The porous TiO2 pellets were prepared based on pigment grade titaina, P25 titania powder and titanium(IV) butoxide. The characterization was done with X-Ray diffraction, scanning electron microscopy and BET measurements. The result shows that TiO2 pellets by using titanium(IV) butoxide with some addictive have the best surface porosity, with specific surface area of 196.9m2/g. For pigment grade titania and P25 titania powder, it is still effective to enhance the surface area after reassembling. The surface area increased from 11.6 to 29.2 m2/g for pigment grade titania and from 50 to 84.4 m2/g for P25 titania powder. Furthermore, it has been investigated on how to optimize and get the highest surface area by controlling the sintering temperature, reaction temperature, pH of solution, and the amount of alcohol and addictive of surfactant during preparation. The experimental photocatalytic degradation of acetone and toluene was performed using titania pellets made from P25 titania powder.