Work & Limitations: Conventional MIL-100(Fe) synthesis relies on corrosive HF as a mineralizing agent, hindering large-scale production. Alternative fluoride-free routes yielded low crystallinity/porosity.
2.Innovation: The authors pioneered ahigh-concentration hydrothermal method using Fe(NO₃)₃·9H₂O combined withsolvent extraction + NH₄F purification, achieving scalable, high-quality MIL-100(Fe) without HF.


Research Content:
1.Synthesis:
- Hydrothermal reaction of Fe(NO₃)₃·9H₂O + trimesic acid (1:0.67 molar ratio) at 160°C for 12 h.
- Purification via hot water/ethanol extraction + 38 mM NH₄F treatment.
2.Characterizations:
-BET: Surface area 1800–2280 m²/g; pore volume 1.04 cm³/g.
-SEM/TEM: Uniform octahedral particles (~200–500 nm).
-XRD/FTIR: Confirmed zeolite MTN topology and purity.
3.Application:
-Adsorption: High uptake for toluene (6.51 mmol/g) and ethanol (13.2 mmol/g).
-Hydrophobicity: HI = 2.87 (superior to zeolite β and Basolite F300).
4.Mechanism:
-Synergistic effect: High precursor concentration + nitrate anions stabilized Fe₃O trimers, compensating for fluoride’s absence.
-Pore structure: Hierarchical meso/micropores enabled dual adsorption sites (hydrophilic/hydrophobic).

Outlook:
This work enablesscalable, eco-friendly MIL-100(Fe) production for gas/liquid separation, catalysis, and drug delivery, advancing MOF industrialization.
Large Scale Fluorine-Free Synthesis of Hierarchically Porous Iron(III) Trimesate MIL-100(Fe) with a Zeolite MTN Topology
Authors: You-Kyong Seo, Ji Woong Yoon, Ji Sun Lee, et al.
DOI: 10.1016/j.micromeso.2012.02.027
Link: https://www.sciencedirect.com/science/article/pii/S1387181112000935
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