Cu1–xNixO/Fe2O3 (with x = 0.01, 0.02, 0.03, 0.04 wt%) were synthesized by plant extraction technique. The absorbance and degradation performance of Ni-doped CuO and Fe2O3 nanocomposite against methylene blue (MB) was analyzed, and the 2% Ni-doped CuO yielded an optimum result, and the optical bandgap of CuO, 2NCO, Fe2O3, and (60%) 2NCO/40% Fe2O3 was found to be 1.88, 1.73, 2.1, and 1.80 eV, respectively. Hence, the 2% Ni-doped CuO (2NCO) was further used for the establishment of a composite with Fe2O3. The lowest composition of the oxide composite was (1−x) 2NCO/(x) Fe2O3 (x = 0.1, 0.2, 0.3, 0.4, and 0.5). The degradation performance of those oxide composites was determined against (MB) with the nominal composition of sample (60%) 2NCO/40% Fe2O3 resulted in an optimum degradation of MB with a percentage of 94% at 120 min. The recyclability takes a look at was performed for five cycles at the start of 94%; after five cycles, the sample remained stable at 120 min. Therefore, 2NCO/40% Fe2O3 composite is going to be the selection material for waste product treatment.