A spinning disc photoreactor using immobilized TiO2 on a stainless steel disc is employed to study the degradation of phenol in aqueous solutions. The characterizations of the immobilized TiO2 film are carried out by scanning electron microscopy, field emission scanning electron microscopy, X-ray diffraction, Brunauer-Emmett-Teller analysis, and tensile adhesion test. The Box-Behnken design method is employed to identify the effects of three key operational parameters. The maximum predicted nanophoto-catalytic degradation percent of phenol was 100% at the optimum processing condition (rotational speed, 290 rpm; flow rate, 2000 mL/min; and disc diameter, 22 cm). For a description of the flow pattern, the residence time distribution analysis is performed. By using a tanks-in-series model the equivalent number of continuous stirred tanks reactors at the obtained optimum condition was four. Hydrodynamic and kinetic models were combined to predict the degradation of phenol. Good agreement between the experimental and predicted results is shown.