The paper deals with the waste disposal problem of the alcohol industry caused by the widespread use of alcohol as biofuels. In the technology for the production of alcohol from cereal crops, a distillery spent wash (DSW) is formed (per 1 dm3 of alcohol – 10–20 dm3 DSW), which refers to highly concentrated wastewater, the COD value reaches 40 g O2/dm3. Since the existing physical and chemical methods of its processing are not cost-effective, the researchers develop the processing technologies for its utilization, for example, an anaerobic digestion. Apart from the purification of highly concentrated wastewater, the advantage of this method is the production of biogas and highquality fertilizer. The problems of biotechnology for biogas production from the distillery spent wash are its high acidity–pH 3.7–5.0 (the optimum pH value for the methanogenesis process is 6.8–7.4) and low nitrogen content, the lack of which inhibits the development of the association of microorganisms. In order to solve these problems, additional raw materials of various origins (chemical compounds, spent anaerobic sludge, waste from livestock farms, etc.) are used. The purpose of this work is to determine the appropriate ratio of the fermentable mixture components: cosubstrate, distillery spent wash and wastewater of the plant for co-fermentation to produce an energy carrier (biogas) and effective wastewater treatment of the distillery. In order to ensure the optimal pH for methanogenesis, poultry manure has been used as a co-substrate. The co-fermentation process of DSW with manure has been carried out at dry matter ratios of 1:1, 1:3, 1:5, 1:7 respectively. It is found that when the concentration of manure in the mixture is insufficient (DSW/manure – 1:1, 1:3), the pH value decreases during fermentation which negatively affects methane formation; when the concentration of manure in the mixture is increased (DSW/manure – 1:5, 1:7), the process is characterized by a high yield of biogas and methane content. The maximum output of biogas with a methane concentration of 70 ± 2% is observed at the ratio of components on a dry matter “wastewater: DSW: manure” – 0,2:1:7 respectively. The COD reduction reaches a 70% when using co-fermentation with the combination of components “wastewater: DSW: manure” (0,3:1:5) respectively.