Untreated Spent wash discharged from ethanol industries has become an environmental treat. it has been a very challenging task to deal with this eco-toxic waste. The present study aimed at treatment of distillery spent wash using adsorbents extracted from bagasse and modifying its fly ash. The extraction of activated carbon includes chemical activation with the impregnation of phosphoric acid (H3PO4) then carbonizing temperature of 500 oC, while modification of BFA was by using hydrogen peroxide (H2O2) as bleaching agent. The adsorption process parameters such as dosage, contact time and type of adsorbent, were optimized to attain the maximum decolorization efficiency. The structural characteristics of adsorbents were determined by FTIR and surface area using iodine number. The results of the analysis showed that the average reduction of BOD5 and COD was 85.9 %, TDS reduction (52.02 %), decolorization (69.48 %) and low acidity (pH 6.2) were recorded. Then after, adsorption of spent wash on activated carbon and modified BFA were investigated at constant room temperature, different contact times and adsorbent doses. Raising dosage from 2 to 8 grams resulted in increasing uptake of the coloring matters, organic matters such as removal of COD, BOD and dissolved solids. The isotherm study of the adsorbents showed best fit to Freundlich isotherm model in both activated carbon and bagasse fly ash.