In this study, pure ZnCo2O4 and SnO2/ZnCo2O4 mix photocatalysts have been synthesized by the sol-gel process with three different SnO2 loading percentages (10, 20, and 30 wt %). Their photocatalytic activities were assessed on the degradation of organic pollutants in water under visible illumination. The structural, morphological, and optical properties were analyzed by X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray (EDX), Fourier transform infrared (FTIR), nitrogen adsorption-desorption isotherms, X-ray photoelectron spectroscopy (XPS), and UV–Visible diffuse reflectance measurements. The results have shown that the materials are composed of a crystalline ZnCo2O4 matrix with a decrease in crystallite size with the amount of SnO2. Weakly crystalline SnO2 is also observed for loaded samples. The specific surface area is modified with the loading ratio. The evaluation of the photoactivity of the samples under visible light for the degradation of p-nitrophenol has highlighted that all materials are highly photoactive under visible light thanks to heterojunction between the two oxides. An application test has been conducted on a dye, congo red, showing the same tendencies. An optimal amount of SnO2 loading is observed for the sample containing 20 wt % of SnO2. A comparison with commercial Evonik P25 showed that the materials developed in this work have five to six times better efficiency under visible light, leading to a promising photocatalyst material.