Adsorption and catalytic degradation of organic dyes were investigated using ZnO/Zn_xFe_3−xO₄ mixed oxides (ZFOs). Two ZFOs with varying ratio of zinc:iron were synthesized by co-precipitation technique and their physico-chemical properties were studied using N₂ adsorption–desorption, X-ray diffraction, thermo-gravimetric analysis, scanning electron microscope, transmission electron microscope, vibrating sample magnetometer, and Zetasizer. The synthesized ZFOs were evaluated for the removal of two azo dyes, Acid Blue 113 (AB-113) and Orange II (OR-II), from water by adsorption and by catalytic degradation. The influence of the factors such as adsorbent/catalyst dosage, amount of the oxidant (H₂O₂), solution pH and reaction temperature on removal of the dyes by the ZFOs was investigated. Increase in reaction temperature led to significant increase in degradation of the dyes by the ZFOs. Regeneration and reuse of the catalysts were also studied up to five cycles.