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The aim of the study was to determine the possibility of using coagulation for treatment of anaerobically digested distillery stillage. Post-fermentation sludge from waste product of bioethanol production is usually drained. Then, condensed sediments are directed as a fertilizer for arable fields. The remaining liquid phase due to the high content of organic compounds cannot be discharged to environment. The study used inorganic salts of iron and aluminum as coagulants to treatment liquid fraction obtained after methane fermentation of distillery stillage. In valorization process, the reduction of organic compounds and suspended solids was not sufficient. The highest doses of coagulants reduced COD concentration of about 80% and lower the pH of the solution. However, the dose 10 mL/L is not economically profitable and due to concentration of aluminum or iron it is too harmful for environment.