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Wastewater treatment is indispensable as wastewater can lead to adverse health effects and deteriorate the quality of life on earth. Photocatalysis is a facile methodology to address this issue. In this study, nanocomposites (NCs) of manganese oxide (Mn₃O₄) and nickel oxide (NiO) were synthesized in different weight ratios via the solid-state reaction route. Structural properties, optical properties, surface morphology, and functional group analysis of the synthesized nanomaterials were conducted using X-ray diffraction (XRD), UV– Vis spectroscopy, scanning electron microscopy (SEM) along with energy-dispersive X-ray (EDX) analysis, and Fourier-transform infrared (FTIR) spectroscopy, respectively. The bandgap of the nanocomposite decreases significantly from 2.35 eV for the Mn₃O₄ NPs to 1.65 eV for the Mn₃O₄/NiO nanocomposite (NC). Moreover, adsorption studies followed by the photocatalytic performance of the Mn₃O₄/NiO NCs were evaluated to determine the removal of methylene blue (MB) dye from wastewater. The photocatalytic performance of the nanocomposite enhances as the ratio of Mn₃O₄ in the composite increases from one weight percentage to three weight percentage. The photocatalytic degradation efficiency was calculated to be 95%. The results show that the synthesized NCs could play an important role in photocatalytic wastewater purification and environmental remediation.