Adsorption treatment of distillery spent wash has great potential as a sustainable method as it is a low-cost method. The aim of this investigation is to study the treatment method for purification of distillery spent wash by using Fly ash and Wood ash. For this, the study comprising evaluation of reduction of various physical-chemical parameters (Color, Odor, pH, COD, TS, TDS, Ca, Mg, Na, and K) of distillery spent wash was checked by passing through the columns of Fly ash and Wood ash. The distillery effluent was acidic (pH 4.7) and dark brown in color which often cause psychological fear in farmers for utilization. Fly ash treatment of spent wash exhibited a good reduction in COD, TS, TDS, Mg, Na, Ca, after 72-hour treatment and increase in pH toward pH 7 followed by Fly ash + Wood ash (1:1).