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The recovery of nickel from molybdenum leach residue by the process of segregation roasting-sulfuric acid leaching-solvent extraction was investigated.The residue was characterized by microscopic investigations,using X-ray fluorescence spectrometry (XRF) and X-ray diffractometry (XRD) techniques and the residue after segregation roasting was characterized by chemical phase analysis method.A series of experiments were conducted to examine the mass ratio of activated carbon (AC) to the residue,segregation roasting time and temperature,sulfuric acid concentration,liquid-to-solid ratio,leaching time,leaching temperature,addition amount of 30％ H2O2,stirring speed (a constant) on the leaching efficiency of nickel.A maximum nickel leaching efficiency of 90.5％ is achieved with the mass ratio of AC to the residue of 1:2.5,segregation roasting time of 2 h,segregation roasting temperature of 850 ℃,sulfuric acid concentration of 4.5 mol/L,liquid-to-solid ratio of 6∶1,leaching time of 5 h,leaching temperature of 80 ℃,addition of 30％ H2O2 of 0.6 mL for 1 g dry residue.Under these optimized conditions,the average leaching efficiency of nickel is 89.3％.The nickel extraction efficiency in the examined conditions is about 99.6％,and the nickel stripping efficiency in the examined conditions is about 99,2％.