Pretreatment of activated sludge with sulfuric acid and bioleaching using Acidithiobacillus ferrooxidans along with addition of Fe2+ on sludge dewaterability was investigated. The sludge dewatering efficiency in terms of capillary suction time (CST) and specific resistant to filtration (SRF) was increased with a decrease in sludge pH. A pH of 2.67 was found to be optimum for dewatering, at which 81% and 63% reduction of CST and SRF were achieved, respectively. The dewaterability of sludge was enhanced after the addition of Fe2+ and A. ferrooxidans. Ideal concentration of Fe2+ was 2 g/L for sludge dewaterability, which showed 96% and 88% reduction in CST and SRF, respectively. In the control sludge, maximum part of the biopolymeric macromolecules was contributing by the tightly bound extracellular polymeric substances (TB-EPS). At optimum Fe2+ concentration, total EPS was reduced by 73%, enhancing sludge dewaterability. Bioleaching conducted by A. ferrooxidans could solubilized 88% Cu and 99% Zn within 120 h.