在不添加氢氟酸的条件下,以九水合硝酸铁和1,3,5-均苯三甲酸(H3BTC)为原料,用水热合成法制备了多孔铁的三聚物金属有机骨架材料(Fe-MIL-100)。采用XRD、BET、SEM、FT-IR和TG等手段表征Fe-MIL-100样品的结晶度、比表面积、形貌和热稳定性,研究了晶化过程中晶化温度、HNO3添加量、晶化时间以及后处理条件对Fe-MIL-100材料结构的影响。优化合成工艺条件后,制备出结晶度较高、热稳定性优异、比表面积可达1744 m2/g、在氮气氛下热分解温度可达520℃的Fe-MIL-100材料。
Hierarchically porous iron(Ⅲ) trimesate Fe-MIL-100 were synthesized by hydro-thermal route of HF free in a large scale, with ironic nitrate and trimesic acid as raw materials. The structure and morphology of Fe-MIL-100 were characterized by X-ray diffraction(XRD), N2 physical adsorption, scanning electron microscopy(SEM), Fourier transform infrared spectroscopy(FTIR) and thermogravimetric analysis(TG). The effect of temperature, HNO3 addition, time and post-treatment on the structure of FeMIL-100 were investigated. The results show that the prepared Fe-MIL-100 has high crystallinity with BET surface area up to 1744 m2/g. The prepared materials have good thermal stability, which can withstand temperature up to 520°C before decomposition in nitrogen.