In this paper, the ability of pillared clay by Al/Fe polymerics as an adsorbent for the removal of p-xylene from an aqueous solution has been investigated under various experimental conditions. Bentonite from Hammam Boughrara located in Maghnia village (Algerian) was purified then, modified by intercalation with Al3+ and Fe3+ polymerics (FeAl/B). The adsorption kinetic study showed that equilibrium could be achieved within 30 min. The maximum adsorption capacities of FeAl/B to p-xylene based on the Langmuir isotherm was 275 g/g with a higher percentage removal up to 99.97%. The adsorption equilibrium data fitted well by the Langmuir adsorption isotherm model. It was found that FeAl/B had high adsorption capacity for p-xylene due to cation exchange and high surface area 224.3 m2 /g. FeAl/B was concluded as a promising and effective adsorbent for the removal of p-xylene from wastewater.