The invention relates to a zinc and iron separation method in the zinc hydrometallurgy process and belongs to the technical field of hydrometallurgy. Firstly, zinc concentrate is subjected to low-temperature roasting to obtain zinc calcine; then the zinc calcine, zinc hydrometallurgy electrolysis post-liquid and produced weak acid fluid are subjected to neutral leaching, and neutral leachate containing 20 mg/L or less of iron and neutral leached residues are produced; the obtained neutral leached residues and indium and copper extraction post-liquid are mixed to be subjected to weak-acid leaching, and weak acid fluid containing 1 g/L or less of iron and weak acid residues are produced; the obtained weak acid residues are subjected to the silver flotation process, and silver concentrate and zinc and iron slag are produced; the obtained zinc and iron slag and zinc hydrometallurgy electrolysis post-liquid are subjected to high-temperature high-pressure leaching, and high-iron slag and high-pressure leachate containing 10 g/L or less of iron are produced; and the obtained high-pressure leachate is subjected to separation for recovery of copper and indium, and indium and copper extraction post-liquid is obtained in the process. According to the zinc and iron separation method, the leaching technology combining traditional hydrometallurgy leaching with pressure leaching is adopted, the leaching process is enhanced, and the slag treatment and deironing process is simplified, so that the zinc leaching rate is high, and the deironing efficiency is high.