The amounts of ethanol, HCl and H2O, and also calcination conditions during sol-gel process of preparing TiO2 photocatalyst were investigated. Methyl orange adsorption on TiO2 prepared using different sol compositions is not more than 4% by varying the amount of ethanol, HCl and H2O. The photocatalytic degradation is related to sol composition, and the optimal composition is composed of 10 ml ethanol, 1.0 ml H2O, and 0.1 ml HCl. Calcination temperature and time are also important in TiO2 preparation. The TiO2 particle prepared at 500 °C for 3 h has the optimal photocatalytic activity. In the irradiation time range up to 100 min, photocatalytic degradation rate constantly increases up to 94.2%.