Heterogeneous Fenton catalyst Fe 2 (MoO 4 ) 3 was prepared and the process efficiency was evaluated for oxidation of water-based Cyan flexo dye in synthetic aqueous solution and printing wastewater. The removal process of printing dye was analyzed by UV/VIS spectrophotometry, while dye mineralization was evaluated by the determination of total organic carbon content and chemical oxygen demand. Four determinants of the heterogeneous Fenton system, including initial dye concentration, iron concentration, pH and hydrogen peroxide concentration were investigated. Statistical method, definitive screening design was applied to generate optimal operational conditions of the four variables, which maximizes the process of dye removal. The initial dye concentration of 20 mgL -1 , catalyst dosage of 0.75 mgL -1 , pH of 2 and H 2 O 2 concentration of 11 mM were chosen as the best operational conditions, contributing to 82% of the process efficiency. The Fenton process efficiency of 79% was achieved within the treatment of printing wastewater under optimal conditions for a 90 minute reaction time. The maximum COD removal efficiency was 61.1%, while 67% mineralization was achieved. The obtained results confirmed synergistic effect of Fe 3+ and MoO 4 2− which contributed to high catalytic activity and high heterogeneous Fenton efficiency.