The invention provides a zinc and cobalt separation method. The zinc and cobalt separation method specifically includes the steps that 1, most metal in slag with high content of zinc and cobalt enters leaching solutions in a leaching mode, the leaching rate reaches 95% of above, and the metal recovery rate is high; 2, iron, copper and cadmium are removed in a combined mode, the purification process is simplified, the content of the iron, the copper and the cadmium in the solutions can be lowered to 5 mg / L or below, and the purification efficiency is high; 3, preliminary separation of the zinc and the cobalt is realized, the technology is simple, and the operation is easy; and 4, residual zinc is further removed, and complete separation of the zinc and the cobalt is realized. According to the method, the technology is simple, separation of the zinc and the cobalt is complete, the consumption is small, the production cost is low, and the recovery rate of the zinc and the cobalt in materials containing the zinc and the cobalt can reach 90% or above.