Ethanol-water near-azeotropic mixture dehydration was investigated by formulated compound starchbased adsorbent(CSA), which consists of corn, sweet potato and foaming agent. The net retention time and separation factor of water over ethanol were measured by inverse gas chromatography(IGC). Results indicated that water has a longer net retention time than ethanol and that low temperature is beneficial to this dehydration process. Orthogonal test was conducted under different vapor feed flow rates, bed temperatures and bed heights, to obtain optimal fixed-bed dehydration condition. Dynamic saturated adsorbance was also studied. It was found that CSA has the same water adsorption capacity(0.15 g/g)as some commercial molecular sieves. Besides, this biosorptive dehydration process was found to be the most energy-efficient compared with other ethanol purification processes. Ethanol-water near-azeotropic mixture dehydration was investigated by prepared compound starch based adsorbent (CSA), which consists of corn, sweet potato and foaming agent. The net retention time and separation factor of water over ethanol were measured by inverse gas chromatography (IGC) Results indicated that water has a longer net retention time than ethanol and that low temperature is beneficial to this dehydration process. Orthogonal test was conducted under different vapor feed flow rates, bed temperatures and bed heights, to obtain optimal fixed-bed dehydration condition. This was found that CSA has the same water adsorption capacity (0.15 g / g) as some commercial molecular sieves. Besides, this biosorptive dehydration process was found to be the most energy-efficient compared with other ethanol purification processes.