The study used nickel ferrite NiFe2O4/activated carbon (NiFe2O4/AC) as a means to remove organic dyes (methylene blue and Reactive red 120) from water-based solutions. The produced photocatalysts were characterized based on their morphological, structural, particle size, and surface charge characteristics. The transmission electron microscopy (TEM) pictures indicated that the NiFe2O4 particles, with an average diameter of around 2–2.5 μm, were evenly distributed and adhered to the outermost layer of the AC nanosheets. The BET analysis revealed that the 10-NiFe2O4/AC material had a surface area of 176 m2/g, a pore volume of 0.354 cm3/g, and an average pore diameter of 0.805 nm. The nanocomposite, as opposed to pure NiFe2O4 and clean AC, demonstrates a notably enhanced photocatalytic degradation efficiency for methylene blue (MB) and Reactive red 120 dye under visible light conditions. The findings indicate that the AC loaded with 10 % NiFe2O4 is the most effective photocatalyst, exhibiting a maximum degradation efficiency of 100 % towards MB dye. Additionally, it displays a high mechanical constant, excellent stability, and ease of recycling. The nanocomposite exhibits increased photocatalytic activity owing to the significant reduction in charge carriers recombination, improved capacity to absorb visible light, and the synergistic impact resulting from the heterojunction with NiFe2O4 and AC. The radical entrapment research revealed that the primary active compounds responsible for the photocatalytic degradation process are superoxide (O2−) and hydroxyl (OH*).