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This paper investigates the mechanism of removal of Sb and Bi from copper electrolyte under the function of arsenic. The precipitation reactions were carried out from a synthetic electrolyte containing 185g/L sulfuric acid and 45g/LCu2+ in the presence of As (III, V), Sb(III, V) and Bi(III) under the temperature 65°C and stirring rate of 300r/min. The structure, morphology and component of the precipitate were clarified by methods of chemical analysis, SEM, XRD, TEM, EDAX and IR spectroscopy. A kind of white precipitate has irregular shape and mainly consists of As, Sb, Bi and O elements forms in this electrolyte. The characteristic bands in the IR spectra of the precipitate are O-H, As-OH, As-O-Sb, Sb-OY (Y=As, Sb, Bi), and O-As-O. The precipitate is a mixture of microcrystalline of (Sb,As)2O3, BiSb2O7, SbAsO4 and amorphous phases by XRD and electronic diffraction. The removal rate of Sb and Bi reaches 43% and 64%, respectively from copper electrolytes by a 4g/L arsenic solution owing to these precipitate.