The objective of this study is to optimize the leaching conditions of sequential leaching and extracting processes for selective Ni recovery from spent Ni-Mo-based catalyst. The selective Ni recovery process consists of two processes of leaching and extracting process. In this 2-step process, Ni component is dissolved from solid spent Ni-Mo-based catalyst into leaching agent in leaching process and sequentially extracted to Ni complex with an extracting agent in the extracting process. The solutions of nitric acid (), ammonium carbonate () and sodium carbonate () were used as a leaching agent in leaching process and oxalic acid was used as an extracting agent in extracting process. solution is the most efficient leaching agent among the various leaching agent. Also, the optimized leaching conditions for the efficient and selective Ni recovery were the leaching temperature of concentration of 6.25 vol% and elapsed time of 3 h. As a result, Nickel oxalate having the highest yield of 88.7% and purity of 100% was obtained after sequentially leaching and extracting processes under the optimized leaching conditions.