Biodegradation of pentachlorophenol (PCP) has been studied in a sequence of two completely mixed reactors. Investigation on the first anaerobic sequencing batch reactor (AnSBR) is discussed in detail in this paper. Key technological and microbiological features were studied: two different types of adaptation process of anaerobic sludge towards PCP detoxication; the influence of the sludge concentration upon the rate of PCP biodegradation; minimum retention time for PCP degradation in dependence on the PCP concentration; modeling of the PCP degradation process; effluent COD and SS concentrations; changes in the micro- and macrostructure of the sludge during acclimatization process.