Citation: GUO Xing-Zhong, SHAN Jia-Qi, DING Li, YU Huan, ZHANG Xiao-Qi, YANG Hui. Preparation and Characterization of Hierarchically Porous Silica Monoliths[J]. Chinese Journal of Inorganic Chemistry, ;2015, (4): 635-640. doi: 10.11862/CJIC.2015.118
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Hierarchically porous SiO2 monoliths were prepared via sol-gel process accompanied by phase separation with tetramethoxysilane (TMOS) as precursor, poly (ethylene oxide) (PEO) as phase separation inducer, propylene oxide(PO) as gelation agent, 0.01 mol·L-1 hydrochloric acid as catalyst, and twelve sodium dodecyl sulfate(SDS) as mesopore forming agent. The resultant monoliths were characterized by differential thermal analysis (DTA), thermogravimetry (TG), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), and nitrogen adsorption/desorption analysis, and the effects of SDS on the macroporous and mesoporous structure of the monoliths were investigated. The results show that the SDS uniformly distributes into the skeletons in the form of micelles, which leads to the formation of mesopores. When SDS is 0.21 g, the optimum hierarchically porous structure is obtained with macropore size of 1~3 μm, mesopore size of 4~5 nm, and BET specific surface area as high as 650 m2·g-1. After heat treatment at 800℃, macroporous structure and mesopores on the skeleton basically remain, and the BET specific surface area still maintains at 421 m2·g-1, which indicates good thermal stability.
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