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Synthesis of Fe–MOF/COF Hybrid Materials for Methane Adsorption Using Design of Experiments

Min Hyung Lee Sangmin Lee¹ Kye Sang Yoo^†

Department of Energy and Chemical Engineering, Graduate School of Convergence Science , Seoul National University of Science and Technology , Seoul 01811 , Korea ¹Department of Chemical and Biomolecular Engineering , Seoul National University of Science and Technology , Seoul 01811 , Korea

kyoo@seoultech.ac.kr

Korean Journal of Chemical Engineering, February 2024, 41(2), 435-444(10), https://doi.org/10.1007/s11814-024-00015-6

Abstract

This study focuses on the synthesis of Fe–MOF/COF (metal–organic framework/covalent organic framework) materials for

methane adsorption. The synthesis process involves several steps, starting with the preparation of MIL-100(Fe) through the

reaction of trimesic acid and iron(III) nitrate nonahydrate. MIL-100(Fe)_NH 2 is then synthesized by combining MIL-100(Fe)

with ethylenediamine, followed by the synthesis of MIL-100(Fe)/COF through the addition of melamine, terephthalaldehyde,

and dimethylsulfoxide. A defi nitive screening design and mixture method are employed to optimize the synthesis process by

determining the infl uential factors and their respective ratios. The nitrogen content of samples is used as the response variable,

and the optimized precursor molar ratio for MIL-100(Fe)/COF synthesis is estimated. From the main eff ect plots, TPA has the

lowest eff ect on the response. The estimated actual precursor ratio for the optimized synthesis of MIL-100(Fe)/COF is MIL-

100(Fe)_NH 2 :TPA:MEL:DMSO:DIW = 1 mol:13 mol:10 mol:1884 mol:1648 mol. For the methane adsorption, the response

optimizer indicated that MIL-100(Fe)/COF synthesized with a modifi ed molar ratio of 0.1:0.4:0.5 (MEL:DMSO:DIW) was

expected to exhibit the highest value.

Keywords

Fe–MOF · COF hybrid · Toluene adsorption · Design of experiments · Optimization