A new process of oxidation precipitation was developed to separate cobalt from dilute zinc-bearing deironing solution with sodium persulfate as oxidant.The effects of parameters on oxidative precipitation rate of metals were investigated.The results show that after acid washing cobalt content in residue is 15.6% which is nearly 9times to that in existing residue under the optimum conditions including dosage of sodium persulfate of 4times of theoretical cobalt consumptions,temperature of 80 ℃,pH of 4.8~5.0,and oxidation time of 3h.Post-precipitation solution containing exclusively zinc can be neutralized by sodium carbonate to precipitate basic zinc carbonate product with zinc content of 51.78%.