Polystyrene resin was functionalized by diethanolamine for the efficient removal of p -toluenesulfonic acid (p-TSA) from aqueous solution. Functionalized adsorbent (DEA-PS) was characterized by elemental analysis, Fourier transform infrared spectroscopy, point of zero charge measurement and field-emission scanning electron microscopy. According to the results, maximum removal of p-TSA was observed at the pH range of 2.5–5. The adsorption kinetics of p-TSA onto DEA-PS was represented by pseudo-first-order model and the equilibrium data followed Langmuir model well. The adsorption process was endothermic and spontaneous, along with the positive change of entropy. The regeneration of DEA-PS was also conducted by 1 M NaOH solution.