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

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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.

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References

  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 18:5326–5335

    Article  CAS  Google Scholar 

  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 1216:7375–7383

    Article  CAS  Google Scholar 

  3. Zhou T, Lucy CA (2008) Hydrophilic interaction chromatography of nucleotides and their pathway intermediates on titania. J Chromatogr A 1187:87–93

    Article  CAS  Google Scholar 

  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 350:292–297

    Article  CAS  Google Scholar 

  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 1165:128–135

    Article  CAS  Google Scholar 

  6. Ikeguchi Y, Nakamura H (2000) Selective enrichment of phosphlipids by titania. Anal Sci 16:541–543

    Article  CAS  Google Scholar 

  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 394:1453–1461

    Article  CAS  Google Scholar 

  8. Zhou T, Lucy CA (2010) Separation of carboxylates by hydrophilic interaction liquid chromatography on titania. J Chromatogr A 1217:82–88

    Article  CAS  Google Scholar 

  9. Winkler J, Marmé S (2000) Titania as a sorbent in normal-phase liquid chromatography. J Chromatogr A 888:51–62

    Article  CAS  Google Scholar 

  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 18:864–866

    Article  CAS  Google Scholar 

  11. Shi ZG, Xu LY, Feng YQ (2006) A new template for the synthesis of porous inorganic oxide monoliths. J Non Cryst Solids 352:4003–4007

    Article  CAS  Google Scholar 

  12. Davis SA, Mann S (2004) Spongelike macroporous TiO2 monoliths prepared from starch gel template. J Sol Gel Sci Technol 32:99–105

    Article  Google Scholar 

  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 28:115–119

    Article  CAS  Google Scholar 

  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 18:6069–6074

    Article  CAS  Google Scholar 

  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 3:176–180

    Article  CAS  Google Scholar 

  16. Randon J, Guerrin JF, Rocca JL (2008) Synthesis of titania monoliths for chromatographic separations. J Chromatogr A 1214:183–186

    Article  CAS  Google Scholar 

  17. Hench LL, West JK (1990) The sol-gel process. Chem Rev 90:33–72

    Article  CAS  Google Scholar 

  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 146:69–73

    Article  Google Scholar 

  19. Yao B, Zhang L (1999) Preparation and characterization of mesoporous titania gel-monolith. J Mater Sci 34:5983–5987

    Article  CAS  Google Scholar 

  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 37:147–151

    Google Scholar 

Download references

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).

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Correspondence to Zi-Tao Jiang.

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Zhao, J., Jiang, ZT., Tan, J. et al. Sol–gel synthesis and characterization of titania monolith with bimodal porosity. J Sol-Gel Sci Technol 58, 436–441 (2011). https://doi.org/10.1007/s10971-011-2410-2

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  • DOI: https://doi.org/10.1007/s10971-011-2410-2

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