Abstract: In this article, Ni/CNTs(carbon nanotubes) catalyst′s effect for methanol vaporphase carbonylation under atmospheric pressure were studied. The relations between the catalyst activity and drying condition, the temperature of thermal treatment(with N2) and reduction(with H2) were investigated. The catalyst showed high activity when catalyst were dried step by step. The optimal temperature for thermal treatment with N2 and reduction with H2 were 300℃ and 700℃respectively.