The catalytic activity was found strongly influenced by the reaction parameters such as initial total pressure, reaction temperature,molar ratio of CO/C2H2, the volume ratio of solvent/water and the catalyst amount. In addition, the copper salt plays an indispensable but double role in the hydrocarboxylation of acetylene. It will work with acetylene as well in ı-metal–carbon bonds as in -metal–carbon bonds. These copper–acetylene complexes are much easier to coordinate toward Ni center.The XRD and XPS characterization indicates that the nickel oxide remains in its state unchanged during the whole reaction. The SEM,TG and XRD analyses of the reacted catalysts suggest the occurrence of coke with filamentous lines and helical structures deposited on the surface of the nickel oxide. The three types of coke occurred at a low temperature ranging from 250◦C to 400◦C and can be assigned to soft coke. Different reaction conditions will result in different coke amount, and it can be removed through calcination.