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Breaking Phase-Selectivity Barriers: Scalable Room-Temperature Synthesis and Catalytic Properties of Functionalized
Yonghong Xiao1,2,3, Yue Diao1, Li-Tian Zhang1,3
1College of Chemistry & Chemical Engineering, Key Laboratory for Preparation and Application of Ordered Structural Materials of Guangdong Province, Shantou University, Guangdong515063, China.
Inorganic Chemistry
|July 22, 2026
Summary
A new room-temperature synthesis method produces phase-pure MIL-101(Fe) metal-organic frameworks (MOFs) at scale. This approach enables solvent recycling and controls phase formation based on substituent size for diverse applications.
Area of Science:
- Materials Science
- Nanotechnology
- Catalysis
Background:
- Sustainable and scalable synthesis of metal-organic frameworks (MOFs) is vital for industrial use.
- Achieving phase purity at room temperature, especially for kinetically metastable MOFs like MIL-101(Fe), is challenging.
Purpose of the Study:
- To develop a room-temperature synthesis strategy for gram-scale, phase-pure MIL-101(Fe).
- To establish substituent-dependent synthesis rules for functionalized MIL-101(Fe) materials.
- To evaluate the catalytic performance of functionalized MIL-101(Fe) in diindolylmethane synthesis.
Main Methods:
- A ternary solvent system (dioxane/pyridine/H2O) with pyridine as a phase-directing agent was employed.
- Systematic investigation of steric effects on solvent selection for substituent-dependent synthesis.
- Evaluation of synthesized MIL-101(Fe) derivatives as heterogeneous catalysts.
Main Results:
- Gram-scale (∼50 g/batch) production of phase-pure MIL-101(Fe) achieved at room temperature with solvent recyclability.
- Pyridine-directed synthesis kinetically favored MIL-101(Fe) over thermodynamic products.
- Substituent-dependent synthesis rules were established, utilizing different solvent systems (dioxane/pyridine/H2O or DMF/DMA) for small vs. bulky/multiple substituents.
Conclusions:
- A scalable, room-temperature synthesis framework for phase-pure MIL-101(Fe) and its derivatives was established.
- The developed method links substituent identity, synthetic conditions, and catalytic performance.
- Functionalized MIL-101(Fe) materials show promise as heterogeneous catalysts for solvent-free reactions.

