The purpose of this study is to elucidate the adsorption properties of fly ash (FA)-derived zeolites A and X for the divalent cationic herbicides, paraquat and diquat. Their adsorption isotherms were well fitted to the Langmuir equation, indicating that adsorption mainly occurred on the crystal surface. FA-zeolite X showed a higher adsorption capacity than that of FA-zeolite A due to wide pore window size in spite of its low CEC. The equilibrium adsorption increased with increasing the reaction temperature because of the enhanced molecule activity and the thermal expansion of zeolite pore windows. Overall, these results demonstrated that the FA-zeolite synthesized from fly ash could be used as a low-cost mineral adsorbent for the removal of environmental cationic organic pollutants from the aqueous solution.