Abstract: the "diffusion dialysis pretreatment countercurrent purification andneutralization and precipitation of copper - PH nickel deposition" recovery of copper sulphate removal process in mother liquor of arsenic acid and valuable metals copper, nickel. Experiments show that: the control of arsenic removal liquid flow rate is 220L / h, arsenic removal liquid flow and water flowratio is 1.1, acid recovery rate reached 77.92%, copper, nickel interceptionrate reaches above 98%, arsenic retention rate is above 80%; neutralization and precipitation of copper to control the temperature of 80-90 ℃, solid-liquid ratio (2-3): 1, the reaction time is 3h, the end pH value of 5, Cu depositionrate is above 95%, the nickel deposition rate is below 2%; adjusted PH nickel deposition pH control to 12-13, temperature 80-90 ℃, reaction time 3h, nickel precipitation rate of more than 98%, nickel slag from nickel containing up to 32.83%, can be used as the production of nickel sulfate and other chemical products raw material.