Many industries use huge amounts of synthetic dyes which may release into the wastewater in dyeing processes causing serious damage to aquatic life as they are recalcitrant, nonbiodegradable, stable to oxidizing agents, and toxic. Adsorption on activated carbon has been found to be a very efficient treatment method. In this work, a new adsorbent material composed of activated carbon and aluminum chloride (AC-Al) was prepared for the removal of a commercial anionic and anthraquinonic reactive dye, i.e., Reactive Black 5 (RB5) under various experimental conditions. Several parameters, such as the adsorbent’s dosage, initial RB5 concentration, pH, and contact time, were studied in order to determine the feasibility of AC-Al. According to the results, it was found that there was an increase in RB5 removal as the adsorbent’s dosage increased, especially, in pH 2 ± 0.1, where the removal rate increased, and reaching 100% by 1.0 g/L of AC-Al. Freundlich isotherm and pseudo-second-order kinetic models adequately fit the experimental data, indicating that favorable and heterogeneous adsorption occurred, closer to chemisorption. According to thermodynamics, it was found that the adsorption procedure was endothermic in nature (∆H0 = 62.621 kJ/mol) and spontaneous (∆G0 < 0), and according to the positive value of ∆S0 0.0293 (kJ/mol∙K), there is an increase in random interaction between solid and liquid interfaces. Finally, the AC-Al adsorbent was successfully regenerated and reused for four cycles.