Titanium dioxide shows outstanding chemical stability, high refractive index photochemical activity and high dielectric constant, which are expected to play important roles in many fields. In recent years, there has been increasing interest in the application of TiO2 nanoparticles for pigments,catalysts and supports, ceramics, gas sensors, inorganic membranes,waste water purification and solar energy conversion. The uses and performances for a given application are, however, strongly influenced by the crystalline structure, the morphology and the size of the particles. Therefore, in this book development of synthetic methods of the production of TiO2 nanoparticles in which the particle size and the crystal structure of the products are being controlled are precisely describe.Different characterization techniques (SEM, EDS and UV-Vis Spectroscopy)are also displayed. The photocatalytic degradation kinetics was studied with these synthesized TiO2 on methylene blue (MB) and congo red (CR).The effect of pH on the photocatalytic degradation was also investigated. The TiO2 showed enhanced photocatalytic performance in presence of basic media than that of neutral or acidic.