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The separation of iron from zinc is a difficult problem faced by the zinc smetlting industry using high iron-bearing zinc ores.This paper proposed a kind of pyro-hydrometallurgy process for the solving of this problem.Firstly, the zinc calcine was selectively reduced into magnetite and zinc oxide, then the ammonia leaching was carried out to extract zinc from roasted product.And the iron was perserved in leaching residues in the form of magentite and recovered by magnetic separation.The optimal conditions were as follows: temperature, 30C; reaction duration, 1 h; solid-to-liquid ratio, 1/7; stirring speed, 200rpm.Under these conditions, extraction of zinc and iron were 88.56％ and 4.20％ respectively.The recovery and grade of iron in concentration of magnetic separation were 86.46％ and 46.5％ respectively.