Anaerobic treatment of distillery wastewaters containing high sulfate concentrations was carried out on a two-phase process. The acidogenic phase was operated so as to produce the more favourable intermediates for methanogenic bacteria coupled with maximum sulfate removal. Sulfate removal was directly affected by pH and dilution rate (D). The maximum sulfate removal and acetic acid production was achieved at pH 6.6 and D=0.035 h-1. A linear relationship between acetic acid produced and sulfate removal was observed, indicating that acetic acid was mainly produced by sulfate reducing bacteria with important operational advantages. Higher concentrations of butyric acid were obtained at low pH values and high dilution rates.