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Template synthesis of mesoporous silicas containing phosphonic groups

  • Proceedings of the First All-Russian Conference “Sol-Gel Synthesis and Study of Inorganic Compounds, Hybrid Functional Materials, and Disperse Systems” (St. Petersburg, Russia, November 22–24, 2010)
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Abstract

Mesoporous silicas containing the functional group ≡Si(CH2)2P(O)(OC2H5)2 in the surface layer have been obtained using the template method (template—P123). Their treatment by a concentrated hydrochloric acid results in the formation of functional groups of the composition ≡Si(CH2)2P(O)(OH)2 that is in agreement with the IR spectroscopy data. It has been shown that the above treatment causes an increase of the sample specific surface area (up to 605 m2/g), sorption capacity, and pore diameter. As established by means of the CP/MAS NMR spectroscopy on 31P nuclei, the sample drying in vacuum at 110°C results in the formation of fragments ≡Si(CH2)2P(O)(OH)—OSi≡ with the content of 10–15 wt %. However, according to the TEM data, the sample mesoporous structure is retained.

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References

  1. Marhol, M., Beranova, H., and Cheng, K., Selective Ion-Exchangers Containing Phosphorus in Their Functional Groups, J. Radioanal. Chem., 1974, vol. 21, pp. 177–186.

    Article  CAS  Google Scholar 

  2. Sinyavskaya, E.I., Tsimbal, L.V., and Bogatyrev, V.M., Preparation and Complexing Properties of Phosphoryl-Containing Ligands Grafted Onto Silica Surface, Adsorbts. Adsorbenty, 1984, no. 12, p. 51–55.

  3. Fryxell, G.E., Wu, H., Lin, Y., Shaw, W.J., Birnbaum, J.C., Linehan, J.C., Nie, Z., Kemner, K.M., and Kelly, S., Lanthanide Selective Sorbents: Self-Assembled Monolayers on Mesoporous Supports (SAMMS), J. Mater. Chem., 2004, vol. 14, no. 22, pp. 3356–3363.

    Article  CAS  Google Scholar 

  4. Grinenko, S.B., Belousov, V.M., Noskov, A.M., Lysova, N.N., Bugerenko, E.F., and Chernyshev, E.A., Synthesis and Study of Siliceous Carriers for Catalysts with Surface Amine and Phosphoryl Groups, Ukr. Khim. Zh., 1983, vol. 49, no. 2, pp. 136–140.

    CAS  Google Scholar 

  5. Lisichkin, G.V., Kudryavtsev, G.V., Serdan, A.A., Staroverov, S.M., and Yuffa, A.Ya., Modifitsirovannye kremnezemy v sorbtsii, katalize i khromatografii (Modified Silicas in Sorption, Catalysis and Chromatography), Moscow: Khimiya, 1996 [in Russian].

    Google Scholar 

  6. Collinson, M.M., Analytical Applications of Organically Modified Silicates, Microchim. Acta, 1998, vol. 129, nos. 3–4, pp. 149–165.

    Article  CAS  Google Scholar 

  7. Kholin, Yu.V., Zaitsev, V.N., Zaitseva, G.N., and Mernyi, S.A., Complexing in Interfacial Layers of Silicas with Immobilised Aminophosphonic and Aminodiphosphonic Acids, Russ. J. Inorg. Chem., 1995, vol. 40. no 2. pp. 261–269.

    Google Scholar 

  8. Khimiya privitykh poverkhnostnykh soedinenii (Chemistry of Grafted Surface Compounds), Lisichkin, G.V., Ed., Moscow: Fizmatlit, 2003.

    Google Scholar 

  9. Zub, Yu.L., Synthesis of Functionalized Mesoporous Silicas, Structure of Their Layer and Sorption Properties, in Nanomaterials and Supramolecular Structures: Physics, Chemistry, and Applications, Shpak, A.P. and Gorbyk, P.P., Eds., Berlin: Springer, 2009, pp. 179–196.

    Chapter  Google Scholar 

  10. Fowler, S., Burkett, S.L., and Mann, S., Synthesis and Characterization of Ordered Organo-Silica-Surfactant Mesophases with Functionalized MCM-41-Type Architecture, Chem. Commun. (Cambridge), 1997, vol. 2, no. 18, pp. 1769–1770.

    Article  Google Scholar 

  11. Kresge, C.T., Leonowicz, M.E., and Roth, W.J., and All. Ordered Mesoporous Molecular Sieves Synthesized by a Liquid-Crystal Template Mechanism, Nature (London), 1992, vol. 359, pp. 710–712.

    Article  CAS  Google Scholar 

  12. Raman, N.K., Anderson, M.T., and Brinker, C.J., Template-Based Approaches to the Preparation of Amorphous, Nanoporous Silicas, Chem. Mater., 1996, vol. 8, no. 8, pp. 1682–1701.

    Article  CAS  Google Scholar 

  13. Mel’nyk (Seredyuk), I.V., Zub, Yu.L., Chuiko, A.A., Jaroniec, M., and Mann, S., Polyfunctionalized Silica Adsorbents Obtained by Using Dodecylamine as Template, in Nanoporous Materials III, A. Sayari, A. and Jaroniec, M., Eds., Amsterdam: Elsevier, 2002, vol. 141, pp. 205–212.

    Google Scholar 

  14. Dudarko, O.A., Melnyk, I.V., Zub, Yu.L., and Dabrowski, A., Structure-Adsorptive Characteristics of Template-Based Mesoporous Silicas Containing Residues of Some Phosphorus Acids Derivatives in Their Surface Layer, Stud. Surf. Sci. Catal., 2007, vol. 160, pp. 479–486.

    Article  CAS  Google Scholar 

  15. Yaroshenko, N.A. and Il’in, V.G., Solubilization Compositions for Template Synthesis of Mesoporous Sorbents, Russ. J. Appl. Chem., 2004, vol. 77, no. 11, pp. 1769–1776.

    Article  CAS  Google Scholar 

  16. Zhao, D., Huo, Q., Feng, J., Chmelka, B.F., and Stucky, G.D., Nonionic Triblock and Star Diblock Copolymer and Oligomeric Surfactant Syntheses of Highly Ordered, Hydrothermally Stable, Mesoporous Silica Structures, J. Am. Chem. Soc., 1998, vol. 120, no. 24, pp. 6024–6036.

    Article  CAS  Google Scholar 

  17. Brunauer, J.S., Emmet, P.H., and Teller, E., Adsorption of Gases in Multimolecular Layers, J. Am. Chem. Soc., 1938, vol. 60, no. 2, pp. 309–319.

    Article  CAS  Google Scholar 

  18. Barrett, E.P., Joyner, L., and Halenda, P.P., The Determination of Pore Volume and Area Distributions in Porous Substances. I. Computations from Nitrogen Isotherms, J. Am. Chem. Soc., 1951, vol. 73, no. 1, pp. 373–380.

    Article  CAS  Google Scholar 

  19. Nguyen, C. and Do, D.D., New Method for the Characterization of Porous Materials, Langmuir, 1999, vol. 15, no. 10, pp. 3608–3615.

    Article  CAS  Google Scholar 

  20. Gun’ko, V.M. and Do, D.D., Characterization of Pore Structure of Carbon Adsorbents Using Regularization Procedure, Colloids Surf., A, 2001, vol. 193, nos. 1–3, pp. 71–83.

    Article  Google Scholar 

  21. Do, H.D., Characterization of Micro-Mesoporous Carbon Media, Colloids Surf., A, 2001, vols. 187–188, nos. 1–3, pp. 51–71.

    Article  Google Scholar 

  22. Yang Qihua, Yang Jie, Liu Jian, Li Ying, and Li Can, Synthesis and Characterization of Phosphonic Acid Functionalized Organosilicas with Bimodal Nanostructure, Chem. Mater., 2005, vol. 17, no. 11, pp. 3019–3024.

    Article  CAS  Google Scholar 

  23. Aliev, A., Ou, D.L., Ormsby, B., and Sullivan, A.C., Porous Silica and Polysilsesquioxane with Covalently Linked Phosphonates and Phophonic Acids, J. Mater. Chem., 2000, vol. 10, no. 12, pp. 2758–2764.

    Article  CAS  Google Scholar 

  24. Dabrowski, A., Barchak, M., Dudarko, O.A., and Zub, Yu.L., Preparation and Characterization of Polysiloxane Xerogels Having Covalently Attached Phosphonic Acids Groups, Pol. Chem. J., 2007, vol. 81, no. 4, 475-483.

  25. Mercier, L. and Pinnavaia, T.J., Direct Synthesis of Hybrid Organic-Inorganic Nanoporous Silica by a Neutral Amine Assembly Route: Structure-Function Control by Stoichiometric Incorporation of Organosiloxane Molecules, Chem. Mater., 2000, vol. 12, no. 1, pp. 188–196.

    Article  CAS  Google Scholar 

  26. Slinyakova, I.B. and Denisova, T.I., Kremniiorganicheskie adsorbenty: Poluchenie, svoistva, primenenie (Organo-Silicon Adsorbents: Preparation, Properties, Application), Kiev: Naukova Dumka, 1988 [in Russian].

    Google Scholar 

  27. Dudarko, O.A., Mel’nik, I.V., Zub, Yu.L., Chuiko, A.A., and Dabrowski, A., Synthesis of Polysiloxane Xerogels Using Tetraethoxysilane/(Diethylphosphatoethyl)triethoxysilane System, Colloid J., 2005, vol. 67, no. 6, pp. 683–687.

    Article  CAS  Google Scholar 

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

    Google Scholar 

  29. Schrotter, J.C., Cardenas, A., Smaihi, M., and Hovnanian, N., Silicon and Phosphorus Alkoxide Mixture: Sol-Gel Study by Spectroscopic Technics, J. Sol-Gel Sci. Technol., 1995, vol. 4, no. 1, pp. 195–204.

    Article  CAS  Google Scholar 

  30. Rouquerol, F., Rouquerol, J., and Sing, K., Adsorption by Powders and Porous Solids: Principles, Methodology and Application, London: Academic, 1999.

    Google Scholar 

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Correspondence to O. A. Dudarko.

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Original Russian Text © O.A. Dudarko, Yu.L. Zub, M. Barczak, A. Dabrowski, 2011, published in Fizika i Khimiya Stekla.

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Dudarko, O.A., Zub, Y.L., Barczak, M. et al. Template synthesis of mesoporous silicas containing phosphonic groups. Glass Phys Chem 37, 596–602 (2011). https://doi.org/10.1134/S1087659611060083

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