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Synthesis and structure-related adsorption characteristics of bifunctional polysiloxane xerogels with methyl and 3-mercaptopropyl groups

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Abstract

Polysiloxane xerogels containing 3-mercaptopropyl and methyl groups in the surface layer were synthesized by the sol-gel method with ethanol used as a solvent and fluoride ion used as a catalyst. It is established that an increase in the relative content of methyltriethoxysilane in the initial reaction mixture results in formation of xerogels with a developed porous structure. The tendency for an increase in other characteristics of porous structure, the sorption volume and pore size, is also observed. The analogous effect is found upon increasing relative content of tetraethoxysilane with a constant ratio between two trifunctional silanes. By means of atomic force microscopy, it is shown that the xerogels are composed of aggregated particles with mean sizes of 35–45 nm. These results correlate with the data of scanning electron microscopy. On the basis of the data of IR spectroscopy and 13C CP/MAS NMR spectroscopy, it is concluded that the surface layers contain not only 3-mercaptopropyl and methyl groups but also silanol groups, a part of the unhydrolyzed alkoxy groups, and water molecules involved in the formation of hydrogen bonds. The results obtained by 29Si CP/MAS NMR spectroscopy testify that, in synthesized xerogels, the structural units of T1 type [(≡SiO)Si(OR′)2CH3 and/or (≡SiO)Si(OR′)2(CH2)3SH, R′ = H, OCH3 or OC2H5] are absent and the structural units of T3 type [(≡SiO)3SiCH3 and (≡SiO)3Si(CH2)3SH] dominate compared to the units of T2 type [(≡SiO)2Si(OR′)CH3 and (≡SiO)2Si(OR′)(CH2)3SH]. These results are an indirect indication of enhanced hydrolytic stability of surface layers in such xerogels.

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References

  1. Functional Hybrid Materials, Gomez-Romero, P. and Sanchez, C., Eds., Weinheim: Wiley-VCH, 2004.

    Google Scholar 

  2. Handbook of Sol-Gel Science and Technology: Processing, Characterization, and Applications, vols. 1–3, Sakka, S., Ed., Dordrecht: Kluwer, 2005.

    Google Scholar 

  3. Slinyakova, I.B. and Denisova, T.I., Kremniiorganicheskie adsorbenty. Poluchenie, sovistva, primenenie (Organosilicon Adsorbents: Synthesis, Properties, Applications), Kiev: Naukova Dumka, 1988.

    Google Scholar 

  4. Zub, Yu.L. and Parish, R.V., Stud. Surf. Sci. Catal., 1996, vol. 99, p. 285.

    Article  CAS  Google Scholar 

  5. Avnir, D., Klein, L.C., Levy, D., et al., in The Chemistry of Organic Silicon Compounds, Rappoport, Z. and Apeloig, Y., Eds., New York: Wiley, 1998, vol. 2, p. 2317.

    Chapter  Google Scholar 

  6. Voronkov, M.G., Vlasova, N.N., and Pozhidaev, Yu.N., Appl. Organomet. Chem., 2000, vol. 14, p. 287.

    Article  CAS  Google Scholar 

  7. El-Nahhal, I.M., Yang, J.J., Chuang, I.-S., and Maciel, G.E., J. Non-Cryst. Solids, 1996, vol. 208, p. 105.

    Article  CAS  Google Scholar 

  8. Yang, J.J., El-Nahhal, I.M., Chuang, I.-S., and Maciel, G.E., J. Non-Cryst. Solids, 1997, vol. 212, p. 281.

    Article  CAS  Google Scholar 

  9. Zub, Yu.L., Chuiko, A.A., and Stechenko, E.V., Dokl. Akad. Nauk Ukr., 2002, no. 4, p. 150.

  10. Melnyk (Seredyuk), I.V., Zub, Yu.L., Chuiko, A.A., and Van der Voort, P., Chem. Phys. Technol. Surf., 2002, vol. 8, p. 125.

    Google Scholar 

  11. Zub, Yu.L., Drozd, L.S., and Chuiko, A.A., Abstracts of Papers, IUPAC Symp. on Characterization of Porous Solids, Marseille, 1993, p. 95.

  12. Zub, Yu.L. and Chuiko, A.A., in Colloidal Silica: Fundamentals and Applications, Bergna, H.E., Eds., Washington, DC: Marcel Dekker, 2005, p. 397.

    Google Scholar 

  13. Dobryanskaya, G.I., Mel’nik, I.V., Zub, Yu.L., et al., Abstracts of Papers, X Vserossiiskii simpozium s uchastiem inostrannykh uchenykh “Aktual’nye problemy teorii adsorbtsii, poristosti i adsorbtsionnoi selektivnosti” (X All-Russia Symp. with Participation of Foreign Scientists “Current Problems of Theory of Adsorption, Porosity, and Adsorption Selectivity”), Moscow-Klyaz’ma, 2005, p. 54.

  14. Dobryanskaya, G.I., Mel’nik, I.V., Zub, Yu.L., et al., Zh. Fiz. Khim., 2006, vol. 80, no. 6.

  15. Brunauer, J.S., Emmett, P.H., and Teller, E., J. Am. Chem. Soc., 1938, vol. 60, p. 309.

    Article  CAS  Google Scholar 

  16. Barret, E.P., Joyner, L.G., and Halenda, P.P., J. Am. Chem. Soc., 1951, vol. 73, p. 373.

    Article  Google Scholar 

  17. Gregg, S. and Sing, K.S.W., Adsorption, Surface Area and Porosity, New York: Academic, 1982.

    Google Scholar 

  18. Corriu, R.J.P., Perz, R., and Reye, C., Tetrahedron, 1983, vol. 39, p. 999.

    Article  CAS  Google Scholar 

  19. Diaz, I., Mohino, F., Perez-Pariente, J., and Sastre, E., Thermochim. Acta, 2004, vol. 413, p. 201.

    Article  CAS  Google Scholar 

  20. Finn, L.P. and Slinyakova, I.B., Kolloidn. Zh., 1975, vol. 37, p. 723.

    CAS  Google Scholar 

  21. Lin-Vien, D., Colthup, N.B., Fateley, W.G., and Grasselli, J.G., in The Handbook of Infrared and Raman Characteristic Frequencies of Organic Molecules, London: Academic, 1991, p. 263.

    Google Scholar 

  22. Maciel, G.E., in Solid State NMR of Polymers, Ando, I. and Asakura, T., Eds., Amsterdam: Elsevier, 1998, p. 923.

    Google Scholar 

  23. Engelhardt, G. and Michel, D., High-Resolution Solid-State NMR of Silicates and Zeolites, Chichester: Wiley, 1987, p. 405.

    Google Scholar 

  24. Khatib, I.S. and Parish, R.V., J. Organomet. Chem., 1989, vol. 369, p. 9.

    Article  CAS  Google Scholar 

  25. Sing, K.S.W., Everett, D.H., Haul, R.A.W., et al., Pure Appl. Chem., 1985, vol. 57, p. 603.

    CAS  Google Scholar 

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Authors and Affiliations

  1. Institute of Surface Chemistry, National Academy of Sciences of Ukraine, ul. Generala Naumova 17, Kiev, 03164, Ukraine

    G. I. Dobryanskaya & Yu. L. Zub

  2. Faculty of Chemistry, Marie Curie-Sklodowska University, pl. M. Curie-Sklodowskiej 3, 20-131, Lublin, Poland

    M. Barczak & A. Dabrowski

Authors
  1. G. I. Dobryanskaya
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  2. Yu. L. Zub
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  3. M. Barczak
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  4. A. Dabrowski
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Original Russian Text © G.I. Dobryanskaya, Yu.L. Zub, M. Barczak, A. Dabrowski, 2006, published in Kolloidnyi Zhurnal, 2006, Vol. 68, No. 5, pp. 601–611.

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Dobryanskaya, G.I., Zub, Y.L., Barczak, M. et al. Synthesis and structure-related adsorption characteristics of bifunctional polysiloxane xerogels with methyl and 3-mercaptopropyl groups. Colloid J 68, 548–557 (2006). https://doi.org/10.1134/S1061933X06050048

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  • DOI: https://doi.org/10.1134/S1061933X06050048

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