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This work presents an efficient method for treating industrial wastewater containing aniline and benzothiazole, which are refractory to conventional treatments. A combination of heterogeneous photocatalysis operating in a fluidised bed reactor is studied in order to increase mass transfer and reduce reaction times. This process uses a manganese dioxide catalyst supported on granular activated carbon with environmentally friendly characteristics. The manganese dioxide composite is prepared by hydrothermal synthesis on carbon Hydrodarco^® 3000 with different active phase ratios. The support, the metal oxide, and the composite are characterised by performing Brunauer, Emmett, and Teller analysis, transmission electron microscopy, X-ray diffraction analysis, X-ray fluorescence analysis, UV–Vis spectroscopy by diffuse reflectance, and Fourier transform infrared spectroscopy in order to evaluate the influence of the metal oxide on the activated carbon. A composite of MnO₂/GAC (3.78% in phase α-MnO₂) is obtained, with a 9.4% increase in the specific surface of the initial GAC and a 12.79 nm crystal size. The effect of pH and catalyst load is studied. At a pH of 9.0 and a dose of 0.9 g L⁻¹, a high degradation of aniline and benzothiazole is obtained, with an 81.63% TOC mineralisation in 64.8 min.