Mixed metal oxides (MMOs) are important semiconductor photocatalysts for water treatment, such as removal of organic dyes and metal ions. In this paper, CuAl hydrotalcite-like compounds (CuAl-HTLcs) were synthesized by the coprecipitation method using Al(NO 3 ) 3 ⋅9H 2 O and Cu (NO 3 ) 2 ⋅3H 2 O as raw materials. Cu 2 O/Cu 2 Al 2 O 4 mixed metal oxides (MMO) were prepared by calcining CuAl-HTLcs at 900°C. The obtained composites were characterized by various methods, including X-ray diffraction (XRD), Scanning electron microscopy (SEM), and UV-Vis diffuse reflectance spectroscopy (DRS), among others. Their photocatalytic activities towards removal of Rhodamine B (RhB) and Cr(VI) were evaluated by spectrophotometry, XRD revealed that CuAl-MMO composites were composed of high crystallinity Cu 2 O and Cu 2 Al 2 O 4 grains. DRS showed the strong ultraviolet absorption ability of the composites. The electrochemical testing demonstrated CuAl-MMO composites with good photocatalytic activities towards the removal of Rhodamine B (RhB) and Cr(VI) under ultraviolet light, with reaction rate constants determined as 0.41 h À 1 and 0.49 h À 1 , respectively. The relevant photocatalytic activities of CuAl-MMO composites were attributed to the synergy between the two components. Overall, these data look promising for future use of CuAl-MMO as an important photocatalyst for water remediation.