Abstract: The UiO-66 catalysts with different doping ratio of Fe were prepared by hydrothermal synthesis method in this study. The physicochemical properties of the catalysts were characterized by means of XRD, SEM and XPS. The benzene removal efficiency of the catalysts was investigated using a bench-scaled heterogeneous Fenton-like system device. The effects of Fe loading amount, H₂O₂ concentration, superficial velocity and reaction temperature on benzene removal efficiency were studied. The results showed that the Fe doped UiO-66 was irregularly spherical and of high crystallinity. The highest benzene removal efficiency was obtained at 93% over the catalyst with 30% Fe loading. The EPR results proved that increasing Fe loading on UiO-66 evidently promoted the production of ·OH radicals, which promoted the degradation of benzene to a certain extent. The benzene removal efficiency decreased with the rise of temperature at higher range because H₂O₂ was unstable at high temperature.