The lab-scale and pilot-scale physical-chemical and biochemical combined technology tests were carried out for the treatment of refractory petrochemical dry-spun acrylic fiber wastewater in Liaohe River, in which the multi-compartment anoxic/oxic membrane bioreactor (A/O MBR) and multi-technology coordinated catalyzed ozone oxidation were used as core unit process. The results showed that the removal performance could be improved significantly by reasonable coupling of physical-chemical and biochemical technologies in the treatment of acrylic fiber wastewater, the COD, ammonium and total nitrogen removal efficiency in combined process of MBR, ozone oxidation and biological aerated filter(BAF) could reach 90 %, 95 % and 80 %, respectively, and their concentration of effluent were below 100 mg/L, 5 mg/L and 35 mg/L. In addition, due to the lack of biodegradable organic carbon source and the refractory of acrylonitrile oligomers and nitrogen-containing heterocyclic organic matter in dry-spun acrylic fiber wastewater, the ammoniation steps which converted organic nitrogen to inorganic ammonium had limited the total nitrogen removal effect of overall process.