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

Synthesis of MIL‐100(Fe) at Low Temperature and Atmospheric Pressure

“…Therefore, more work is still needed in order to successfully synthesize MOFs under HF-free conditions. Luckily, Seo and coworkers also synthesized MOF-100(Fe) in HF-free conditions [11], with the BET specific surface area and pore volume larger than those obtained in the current case, suggesting that commercial MIL-100(Fe) in large scale is expected in the near future.…”

“…Therefore, it is another benefit when safety operation is taken into consideration. Furthermore, a high MOF yield (>90%) could be achieved for the MIL-100(Fe) synthesized in the current case, probably because of the lower water fraction in the synthesis recipe (see Section 2) than that needed in the literature [7][8][9]11], besides being assisted by stirring during the synthesis. Additionally, the developed MIL-100(Fe) is highly stable in air for more than one month, and no change in XRD pattern was found for the sample during this period (see Figure 1(c)).…”

“…It should be noted that our synthesis is carried out under a dynamic condition in which mass transfer could be significantly intensified; therefore, the synthesis temperature is much lower than that under static conditions applied in the literature. In addition, high (autogeneous) pressure is required in the literature for the conventional hydrothermal synthesis [7][8][9]11], while in the current case the synthesis was carried out at atmospheric pressure. Therefore, it is another benefit when safety operation is taken into consideration.…”

“…Notably, MIL-100(Fe) exhibits a high thermal stability (>270 ∘ C) and a remarkable chemical resistance (organic solvents or water under reflux). In addition, the presence of accessible coordinatively unsaturated metal sites allows the coordination of different species, making it an interesting candidate for many potential applications [8][9][10][11][12][13].…”

“…MIL-100(Fe) is mainly obtained by a hydrothermal synthesis in a Teflon-lined autoclave at high temperature (>150 ∘ C) under static conditions [7][8][9][10][11]. However, this method has several disadvantages, such as high temperature, high (autogeneous) pressure, long time, and comparable low MOF yield.…”