CuO/UiO-66-NO2 composite photocatalysts were successfully synthesized. The as-fabricated samples were characterized by XRD, FT-IR, and UV-Vis DRS techniques. The photocatalytic activity of the materials was evaluated by the decomposition of methylene blue (MB) under visible light. The influence of several factors such as pH of solution and dosage of the catalyst on the photodegradation was studied. The optimum conditions for the synthesis of the catalyst were also determined. Under optimal conditions, it was found that 100% of MB was removed due to the adsorption in darkness and the degradation in visible light illumination within 200 min. The kinetics of the photocatalytic process were investigated and compared with pseudofirst-order and pseudo-second-order. The experiment data revealed that the kinetics of the photodegradation fitted with the pseudo-first-order model and relatively fitted with the pseudo-second-order.