The most ideal conditions for preparing activated carbon from grapefruit peel (GPAC) were studied using NH4H2PO4 as a chemical activating agent and the obtained material was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and Brunauer–Emmett–Teller (BET) analysis. The adsorption capacity of the resulting material has been checked using three phenolic compounds (pyrocatechol (CA), 4-chlorophenol (4-CP) and 2,4-dichlorophenol (2,4-DCP)). The adsorption characteristics of phenolic compounds from aqueous solution by GPAC have been investigated as a function of contact time, pH, initial concentration and temperature. The equilibrium experimental data fitted well with Freundlich and Koble–Corrigan isotherms. The adsorption of the three phenolic compounds on GPAC fitted well with pseudo-second-order kinetic model. Different thermodynamic parameters were also evaluated and it was found that the adsorption was spontaneous, feasible and endothermic in nature. Adsorbents were regenerated by 0.1 mol/L NaOH and GPAC could be reused in phenolic compounds removal.