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

1.
1 Department of Materials Science and Engineering of Zhejiang University, Hangzhou 310027, P. R. China;
2 Department of Chemistry, Graduate School of Science, Kyoto University, Kyoto 606-8502, Japan

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 (M_v): 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.
- Porous monolith,
- Silica,
- Sol-gel,
- Phase separation,
- Propylene oxide,
- Poly(ethylene oxide)
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沈阳化工大学材料科学与工程学院沈阳 110142

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

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