Industrial & Engineering Chemistry Research, Vol.58, No.19, 7801-7807, 2019
Dry Gel Conversion Synthesis of Hierarchical Porous MIL-100(Fe) and Its Water Vapor Adsorption/Desorption Performance
With an S-shaped water sorption isotherm and high vapor uptake, as one of the famous metal organic frameworks (MOFs), MIL-100(Fe) (MIL stands for Materials of Institute Lavoisier) has been considered as a very promising candidate for adsorption heat pumps. Usually, MIL-100(Fe) is synthesized by a hydrothermal method under harsh synthesis conditions, such as high temperature and vapor pressure. In this study, in the absence of any solvent, a novel facile MIL-100(Fe) synthetic strategy, which used the dry gel conversion method, was developed. X-ray diffraction (XRD) patterns showed that the new dry gel conversion technology could expediently synthesize MIL-100(Fe) with a low reaction temperature (140 degrees C) and high yield (85%), which is superior to the hydrothermal method with reaction temperature of 160 degrees C and yield of 76%. Scanning electron microscopy (SEM) images illuminated that, compared with the conventional synthesized MIL-100(Fe) in the liquid aqueous solution, the new process synthesized one in the dry gel state exhibited a smaller crystal size (about 50 nm) due to the confined growth of the crystals. The pore analysis indicated that the MIL-100(Fe) synthesized by both processes had a similar hierarchical porous structure with the mesopore and micropore; however, compared with the traditional synthesized adsorbent, the new technology synthesized one possessed a larger pore volume due to the formation of the extra mesopores from the interconnection of the nanocrystals. The static adsorption curve exhibited that the water vapor adsorption capacity of MIL-100(Fe) synthesized by the new process was a little higher than the one synthesized by the traditional hydrothermal method. Moreover, it had a smaller desorption activation energy and better cycle stability.