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Studies on functionalized mesoporous materials—Part I: characterization of silylized mesoporous material of type MCM-41

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Abstract

The synthesis of organic–inorganic composite materials was performed by the surface modification of mesoporous material type MCM-41 by chlorodimethylphenylsilane and dichloromethylphenylsilane. Applying IR spectroscopy, low temperature nitrogen adsorption/desorption (isotherms BET), thermogravimetric measurements and technique of competitive adsorption of toluene and water it was shown that the degree of silylation, hydrophobicity, surface and volume properties (pore size distribution, pore volume) strongly depends on the nature of silylation agent and the ratio of calculated amount of silanol groups to the modifier. Two types of condensation reaction take place: (1) the reaction of the modifier with surface silanol groups, and (2) an inter-molecular condensation of the modifier, resulting in additional pore blocking. Only 24–36 % of the surface silanol groups react with modifier agent. The materials are stable up to temperatures of about 170 °C that is higher than the corresponding polymeric resins. The TG/DTA data allowed concluding that the degree of grafting depends on the ratio silylation agent to SiOH groups. As shown by Fourier transform diffuse reflectance mode spectroscopy only free silanol groups react with modifier.

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Acknowledgments

This work was financially supported by the German Academic Exchange Service (DAAD) and Russian Ministry of Education and Science in the frame of program “Mikhail Lomonosov”. The authors are grateful to M. Wickleder and M.Ahlers (Institute of Chemistry, Carl von Ossietzky University, Germany) for TGA/DTA measurements. We also thank E. Borodina, F. Kirby (University of Utrecht, Department of Inorganic Chemistry and Catalysis) and E. Corker (Technical University of Denmark, Department of Chemistry) for valuable discussion.

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Authors and Affiliations

  1. Voronezh State University, Voronezh, Russia

    S. I. Karpov & V. F. Selemenev

  2. Industrial Chemistry 2, Carl von Ossietzky University, 26111, Oldenburg, Germany

    F. Roessner

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  1. S. I. Karpov
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  2. F. Roessner
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  3. V. F. Selemenev
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Correspondence to S. I. Karpov.

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Karpov, S.I., Roessner, F. & Selemenev, V.F. Studies on functionalized mesoporous materials—Part I: characterization of silylized mesoporous material of type MCM-41. J Porous Mater 21, 449–457 (2014). https://doi.org/10.1007/s10934-014-9791-x

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