Synthesis, characterization and photocatalytic activity of TiO2 powders prepared under different gelling and pressure conditions

Homogeneous TiO2 gel powders were prepared by hydrolysis and condensation of titanium(IV) isopropoxide with HCl or SnCl2 catalysts, by working under reduced pressure or in air. Ti(IV) alkoxide was previously modified by reaction with formic or acetic acid, used as chelating ligands, when gelation was performed in acidic catalysis. Crude TiO2 xerogels were purified by water reflux treatment in order to induce a low temperature crystallisation to the anatase phase. Both crude and purified TiO2 samples were characterised by XRD, FT-IR, SEM, and N-2 adsorption analysis. Thermoanalyses (TG, DTA, DTG, TG-MS, TG-GC-MS) were carried out to quantify the residual organic components in the crude TiO2 gels and to obtain stoichiometric formulas to describe their chemical compositions. XRD data of purified TiO2 powders were processed by means of a Rietveld refinement procedure to determine TiO2 polymorphs, crystallite sizes and cell parameters, before their use in photocatalytic tests. The photoactivity of the purified TiO2 anatase powders was studied by using 4-nitrophenol degradation as "probe" reaction carried out in a batch and/or a membrane photoreactor. Samples prepared by using formic acid or SnCl, were the most photoactive, whereas specimens gelled under vacuum treatment showed detrimental effects.