The rise in the discharge of pharmaceutical wastewater in the form of heavy metals Cr6+, Fe3+, and Pb2+ has become an issue of serious concern to the environment and to the general population since these elements are toxic, persistent, and may accumulate in the body. Cr(vi), FE(iii) and Pb(ii) are common toxic contaminants in the Pharma effluents and their quick, effective elimination is paramount in regulation compliance and environmental safety. A simple, scalable synthesis of a bimetallic NiO/CuO nanocomposite was reported in this study through a concurrent coprecipitation-hydrothermal reaction, and then subjected to calcination at 400 0 C. This paper is concerned with synthesis and use of nickel oxide/copper oxide (NiO/CuO) nanocomposites to effectively clean such metal ions that are present in pharmaceutical effluents. NiO/CuO nanocomposite was produced by a slight modification of the sol-gel technique and investigated by X-ray diffraction (XRD), and scanning electron microscopy (SEM) to ascertain the structural, morphological and functional characteristics of the material. The effect of pH, contact time and adsorbent dosage on the adsorption efficiency was studied through batch adsorption. It was found that, at a dosage of 0.8 g, the removal efficiencies increase to 100% for Cr, 96.81% for Fe, and 92.40% for Pb. This demonstrates near-complete removal of Cr and very high removal for Fe and Pb, indicating that the adsorption capacity of the nanocomposite is nearing saturation. Kinetics of the adsorption process was in pseudo-second order and adsorbed monolayers on a homogeneous surface which is pointing to Langmuir isotherm. The regeneration studies indicated the multiple adsorption-desorption cycles of the nanocomposite with its stability and reusability. This report establishes the possibilities of NiO/CuO nanocomposites as a powerful, inexpensive, and ecologically safe adsorbent to treat heavy-metal-contaminated pharmaceutical wastewater to be a part of the sustainability of waste sources and pollution prevention.