Abstract: Two kinds of wastewater generated in the decontamination of smelting titanium slag by hydrochloric acid and sulfuric acid washing respectively were utilized as raw materials, and composite flocculants were prepared at different pH values, polymerization durations of SiO₂ and recruitment amounts of Fe³⁺. The average turbidity removal rate of the polysilicate aluminum ferrite titanium flocculant (PSAFTC) on simulated turbid solution prepared at hydrochloric acid system with solution pH value of 3.0, SiO₂ polymerization time of 4 h at room temperature, FeCl₃-6H₂O incorporation of 50.0 g/L and NaClO₃ incorporation of 5.0 g/L was 95.62%. The average turbidity removal rate of the polysilicate aluminum ferrite titanium flocculant (PSAFTS) on simulated turbid solution was 96.99% when prepared at the conditions of sulfuric acid system, solution pH value of 1.30, Fe₂(SO₄)₃ addition of 50.0 g/L, and NaClO₃ addition of 5.0 g/L. The shelf life of the PSAFTC flocculant can reach 90 days, while that of the PSAFTS flocculant is only 7 days. However, the turbidity removal effect of the former is slightly lower than that of the latter. This paper focuses on preparation of flocculant agents from the wastewater generated from the decontamination of smelting titanium slag. The introduced method possesses significant economic and environmental benefits.