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.
Similar content being viewed by others
References
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
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
Zhou T, Lucy CA (2008) Hydrophilic interaction chromatography of nucleotides and their pathway intermediates on titania. J Chromatogr A 1187:87–93
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
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
Ikeguchi Y, Nakamura H (2000) Selective enrichment of phosphlipids by titania. Anal Sci 16:541–543
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
Zhou T, Lucy CA (2010) Separation of carboxylates by hydrophilic interaction liquid chromatography on titania. J Chromatogr A 1217:82–88
Winkler J, Marmé S (2000) Titania as a sorbent in normal-phase liquid chromatography. J Chromatogr A 888:51–62
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
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
Davis SA, Mann S (2004) Spongelike macroporous TiO2 monoliths prepared from starch gel template. J Sol Gel Sci Technol 32:99–105
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
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
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
Randon J, Guerrin JF, Rocca JL (2008) Synthesis of titania monoliths for chromatographic separations. J Chromatogr A 1214:183–186
Hench LL, West JK (1990) The sol-gel process. Chem Rev 90:33–72
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
Yao B, Zhang L (1999) Preparation and characterization of mesoporous titania gel-monolith. J Mater Sci 34:5983–5987
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
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).
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
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
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10971-011-2410-2