AbstractThe study intended to devise a sustainable treatment scheme for acrylic fiber dyeing process effluents, which significantly differ from other textile plant wastewaters. The necessary experimental support was generated from a set of tests conducted on the wastewater of a plant operation, focused solely on acrylic fiber dyeing. Related experiments involved effluent characterization, biological treatability, and chemical settling/oxidation performed on raw and bio‐treated effluent, as pre‐treatment and/or polishing steps. A total COD level of 910 mg/L with a 70% soluble ratio, low total N and P contents below 10 mg/L, a detergent content of 50 mg/L and a dark/black color of 1150 Pt‐Co unit defined the average properties of the raw plant effluent. Experimental support indicated that activated sludge operation at a sludge age level above 25 d, remained insufficient as it could only provide an effluent with a soluble COD level above 150 mg/L, a biomass escape in the range of 40 to 100 mg/L and with an intense dark color. A similar experimental template, including chemical settling, chemical oxidation by NaOCl and combination of the two processes, was tested as pre‐treatment and a polishing step after biological treatment. Pre‐treatment, although with some benefit to remove toxic and inhibitory compounds, proved to be highly costly, due to excessive chemical usage and sludge generation for a sustainable, cost‐effective approach. The sequence of chemical oxidation and settling steps implemented as a polishing stage was quite effective as it secured complete color removal, a major source of concern for the selected wastewater and also, it reduced COD down to 60 mg/L, a level significantly below the residual COD threshold for biological treatment. This approach, although case‐specific for this study, provided a scientific and general perspective for similar work.