Application of two-step flotation for removing dioxins and heavy metals from hospital solid waste incinerator (HSWI) fly ash was studied. In the first step, decarburization flotation was executed to remove dioxins from raw fly ash. The second step of precipitation flotation was carried out to recycle the toxic metals in the residual slurry. Finally, an acid leaching-sulphide precipitation-flotation method was proposed. The results showed that carbon removal rate was 90.7%, and the dioxin removal percentage was 91.0% during decarburization flotation. And Zn, Pb and Cu in residual slurry were acid-leached with the removal efficiencies being 91.3%, 79.2% and 85.6%, respectively. The optimum sulphidation condition of heavy metals in the residual slurry were Na2S molar ratio of 1.4 and sulphidation time of 30 min. Subsequently, precipitation flotation could recover 49.9% of Zn, 42.0% of Pb and 48.7% of Cu from the raw fly ash. After the two-step flotation, the toxicity of the tailings reduced considerably, and the tailings could be disposed in landfill. Therefore, this two-step flotation treatment of HSWI fly ash may result in both detoxiﬁcation and potential resource recovery.