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This study investigated the geochemical and physicochemical characteristics of natural clay collected in the Democratic Republic of Congo. The optical properties of the sample collected in Golf (GOL) were tested in the removal of 4-nitrophenol in aqueous solution. The geochemical analysis depicted that all the samples are plotted within the shale quadrant. Furthermore, the Chemical Index of Alteration (CIA) indicated that the samples are extremely weathered. The particle size distribution ranged from 0.41 to 418.6 μm, while the pore diameters for all the samples were under 100 Å. A flake-like surface morphology was observed in all the samples. SiO2, Al2O3, Fe2O3, K2O, and TiO2 were the major chemical compounds found in all the samples, while the XRD analysis showed the presence of quartz, kaolinite, magnetite, and illite. The presence of metal oxides (i.e., TiO2 and Fe2O3) indicated that these natural clays can be used for photocatalytic oxidation of pollutants. The sample collected in Katuba (KAT) displayed the higher reflectance percentages for the selected wavelengths except at 200 nm. Interestingly, the GOL sample exhibited lower energy band gaps (2.68 and 3.94 eV) necessary for photocatalysis. The untreated GOL clay sample removed 99.13% of 4-nitrophenol from aqueous solution through the photodegradation process. The usage of the untreated GOL clay could be a cost-effective solution in the removal of 4-nitrophenol in wastewater.