The hypercrosslinked polymers Macronet MN-150 and MN-500 (denoted as MN-150 and MN-500) were investigated to remove the pesticide methomyl from aqueous solutions via adsorption. Furthermore, the effect of humid acid (used as background organic compound) on the adsorption capacity of methomyl for MN-150 was examined. The equilibria and kinetics of the adsorption of methomyl onto MN-150 and MN-500 can be well correlated with Langmuir and Freundlich isotherms, and conventional kinetic models (e.g., surface and pore diffusion models), respectively. The polymer MN-150 possesses a high potential to be applied as adsorbent for the removal of methomyl from aqueous solution when compared with MN-500. Furthermore, the competitive effect of humic acid on adsorption of methomyl on MN-150 can be ignored at low equilibrium concentrations. The transport of methomyl from solution into the polymer adsorbents is controlled by both, external and internal mass transfer mechanisms with film-surface diffusion model offering the better description. The surface mobility and flux of surface diffusion increase as the initial concentration increases.