This paper describes the adsorption properties of Cu(II) ions from aqueous media by 4-ethyl thiosemicarbazide (ETSC) intercalated organophilic calcined hydrotalcite (OHTC). Elemental analysis, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and thermogravimetric–differential thermogravimetric (TG/DTG) studies have helped in characterizing the adsorbent. The effects of various factors like adsorbent dose, pH, initial concentration, and contact time were studied. The pH study indicated that Cu(II) has a good adsorption potential at pH 5.5. The adsorption of metal ion remained constant after 4 h. The pseudo-second-order model was the best fit to describe the adsorption kinetics. The FTIR spectroscopy revealed that both amino and thiocarbonyl groups in ETSC–OHTC are responsible for Cu(II) removal. The Freundlich model described the adsorption results very well, and the KF value was found to be 21.38 at 303 K. Electroplating industry wastewater was used to test the adsorption efficiency toward Cu(II) removal. The recovery (∼95.0 %) of Cu(II) ion from the loaded adsorbent was possible with 0.01 mol·kg–1 HCl solutions. Many successive adsorption/desorption cycles were achieved without any noticeable change in the adsorption capacity.