This study presents the preparation, characterization and application of TiO2-bentonite (Ti-BNP), with the aim of promoting natural bentonite, designed for the degradation of methyl orange (MO) under UV light (365 nm). The natural bentonite has been purified (BNP) and doped with various TiO2 mass ratios. The structural, mineralogical and morphological composition of *x*%Ti-BNP (*x* = mass % of TiO2 in bentonite) have been investigated using various techniques such as Fourier-transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) surface area analysis, UV–vis diffuse reflectance spectroscopy (DRS), scanning electron microscopy (SEM), and transmission electron microscopy (TEM-EDS). The obtained results revealed that *x*%Ti-BNP undergo structural modifications, with spectral intensity scaling proportionally to TiO2 content. While pure TiO2 demonstrated superior activity, the composites’ photocatalytic performance improved with higher TiO2 loading. Degradation kinetics adhered to the Langmuir-Hinshelwood model, underscoring the critical role of surface adsorption. Optimal conditions were identified as acidic pH (enhancing interactions with anionic MO) and a catalyst mass of 25 mg (beyond which turbidity reduced efficiency). These findings suggest the promise of clay-TiO2 hybrids for pollution mitigation, though further optimization of TiO2 dispersion and surface properties is required to rival pure TiO2.
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