AbstractPalygorskite–TiO2 nanoparticles are frequently used as nanocatalysts. In the present study, two different nanocatalysts were developed based on the use of different palygorskite–TiO2 ratios: 40–60 and 10–90. The nanocomposites were investigated for the photocatalytic degradation of the common fungicide tebuconazole (TEB), under aquatic conditions. The samples were extensively characterized by X‐ray powder diffraction, attenuated total reflectance–Fourier transform infrared spectroscopy, scanning electron microscopy and N2 specific surface area (SSA) by Brunauer–Emmett–Teller (BET) analytical techniques. The TiO2 nanoparticles were successfully dispersed on the mineral's surfaces and the photocatalytic activity reached 88.4% for the palygorskite–TiO2 ratio of 40:60, where the dispersion was better as proved by the total pore volume and BET parameters (0.49 cm3/g and 258 m2/g compared to 0.33 cm3/g and 220 m2/g of the 10:90 ratio). The photocatalytic efficiency of the proposed materials was significantly higher than Degussa P25 (33.2%), and that makes the palygorskite–TiO2 nanocomposites very promising for advanced application in fungicides' degradation in aquatic environments.