Methylene blue (MB) dye waste is organic pollutant from the chemical industry. The parameters of the MB dye content that are permitted in the form of methylene blue active substance (MBAS) do not exceed 200 μg/L. The MB dye waste treatment system can be carried out through the adsorption process using TiO2 nanoparticles. This study aims to synthesize TiO2 nanoparticles using PVA as surfactant and titanium tetraisopropoxide (TTIP) as precursors through a sol-gel process followed by a hydrothermal process at 400 and 600oC calcination temperatures. The results of the XRD spectrum characteristics show tetragonal crystal shape, anatase phase, and particle size around 1.66-3.15 nm. IR (infrared) spectroscopy proves the existence of Ti-O group bonds in the spectrum of 467 cm-1 and the presence of hydroxyl groups on the surface of TiO2. DSC analysis shows the thermal stability of TiO2 at 250oC. The application of TiO2 nanoparticles as MB adsorbents was carried out through photodegradation using 150 watt Hg lamps for 60 minutes. The largest adsorption capacity was obtained from the calcined TiO2 samples at 600oC at 217 mg/g and 81% adsorption capacity. The adsorption process of MB by TiO2 nanoparticles follow the equation of Langmuir and Freundlich isotherms with the coefficient of determination, R2 close to the value of 1