The pollution of underground and surface water streams is a tremendous environmental problem. Adsorption, in which activated carbon (AC) is used as an adsorbent, is one of efficient procedures to remove organic and inorganic pollutants from industrial wastewaters. Activated carbon fiber (ACF), a newly developed form of AC, has high adsorption rate and surface area and can be used for the treatment of industrial wastewaters. In this work, ACF was prepared by physicochemical activation method from kenaf and we studied its ability in the treatment of indigo-containing wastewater produced from a dying factory. The filtered wastewater was treated via adsorption by ACF, and response surface experimental design method was used to study the effect of ACF dosage, contact time, temperature, and pH of the wastewater on the removal process. ACF dosage of 0.256 g, temperature of 12.5°C, pH 8.5, and contact time of 125 min were optimum treatment conditions. The adsorption process obeys pseudo-second-order kinetic and Freundlich isotherm models.