Recovery and separation of cobalt and manganese from one of zinc plant residues (ZPR), namely hot filter cake (HFC) using a hydrometallurgical process was studied. The process is carried out in four steps as follows: (1) washing zinc, (2) reductive leaching with hydrogen peroxide, (3) cadmium cementation with zinc powder and (4) separation of cobalt from manganese with beta naphthol. In this research, the separation between manganese and cobalt from the HFC using N-N reagent was investigated. The influence of several parameters on the course of the reaction such as N-N quantity, pH, temperature and reaction time was also examined. The optimum separation conditions were found to be N-N quantity: 8 times of stoichiometric value, time: 30 min, temperature: 25°C and pH = 1.5. Using the optimized conditions, the cobalt and manganese precipitation was nearly 99% and 0%, respectively. A kinetic study of manganese precipitation through N-N reagent has been carried out to assess the effect of kinetics parameters. The data obtained for the leaching kinetics indicated that the precipitation of manganese is an ash diffusion controlled reaction and the reaction activation energy is equal to 1.4kJ/mol.