Advertisement

Journal of Sol-Gel Science and Technology

, Volume 58, Issue 2, pp 436–441 | Cite as

Sol–gel synthesis and characterization of titania monolith with bimodal porosity

  • Jing Zhao
  • Zi-Tao Jiang
  • Jin Tan
  • Rong Li
Original Paper

Abstract

Monolithic titania materials with macro-mesoporosity bimodal texture have been prepared through a template-free sol–gel approach, based on the reaction of hydrolysis and polycondensation of titanium isopropoxide promoted by the slow released water from esterification between acetic acid and methanol under a strong acidic condition. With the coarsening of the titania oligomers, phase separation and sol–gel transition processes take place so as to form a homogeneous gel system that will change into a monolith after aging, drying and heat treatment. The synthesized titania monolith possesses a specific surface area of 77 m2 g−1 (calcined at 350 °C), an anatase with partly rutile crystallite structure and great mechanical strength. The synthesis method applied here is simple and easy to implement as no extra chemical modifier such as poly(ethylene oxide) (PEO) and formamide is needed to control the process. The properties of biomodal porous structure, satisfactory surface area and high mechanical strength will enable the monolith to be served as a chromatography column to separate phosphorus organo-compounds.

Keywords

Titania Monolith Sol–gel synthesis Mesoporous Macroporous 

Notes

Acknowledgments

This work was supported by the National Natural Science Foundation of China (Grant No. 20875069) and the Science Foundation for Young Teachers of Tianjin University of Commerce (Grant No. 090107).

References

  1. 1.
    Chen Y, Yi Y, Brennan JD, Brook MA (2006) Development of macroporous titania monoliths using a biocompatible method. Part 1: material fabrication and characterization. Chem Mater 18:5326–5335CrossRefGoogle Scholar
  2. 2.
    Konishi J, Fujita K, Nakanishi K, Hirao K, Morisato K, Miyazaki S, Ohira M (2009) Sol-gel synthesis of macro-mesoporous titania monoliths and their applications to chromatographic separation media for organophosphate compounds. J Chromatogr A 1216:7375–7383CrossRefGoogle Scholar
  3. 3.
    Zhou T, Lucy CA (2008) Hydrophilic interaction chromatography of nucleotides and their pathway intermediates on titania. J Chromatogr A 1187:87–93CrossRefGoogle Scholar
  4. 4.
    Hata K, Morisaka H, Hara K, Mima J, Yumoto N, Tatsu Y, Furuno M, Ishizuka N, Ueda M (2006) Two-dimensional HPLC on-line analysis of phosphopeptides using titania and monolithic columns. Anal Biochem 350:292–297CrossRefGoogle Scholar
  5. 5.
    Hsieh HC, Sheu C, Shi FK, Li DT (2007) Development of a titanium dioxide nanoparticle pipette-tip for the selective enrichment of phosphorylated peptides. J Chromatogr A 1165:128–135CrossRefGoogle Scholar
  6. 6.
    Ikeguchi Y, Nakamura H (2000) Selective enrichment of phosphlipids by titania. Anal Sci 16:541–543CrossRefGoogle Scholar
  7. 7.
    Calvano CD, Jensen ON, Zambonin CG (2009) Selective extraction of phospholipids from dairy products by micro-solid phase extraction based on titanium dioxide microcolumns followed by MALDI-TOF-MS analysis. Anal Bioanal Chem 394:1453–1461CrossRefGoogle Scholar
  8. 8.
    Zhou T, Lucy CA (2010) Separation of carboxylates by hydrophilic interaction liquid chromatography on titania. J Chromatogr A 1217:82–88CrossRefGoogle Scholar
  9. 9.
    Winkler J, Marmé S (2000) Titania as a sorbent in normal-phase liquid chromatography. J Chromatogr A 888:51–62CrossRefGoogle Scholar
  10. 10.
    Konishi J, Fujita K, Nakanishi K, Hirao K (2006) Phase-separation-induced titania monoliths with well-defined macropores and mesostructured framework from colloid-derived sol-gel systems. Chem Mater 18:864–866CrossRefGoogle Scholar
  11. 11.
    Shi ZG, Xu LY, Feng YQ (2006) A new template for the synthesis of porous inorganic oxide monoliths. J Non Cryst Solids 352:4003–4007CrossRefGoogle Scholar
  12. 12.
    Davis SA, Mann S (2004) Spongelike macroporous TiO2 monoliths prepared from starch gel template. J Sol Gel Sci Technol 32:99–105CrossRefGoogle Scholar
  13. 13.
    Backlund S, Smatt JH, Rosenholm JB, Lindén M (2007) Template-free sol-gel synthesis of hierarchically macro-and mesoporous monolithic TiO2. J Disper Sci Technol 28:115–119CrossRefGoogle Scholar
  14. 14.
    Konishi J, Fujita K, Nakanishi K, Hirao K (2006) Monolithic TiO2 with controlled multiscale porosity via a template-free sol-gel process accompanied by phase separation. Chem Mater 18:6069–6074CrossRefGoogle Scholar
  15. 15.
    Huang D, Luo GS, Yang LM, Wang YJ (2005) Synthesis of masoporous TiO2 materials with high specific area using inorganic acids as catalysts. China Particuol 3:176–180CrossRefGoogle Scholar
  16. 16.
    Randon J, Guerrin JF, Rocca JL (2008) Synthesis of titania monoliths for chromatographic separations. J Chromatogr A 1214:183–186CrossRefGoogle Scholar
  17. 17.
    Hench LL, West JK (1990) The sol-gel process. Chem Rev 90:33–72CrossRefGoogle Scholar
  18. 18.
    Mir L, Amlouka A, Elaloui E, Saadoun M, Pierre AC (2008) Preparation and optical characterization of transparent, microporous TiO2 xerogel monoliths. Mater Sci Eng B 146:69–73CrossRefGoogle Scholar
  19. 19.
    Yao B, Zhang L (1999) Preparation and characterization of mesoporous titania gel-monolith. J Mater Sci 34:5983–5987CrossRefGoogle Scholar
  20. 20.
    Yang H, Shen QH, Gao JW (2008) Preparation of TiO2 sol containing anatase-rutile mischcrystal grains and its photocatalytic activity. Rare Metal Mater Eng 37:147–151Google Scholar

Copyright information

© Springer Science+Business Media, LLC 2011

Authors and Affiliations

  1. 1.Tianjin Key Laboratory of Food Biotechnology, College of Biotechnology and Food ScienceTianjin University of CommerceTianjinPeople’s Republic of China

Personalised recommendations