The disposal of sulfur compounds from fossil fuels in general and diesel fuels particularly has been stimulated worldwide due to their harmful environmental emissions during the combustion process. Several desulfurization techniques can be employed; however, photocatalytic desulfurization can be considered as the safest and cost-effective route to achieve such goal. This study introduces a novel hybrid photocatalyst made of coupling both NiO and poly-acrylamide based polymer. Such composite could have improved photo-luminance (PL) properties than that of pure NiO. Additionally, the combination of NiO (which is UV-active photocatalyst) with polymer could result in producing visible-light effective composite. These optical properties had progressively improved the photocatalytic desulfurization performance of this composite. It could attain a sulfur removal of 60 % from a diesel fuel fraction contains 12300 ppm of sulfur. This rate of sulfur removal could be counted as an extremely high and of obvious advancements in the field of diesel fuel desulfurization.