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A low-cost adsorbent was prepared from activated orange peels (AOP). The AOP was characterized and evaluated as an adequate adsorbent for methyl violet (MV) and methylene blue (MB) removal from single and binary systems. The adsorbent dose, initial concentration, pH, and temperature are the parameters examined for adsorption. First, a preliminary study was conducted in order to determine the experimental domain. A full-factor design was performed to ascertain the impact of the investigated factors and their interplay on the adsorption process. To anticipate the values of the response at any point within the experimental zone and to obtain the optimum conditions the response surface methodology according Doelhert was established. Then regeneration was achieved to highlight the ability of the preloaded biosorbent to release dyes and to be reused. As an alternative to industrial wastewater, laboratory waste was used for simultaneous cationic dye removal on AOP. It is possible to consider AOP as a suitable wastewater treatment method.