Super/subcritical fluid extractions for preparation of the crystalline titania

Various extraction techniques which use fluids in super/subcritical state (CO₂, H₂O, CH₃OH) were used for the preparation of crystalline TiO₂ from surfactant-mediated titania organogels (the amorphous reaction intermediate products of surfactant-mediated sol-gel synthesis). Crystallinity, purity and texture of TiO₂ powders (titania aerogels) were studied in detail for different treatment modes of titania organogels. Suitable combinations of extraction solvents and extraction temperature and pressure were considered for synthesis of TiO₂ powder crystalline phase (anatase) with high specific surface area and purity (carbon content < 0.1 wt.%). Optimum results were achieved by combined extraction procedures—subcritical water extraction and supercritical fluid extraction or pressurised liquid extraction. Moreover, the possible tuning of the TiO₂ powder pore-size distribution by regulation of temperature at constant pressure for the combined subcritical water extraction and pressurised liquid extraction was found.