The present work is aimed at increasing the overall efficiency of the treatment process of distillery spent wash using a combination of different treatment techniques. Initially the effluent samples were subjected to Thermal Pretreatment (TPT-DW) and anaerobic treatment (ANA-DW). Advanced oxidation techniques, viz., Ultrasound (US) and Ozone were then used for further COD reduction followed by the conventional aerobic oxidation using mixed microbial consortium. Pretreatment of TPT-DW with US and Ozone (as stand alone techniques) enhanced the subsequent aerobic oxidation rate. For US treated sample, a maximum of 13% COD reduction was attained at the end of 48 h of aerobic oxidation, while for the ozone treated effluent a maximum of 45.6% COD reduction was obtained as compared to mere 1.8% COD reduction for the control (TPT-DW directly subjected to aerobic oxidation) indicating a 25 times increase in the rate of aerobic biodegradation of ozonated sample. Anaerobically treated effluent sample (ANA-DW) could be successfully treated aerobically. In this case, however, the use of advanced oxidation techniques did not result in any synergistic effects. The rate of the aerobic oxidation was slightly higher for the control (ANA-DW directly subjected to aerobic oxidation) as compared to the sample pretreated using ultrasound or ozonation. TOC analysis revealed that between the two pretreatments studied, ozone was found to be superior over US as it led to both COD as well as TOC reduction during the aerobic oxidation step for ANA-DW effluent stream.