Spinning effluents (SE) from dry-spun acrylic fiber manufacturing are hard to degrade due to the containing of vast dimethyl formamide (DMF). Activated carbon, ion exchange and Fenton oxidation were applied to solve this problem. Coconut-shell-based activated carbon exhibited a better performance than the coal-based and nut-shell-based ones did. At the optimal dosage of 1g/L, pH=6 and 30 °C, the removal of COD and DMF were respectively 84.39% and 66.14%. Ion exchange resins are rated as NKA-9 > D301R > D201 > 201×7 respected to the performance, and the optimum COD and DMF removal were 82.31% and 68.76% at the NKA-9 dosage of 0.22 g, pH=7 and 30°C. The most appropriate treatment process appeared to be Fenton. COD and DMF were finally reduced to 23.29 mg/L and 23.43 mg/L, with removal rates of 90.23% and 79.43% respectively. This optimum efficiency was obtained at c(H2O2)/c(Fe2+) of 14:1, pH=3, 50 °C, and an oxidation time of 3 h.