The fresh and reacted catalysts were characterized by TG technology. The TG, DTG, and heat flow results from the temperature-programmed oxidation (TPO) of the various coked catalysts are shown in Fig. 10. The weight ratio in Fig. 10 equals the weight at each temperature point divided by the original sample weight. From the DTG result of those reacted catalysts, three obvious oxidation peaks were observed. It seems that three types of carbon were formed during the reaction. The oxidation peaks appear somewhat different from each other according to the specific reaction conditions, but all of them occur at low temperature zone. For example, the oxidation peaks of recovered Ni2O3(5)occurred at a temperature about 300◦C, 317◦C, and 353◦C, respectively. These three types of coke can be collectively referred to as soft coke, which can be removed at a relative lower temperature [27]. In other words, the reacted catalysts can be regenerated through calcination within 400◦C. From the view of coke amount,the high concentration of CuBr2 in the liquid would boost the formation of coke followed by the reaction with equal molar ratio of CO/C2H2. The TG analysis agrees well with the finding in the XRD and SEM characterization.