Regenerative catalytic oxidizers (RCO) are conveniently used to control the emissions of volatile organic compounds (VOCs), because of their high thermal recovery efficiency (TRE) and low cost. In this work, three catalysts were prepared by impregnation, and used in RCOs to test their performance in toluene oxidation, TRE, the difference between the temperatures of the inlet and the outlet gases (Td), and pressure drop under various operational conditions. Experimental results demonstrate that 10 wt% CuCo/(G) catalyst is the best catalyst in an RCO because it is effective in treating toluene with a toluene conversion of up to 95% at the heating zone temperature (Tset) = 400°C under various conditions. The 10 wt% CuCo/(G) catalyst has the greatest tolerance against the effects of inlet toluene concentration and gas velocity (Ug), and exhibits the best performance in terms of TRE, Td, and pressure drop. The TRE range was from 90.2% to 92.9% and Td ranged from 18.2°C to 30.9°C under various conditions at Tset = 300°C–400°C. Moreover, when 10 wt% CuCo/(G) catalyst was used in an RCO, the results demonstrate (1) high selectivity to CO2; (2) decrease in TRE and increase in Td as increasing the shifting time; (3) an insignificant effect of shifting time on pressure drop; (4) easier destruction of isopropyl alcohol (IPA) than toluene; and (5) excellent stability of 10 wt% CuCo/(G) catalyst in a long period test.