A new heterogeneous catalyst, lead-zinc double oxide, has been prepared for the synthesis of diphenyl carbonate (DPC) by transesterification of dimethyl carbonate (DMC) and phenol. The effects of preparation method, calcination temperature, precursor and molar ratio of Pb/Zn on the catalytic activity have been investigated. XRD, TPR and atomic absorption spectroscopy were employed for the catalyst characterization. The results show that Pb3O4 is the main active species, and that amorphous ZnO plays a role as the promoter. Under the conditions of calcination temperature of 500degreesC and Pb/Zn = 2: 1, the highest activity of the catalyst, DPC yield of 45.6%, was achieved. The reason for deactivation of the catalyst was the vanishing of Pb3O4 (C) 2003 Published by Elsevier B.V.