In this research, we tried to find a solution for problem of urban sewage treatment with coal fly ash and gypsum as industrial wastes. Furthermore, we examine the feasibility of reusing coal fly ash and gypsum which increasing amount of industrial wastes as urban sewage treatment materials and the concern for urban sewage coagulation and adsorption mechanism. The result shows that when 800 mg/L of coal fly ash sintered at 700oC are injected into urban sewage, optimum removal efficiency of CODCr is 87.3%, indicating more 5% improvement than of treating with not sintered condition. The study finds that when 1000 mg/L of gypsum are injected into urban sewage without sintering, optimum removal efficiency of CODCr and turbidity indicate 87.4% and 93.7% respectively.