Citation: GUO Xing-Zhong, LI Wen-Yan, ZHU Yang, NAKANISHI Kazuki, KANAMORI Kazuyoshi, YANG Hui. Macroporous SiO2 Monoliths Prepared via Sol-Gel Process Accompanied by Phase Separation[J]. Acta Physico-Chimica Sinica, ;2013, 29(03): 646-652. doi: 10.3866/PKU.WHXB201212252 shu

Macroporous SiO2 Monoliths Prepared via Sol-Gel Process Accompanied by Phase Separation

  • Received Date: 15 September 2012
    Available Online: 25 December 2012

    Fund Project: 浙江省重点创新团队项目(2009R50010)资助 (2009R50010)

  • Macroporous SiO2 monoliths were prepared via a sol-gel process accompanied by phase separation using a tetramethoxysilane (TMOS) precursor, 0.01 mol·L-1 HCl catalyst, propylene oxide (PO) gelation agent, and poly(ethylene oxide) (PEO, viscosity-averaged molecular weight (Mv): 10000) phase separation inducer. Monoliths were characterized by differential thermal analysis/thermogravimetry (DTA/ TG), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), mercury porosimetry, and nitrogen adsorption/desorption analysis (BET). The mechanism of the epoxide-mediated sol-gel reaction and PEO induced phase separation was discussed. The addition of PEO induced phase separation, and monolithic SiO2 with a cocontinuous macroporous skeletal structure was obtained at PEO/TMOS molar ratio of 0.0018. Monoliths had a narrow pore size distribution of 1-3 μm, surface area as high as 719 m2·g-1 and pore volume of 0.48 m3·g-1. This sol-gel transition is mediated by PO because of its strong nucleophilic properties and irreversible ring-opening reaction. Simultaneous phase separation is induced by PEO adsorbed on the SiO2 oli mers.

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