Coagulating sedimentation and oxidation treatment of process water in iron ore flotation of Yuanjiacun iron mine had been studied. The process water of this mine carried residual polyacrylamide (PAM), poly(diallyldimethylammonium chloride) (PDADMAC), and Ca 2+ from the flotation and caused decrease of the iron flotation recovery or grade of the concentrate. The studies on highintensity magnetic separation (HIMS) tailings for coagulating sedimentation showed that the settling performance of coagulant (named CYH) was better than that of PDADMAC. The analyses of FTIR spectra and zeta potential demonstrated that CYH is adsorbed mainly through electrostatic attraction onto HIMS tailings. Sodium hypochlorite was adopted to oxidize the residual organics in tailings wastewater. When sodium hypochlorite is at the dosage of 1.0 g/L, reaction temperature is of 20 ∘ C, and reaction time is of 30 minutes, the removal rates of PAM, COD, and Ca 2+ were 90.48%, 83.97%, and 85.00%, respectively. Bench-scale flotation studies on the treated tailings wastewater indicated that the iron recovery and grade of concentrate were close to those of freshwater.