A combined process of flocculation and Fenton oxidation was studied for the treatment of polymerization effluents (PME) from the manufacture of dry-spun acrylic fibers. 5 inorganic and 3 organic flocculants were investigated and the optimal regents and conditons were PAC (at 25°C, pH=8 and a dosage of 150 mg/L), and Z7650 (at 25°C, pH=6 and a dosage of 10 mg/L). Under this condition, the COD was removed by 23.1% of the initial 1824 mg/L. The optimum efficiency of Fenton process was determined at 25°C and pH=4 with a reaction time of 90 min. The dosage of H2O2 and the rate of c(H2O2)/c(FeSO4) were respectively 0.53 mol/L and 20:1. Finally, the removal of COD, total nitrogen, ammonia, SO32- and turbidity by the combined process were 64.0%, 99.3%, 99.6%, 99.7% and 89.4% respectively. BOD/COD was also improved from 0.09 to 0.25.