Journal of Sol-Gel Science and Technology

, Volume 67, Issue 2, pp 406–413 | Cite as

Gelation behavior and phase separation of macroporous methylsilsesquioxane monoliths prepared by in situ two-step processing

  • Xingzhong Guo
  • Wenyan Li
  • Hui Yang
  • Kazuyoshi Kanamori
  • Yang Zhu
  • Kazuki NakanishiEmail author
Original Paper


An in situ two-step processing using an initial acid catalysis step accompanied by an epoxide-mediated condensation step in the presence of ammonium chloride (NH4Cl) is reported, and macroporous cocontinuous methylsilsesquioxane (MSQ) monoliths have been successfully prepared by this processing. We explain the hydrolysis, gelation behavior and phase separation of MTMS(methyltrimethoxysilane)-MeOH(methanol)-HCl-PO(propylene oxide) system and the in situ effect of NH4Cl, and examine the macroporous morphology and pore structures of MSQ monoliths obtained under different conditions. Macroporous MSQ monolith under optimized conditions possesses a narrow macropore size distribution between 3 to 10 μm, surface area as high as 366 m2·g−1 and minimal shrinkage of only 1 %.


Methylsilsesquioxane Monolith Sol–gel process Phase separation Ammonium chloride 


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Copyright information

© Springer Science+Business Media New York 2013

Authors and Affiliations

  • Xingzhong Guo
    • 1
  • Wenyan Li
    • 1
  • Hui Yang
    • 1
  • Kazuyoshi Kanamori
    • 2
  • Yang Zhu
    • 2
  • Kazuki Nakanishi
    • 2
    Email author
  1. 1.Department of Materials Science and EngineeringZhejiang UniversityHangzhouChina
  2. 2.Department of Chemistry, Graduate School of ScienceKyoto UniversityKyotoJapan

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