MgZnCr-TiO2 (1:1:2–0.05) was successfully prepared by co-precipitation. MgZnCr-TiO2 (1:1:2–0.05) has a good adsorption capacity of Congo red. Congo red was adsorbed and degraded under visible light irradiation by MgZnCr-TiO2 (1:1:2–0.05). The preparation of MgZnCr-TiO2 and degraded Congo red by this way are economical.