This work developed an innovative activated carbon (ICAC) derived from orange peels (OP) through chemical activation using FeCl3. The traditional activated carbon (PCAC) that was prepared through K2CO3 activation served as a comparison. Three adsorbents (ICAC, PCAC, and OP) were characterized by various techniques, these being: Brunauer-Emmett-Teller (BET) surface area analysis, thermo-gravimetric analysis, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy. They were applied to remove diclofenac from aqueous solution applying batch experiments, in order to investigate the characteristics of adsorptive kinetics, isotherms, and thermodynamics. Results indicated that the S-BET values were in the following order: 457 m(2)/g (PCAC) > 184 m(2)/g (ICAC) > 3.56 m(2)/g (OP). The adsorption process reached a fast equilibrium, with activating energies being 27.6 kJ/mol (ICAC), 16.0 kJ/mol (OP), and 11.2 kJ/mol (PCAC). The Langmuir adsorption capacities at 30 degrees C exhibited the decreasing order: 144 mg/g (ICAC) > 6.44 mg/g (OP) > 5.61 mg/g (PCAC). The thermodynamic parameters demonstrated a signal dissimilarity between biosorbent (Delta C degrees < 0, Delta H degrees < 0, and Delta S degrees < 0) and activated carbon samples (Delta G degrees < 0, Delta H degrees > 0, and Delta S degrees > 0). The presence of iron (FeOCl, gamma-Fe2O3, and FeOOH) on the surface of ICAC played a determining role in efficiently removing diclofenac from solution. The excellent adsorption capacity of ICAC toward diclofenac resulted presumably from the contribution of complicated adsorption mechanisms, such as hydrogen bonding, ion-dipole interaction, pi-pi interaction, pore filling, and possible Fenton-like degradation. Therefore, FeCl3 can serve as a promising activating agent for AC preparation with excellent efficiency in removing diclofenac.