Abstract: In allusion to Zn-Cu containing fly ash,a technology using it as raw material for preparation of active zinc oxide and by-product cupric sulfate was put forward on the basis of the comparison with other schemes.This technology realized the separation of Zn and Cu through volatilizing Zn by carbon reduction method.Then,the active zinc oxide could be obtained by acid leaching method.Cu-containing residue would be used for preparing cupric sulfate.High temperature carbon reduction volatilization was an important key-technology for separation of Zn and Cu during the whole process.Under the assured process conditions,recovery rates of Zn and Cu could be up to 96.21% and 97.95%，respectively in the full process.Obtained active zinc oxide met the Standard of HG/T 2572—1994.Fe(OH)<SUB>3 </SUB>produced during the purification of zinc sulfate and cupric sulfate was dried and calcined,and then high quality iron ore concentrate could be obtained.Ammonium sulfate solution was produced during the process of preparing the precursor of active zinc oxide with zinc sulfate,which was condensed and crystallized,and then ammonium sulfate product was obtained,which could be used as agricultural fertilizer.In addition,the water produced during the condensation could be recycled.This technology provided a good reference for comprehensively making use of the same materials as the fly ash.