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In this paper, Zn(OAc) 2 /AC and Zn-Co/AC catalysts were prepared and applied in an acetylene acetoxylation reaction. Compared with monometallic Zn(OAc) 2 /AC catalyst, which is widely applied in industry, the Zn-Co catalysts exhibited excellent catalytic performance. Transmission electron microscopy results displayed that the addition of cobalt improved the dispersity of zinc acetate particles and inhibited catalyst sintering on the catalyst surface. X-ray photoelectron spectra suggested that the Co additive changed the electron density of zinc acetate probably because of the interaction between Zn and Co species. Temperature programmed desorption analysis demonstrated Co additive strengthened the adsorption of acetic acid and weakened the adsorption of acetylene.