This study successfully applied Fenton-Neutralization process (F–N) for the treatment of industrial textile wastewater polluted with highly concentrated acid black 194 dye. At optimal operating conditions (F: [Fe2+]0 = 834 mg/L, [H2O2]0 = 6078 mg/L, pH0 = 2.0; and N: [Slaked lime] = 2.05 g/L), determined using a D-optimal design of experiments, response surface methodology and multi-objective optimization analysis, the F–N allowed almost total decolorization, COD and TOC removals of 89% and 75%, respectively, with a total operating cost of 10.55 USD/m3. Thus, F–N can be considered as an environmentally and economically friendly, efficient, easy to implement and manipulate alternative for the treatment of textile industrial wastewater.