This work aims at exploring the feasibility of a combined process bioflocculation to concentrate sewage organic matter and anaerobic fermentation to produce volatile fatty acids (VFA). Bioflocculation, using a high-loaded aerobic membrane bioreactor (HL-MBR), was operated at an HRT of 1 h and an SRT of 1 day. The HL-MBR process removed on average 83% of sewage COD, while only 10% of nitrogen and phosphorus was removed. During anaerobic fermentation of HL-MBR concentrate at an SRT of 5 days and 35 °C, specific VFA production rate of 282 mg VFA-COD/g VSS could be reached and consisted of 50% acetate, 40% propionate and 10% butyrate. More than 75% of sewage COD was diverted to the concentrate, but only 15% sewage COD was recovered as VFA, due ...