Abstract The treatment of toxic organic pollutants is extremely important for the conservation of clean air, soil, and water. In this study, (reduced graphene oxide) NiCo2O4/ rGO hybrid nanocomposite was prepared by a facile hydrothermal technique and employed for organic dye degradation from wastewater. The synthesized NiCo2O4/rGO hybrid nanocomposite was studied using FTIR, XRD, SEM, TEM, BET, Raman spectroscopy, and UV-visible. The physical characterizations prove the deposition of NiCo2O4 particles on the rGO surface. The transmission electron microscope image demonstrated that the NiCo2O4 particles with an average size of ~46 nm was dispersed on the rGO surface. The obtained nanoparticles show a higher specific surface area of 56.4 m2/g. Adsorption dynamics as investigated by time and concentration variation show that the adsorption data follows pseudosecond order kinetics and the Langmuir isotherm model, with a maximum adsorption capacity of 106.2 mg/g, indicating homogeneous physiochemical adsorption of CR dye on the adsorbent surface. Besides, the catalytic effectiveness of synthesized nanocomposite towards Congo red (CR) dye reduction mediated by the electron (e-) transfer route of BH4- ions was explained in detail. The electrostatic interaction used between the NiCo2O4/rGO hybrid composite and Congo red increased the degradation effectiveness of the dye sample.