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

Abstract

MIL-100(Fe), a mesoporous metal-organic framework (MOF), has a large BET specific surface area and pore volume with the presence of a significant amount of accessible Lewis acid metal sites upon dehydration. The structural characteristics of MIL-100(Fe) make it a good candidate for potential applications in gas storage, separation, and heterogeneous catalysis. Mainly, this MOF is obtained by the hydrothermal synthesis in a Teflon-lined autoclave at high temperature (>150 ∘ C) under static conditions. However, this method has several disadvantages such as high temperature, high (autogenous) pressure, long time, and comparable low MOF yield. Therefore, development of a facile method for synthesis of MIL-100(Fe) is vitally important for fundamental understanding and practical application. Herein, MIL-100(Fe) is synthesized by a facile low-temperature (<100 ∘ C) synthesis route at atmospheric pressure by reaction of metallic iron and trimesic acid in water. Due to our synthesis is conducted with agitation, higher MOF yield (>90%) still could be achieved, suggesting that this simple and energy saving method has the potential to be used practically.

Enhanced CO2 adsorption capacity of amine-functionalized MIL-100(Cr) metal–organic frameworks

“…family. [55][56][57] These values, as in previous results, [55][56][57] are underestimated in comparison to van der Waals diameters calculated from crystalline structure. Amine grafted samples show a much reduced nitrogen uptake capacity (Table 1), which may be attributed to grafted amine molecules obstructing nitrogen diffusion as well as to the partial occupation of the space inside the pores.…”

Strategies for Enhancing the Catalytic Performance of Metal–Organic Frameworks in the Fixation of CO2 into Cyclic Carbonates

“…Intense infrared absorption bands at 1642 and 1394 cm −1 characterise the carboxylate groups of the MIL‐100 framework (note that the signal at 1642 cm −1 coincides with that of physisorbed water) . The peaks at around 750 cm −1 are assigned to the ν (C−H) of phenyl rings, the band at 1454 cm −1 is assigned to the ν (C=C) of phenyl rings and the weak band at 1708 cm −1 is assigned to ν (C=O) of residual trimesic acid in the sample . Absorption bands in the 3800–3000 cm −1 region are related to the stretching modes of OH groups (owed to adsorbed water molecules or carboxyl groups) .…”

Ambient pressure synthesis of MIL-100(Fe) MOF from homogeneous solution using a redox pathway

“…This can be attributed to the fact that its syntheses must be carried out in water, mostly at T > 100°C, starting from a heterogeneous reaction mixture containing iron(III) chloride and trimesic acid or its trimethyl ester. 18,20,[28][29][30] The original synthesis procedure for MIL-100(Fe) was developed by Férey et al 18 In this original procedure, hydrofluoric acid, HF was used in strongly acidic solution ( pH < 1, HNO 3 ). The use of HF (a classified chemical toxicant) or acidic fluoride solutions is not desirable for large-scale or commercial syntheses.…”