The TiO2 powder was prepared from the spent titanium chips by applying the sol-gel method with neutralization by NaOH solution. The prepared TiO2 powder was characterized using a particle size analysis, BET surface area, and XRD analysis. The crystal structure of the TiO2 powder was rutile type, and the powder was obtained to be nanosized. BET surface area of TiO2 powder was 118 m2/g, average particle size was 266.5 nm. The photocatalytic property of the TiO2 powder was evaluated as decomposition rate of methylene blue (MB) by using a liquid phase stirred reactor. Decomposition rate on TiO2 powder (P-25) was 1.5 times higher than that of the prepared TiO2 powder. Decomposition rate on the prepared TiO2 powder was linearly increased with increasing the amount of TiO2 powder, and approached to a specific value. MB concentration and decomposition rate was not correlated within the experimental range. The maximum value of decomposition rate at about pH 8 was 62%.