Ag in waste Ag/α-Al2O3 catalyst was dissolved by nitric acid to silver nitrate solution,and was diaplaced by copper.The substitute fluid was concentrated to obtain copper nitrate.NaAlO2 solution was synthesized by the reaction of α-Al2O3 and NaOH.The NH4AlO(OH)HCO3 was synthesized by the reac-tion of NH4 HCO3 solution and NaAlO2 solution under pH>9,n(NH4 HCO3)∶n(α-Al2O3)>2∶1,and droplet rate of 110 mL·min-1.Pseudo-boehmite was prepared by calcination of NH4AlO(OH)HCO3 at 300 ℃.The purity and yield of Ag were >99.95% and >98.5%,respectively.Yield of Cu(NO3)2 was>70%.In the discharged wastewater,COD<20 mg·kg-1,Cu2+<5 mg·kg-1.Specific surface area of pseudo-boehmite was about>390 m2·g-1,and pore volume was(1.19~1.32)mL·g-1.This method has the advantages of low cost,simple operation,and is easy to treat wastewater.