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Synthesis and Modification of a Functionalized 3D Open-Framework Structure with MIL-53 Topology
Summary:
The authors from Christian-Albrechts-Universität, University of Bayreuth, and Université de Versailles St-Quentin en Yvelines developed amino-functionalized MIL-53 (MIL-53-NH₂) with 3D open-framework structure, achieving successful postsynthetic modification and stable porous properties.
Background:
1. MOF functionalization is crucial for applications, but direct synthesis is limited; existing postsynthetic modification lacks systematic study on MIL-53-NH₂ activation and modification.
2. The authors proposed a two-step activation method and formic acid-mediated postsynthetic modification, realizing controllable functionalization of MIL-53-NH₂.
Research Content:
1. Synthesis: Hydrothermally synthesized MIL-53-NH₂(as) using AlCl₃·6H₂O and NH₂-H₂BDC (1:1 molar ratio, 150℃, 5h); activated via DMF exchange and thermal treatment, then modified with formic acid (70℃, 3h).
2. Characterizations:
1) N₂ sorption showed MIL-53-NH₂(lt) has hysteresis, reproducible after repeated activation.
2) XRD confirmed lattice parameters (e.g., as phase: a=16.898Å, b=12.539Å, c=6.647Å) and MIL-53 topology.
3) TG showed frameworks stable up to 400℃; IR/NMR verified formamide group formation.
3. Application: Potential for gas separation, storage, and host-guest chemistry.
4. Mechanism: Framework breathing behavior driven by hydrogen bonds; modification via amino-formic acid amidation without side products.
Outlook:
This research establishes a reliable activation and modification strategy for MIL-53-NH₂, enriching functional MOF synthesis methods and promoting its application in porous material fields.
Synthesis and Modification of a Functionalized 3D Open-Framework Structure with MIL-53 Topology
Authors: Tim Ahnfeldt, Daniel Gunzelmann, Thierry Loiseau, Dunja Hirsemann, Jürgen Senker, Gerard Férey, Norbert Stock
DOI: 10.1021/ic8023265
Link: https://pubs.acs.org/doi/10.1021/ic8023265
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