Tailings from the abandoned Tiouit mine site in Morocco are mainly composed of sulfides, hematite, and quartz. They contain 0.06–1.50 wt % sulfur, mostly in the form of pyrite, pyrrhotite, and chalcopyrite. The tailings also contain gold (3.36–5.00 ppm), silver (24–37 ppm), and copper (0.06–0.08 wt %). Flotation tests were conducted to reprocess the tailings for Au, Ag, and Cu recovery, and at the same time to prevent acid mine drainage (AMD) generation through the oxidation of sulfide minerals, including pyrite, sphalerite, arsenopyrite, chalcopyrite, galena. The flotation results confirmed that environmental desulfurization is effective at reducing the overall sulfide content in the tailings. The recovery of sulfides was between 69% and 75%, while Au recovery weight-yield was between 2.8% and 4.7%. The test that showed the best sulfur recovery rate and weight-yield was carried out with 100 g/t CuSO4 (sulfide activator) and 50 g/t of amyl xanthate (collector). The goal of this study was also to assess the remaining acid-generating potential (AP) and acid-neutralizing potential (NP) of the desulfurized tailing. The geochemical behavior of the initial tailings sample was compared to that of the desulfurized tailings using kinetic weathering cell tests. The leachates from the desulfurized tailings showed higher pH values than those from the initial tailings, which were clearly acid-generating. The residual acidity produced by the desulfurized tailings was most likely caused by the hydrolysis of Fe-oxyhydroxides.