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Acta Phys. Chim. Sin.  2013, Vol. 29 Issue (03): 646-652    DOI: 10.3866/PKU.WHXB201212252
PHYSICAL CHEMISTRY OF MATERIALS     
Macroporous SiO2 Monoliths Prepared via Sol-Gel Process Accompanied by Phase Separation
GUO Xing-Zhong1, LI Wen-Yan1, ZHU Yang2, NAKANISHI Kazuki2, KANAMORI Kazuyoshi2, YANG Hui1
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
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Abstract  

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 oligomers.



Key wordsPorous monolith      Silica      Sol-gel      Phase separation      Propylene oxide      Poly(ethylene oxide)     
Received: 15 September 2012      Published: 25 December 2012
MSC2000:  O647  
Fund:  

The project was supported by the Key Innovation Team Project of Zhejiang Province, China (2009R50010).

Cite this article:

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. Acta Phys. Chim. Sin., 2013, 29(03): 646-652.

URL:

http://www.whxb.pku.edu.cn/Jwk_wk/wlhx/10.3866/PKU.WHXB201212252     OR     http://www.whxb.pku.edu.cn/Jwk_wk/wlhx/Y2013/V29/I03/646

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