Adsorptions of methanol and glycerol in their binary mixtures were carried out batch wisely on commercial coconut shell activated carbon at ambient temperature. Adsorption equilibria, as well as adsorption isotherms, were investigated. For recovery of adsorbed methanol and glycerol, a regeneration process had been proposed. The adsorption reached the equilibrium within 60 min. The adsorption isotherms of both methanol and glycerol were agreed very well with Freundlich's model, where the equilibrium constants were 2.1145 and 0.9313, respectively, and the indexes became 0.5642 and 1.2173, respectively. In addition, the adsorbent could be regenerated by drying at 80C, washing with distilled water and drying at 120C for 3 hours. However, the adsorption performance of the regenerated adsorbents was reduced by 30 - 70 % of the original adsorbent depending on the concentration of the binary mixture.