Gas-To-Liquid (GTL) processing involves the conversion of natural gas to liquid hydrocarbons that are widely used in the chemical industry. In this process, the Fischer−Tropsch (F-T) approach is utilized and, as a result, wastewater is produced as a by-product. This wastewater commonly contains alcohols and acids as contaminants. Prior to discharge, the treatment of this wastewater is essential, and biological treatment is the common approach. However, this approach is not cost effective and poses various waste-related issues. Due to this, there is a need for a cost-effective treatment method. This study evaluated the adsorption performance of activated carbon fibers (ACFs) for the treatment of GTL wastewater. The ACF in this study exhibited a surface area of 1232.2 m2/g, which provided a significant area for the adsorption to take place. Response surface methodology (RSM) under central composite design was used to assess the effect of GTL wastewater’s pH, initial concentration and dosage on the ACF adsorption performance and optimize its uptake capacity. It was observed that ACF was vitally affected by the three studied factors (pH, initial concentration and dosage), where optimum conditions were found to be at a pH of 3, 1673 mg/L initial concentration and 0.03 g of dosage, with an optimum uptake of 250 mg/L. Kinetics and isotherm models were utilized to fit the adsorption data. From this analysis, it was found that adsorption was best described using the pseudo-second order and Freundlich models, respectively. The resilience of ACF was shown in this study through conducting a regeneration analysis, as the results showed high regeneration efficiency (~86%) under acidic conditions. The results obtained from this study show the potential of using ACF under acidic conditions for the treatment of industrial GTL wastewater.