In this work, acrylonitrile (AN)/ethylene glycol dimethacrylate (EGDMA) cross-linked polymeric adsorbents were synthesized by the suspension polymerization method. The adsorbents were prepared varying the EGDMA cross-linker ratio from 100 to 60%. It was found that the swelling factor and the specific surface area changed inversely with the crosslinking degree. In addition, the thermal characterization indicated that polymers stability increased as the crosslinking degree decreased. The polymers were tested as phenol adsorbents and it was found that the higher uptake level was reached when the acrylonitrile concentration increased in the polymer. Adsorption isotherm was determined fitting the Langmuir model, indicating a homogeneous surface of the adsorbents. Moreover, the kinetic studies indicated that the rate controlling step corresponded to the in-traparticle diffusion since adsorption is promoted when the adsorbent is swollen.