The process of solvent extraction was applied to separate and recover Cu2+ and Ni2+ from plating wastewater from copper and nickel alloy plating process, because there are abundant Cu2+ and Ni2+. And the influence parameters have been investigated. Lix984 was chosen as the extractant due to it has good performance to extract metals from the water. The results showed the separation of Cu2+ and Ni2+ from sulphate medium can be realized by adjusting pH value with the help of Lix984, And more, the optimal pH values for extracting Cu2+and Ni2+ are 4 and 10, respectively. The maximal extraction efficiency for Cu2+ and Ni2+ can reach above to 90.6% and 93.5% by single-stage extraction. The recovered Cu2+ and Ni2+ were stripped in 170g/L and 200g/L H2SO4 medium, respectively. And the stripping of Cu2+ and Ni2+ are >99.2% and >99.4%, respectively. It can be successfully applied to the field of plating wastewater, decreasing the environment pollution from Cu2+ and Ni2+ and providing a kind of new copper and nickel resource.