In this study, Cu/Fe type mixed oxides catalysts with different ratios of metal irons are successfully synthesized via fixed hydrothermal treatment. The prepared samples were then characterized by a combination of several techniques, such as XRD, BET, SEM, H2-TPR and FT-IR. The catalytic activity enhanced with the increasing amount of Cu in the HT-precursors, but it decreases when the ratio of Cu/Fe is above 4. The influence of calcination temperature was also studied in the search of highly dispersed active catalysts. The catalytic test indicated that the Cu/Fe mixed oxides possessed outstanding highly activity towards toluene oxidation. The highest catalytic activity was exhibited by Cu4Fe-400 of which the T50 and T90 reaches at about 258 °C and 294 °C respectively.