<p>In this study, poly vinyl alcohol assisted Fe₂O₃/NiO hyper cross linked polymer (HCP) were synthesized via Sol-gel method were mainly focused to remove aromatic hydrocarbons, but it also exhibit the adsorption of organic pollutants making it versatile for environmental remediation. The X-ray diffraction analysis shows the formation Fe₂O₃/NiO composites. The morphological studies confirm the formation of hyper cross linked polymer in agglomerated state. Besides the Tauc plot depict the increase in the bandgap after the incorporation of NiO on Fe₂O₃ nanoparticles. Then the Fe₂O₃/NiO HCP composites were characterized using diesel oil as a typical adsorbate via batch adsorption-photocatalytic experiment in aqueous solution. It shows an effective adsorption of Methylene blue (84% in 80 min) and the diesel oil in aqueous solution with the maximum adsorption efficiency of 93% with the linear correlation coefficient of 0.9768 via photocatalytic UV light signal damper. Also the Fourier transform infrared spectra confirm the maximum adsorption occurs for Fe₂O₃/NiO HCP as composites. The TOC analysis shows highest reduction efficiency for Fe₂O₃/NiO HCP as 94.64% (Methylene blue dye), and 85.87% (Diesel sample). This work depict the adsorption of aromatic based compounds in the aqueous solution, since the composite is magnetic in nature it could be removed and recycled for the further use.</p> Graphical Abstract <p></p>