Recyclable aggregates of mesoporous titania with different anatase-rutile ratios have been prepared by thermal treatments of either amorphous or peptized precursors. These last two have been obtained by hydrolysis of either Ti(OC₂H₅)₄ or of Ti(OC₂H₅)₄ in mixture with 5 mol % Zr(OC₃H₇)₄ at room temperature in the presence of NH₄OH as a catalyzing agent. The anatase-rutile ratio, the recyclable aggregates of the nano-sized particles, the mesoporosity, the surface area and the crystallinity of the resulting crystallized products of titania can be controlled by the synthesis parameters including: concentration of ammonia catalyst, stirring time and concentration of the peptizing HNO₃, drying method of peptized precursors, calcination temperature, and finally the ramp rate up to the titania crystallization temperature. A broad range of synthesis parameters control the crystal sizes of titania particles produced. This allows catalyst preparation with very different crystal size, surface area, anatase to rutile crystal ratio and various mesoporous structures. Drying by lyophilization of precursors reduce the aggregation of the primary particles giving micro-/macroporous structures.
Keywords: amorphous and peptized precursors; drying effect; mesoporous titania; micrometer aggregates; peptizing HNO3; thermal crystallization.