This study reports for the first time the adsorption capacity of a novel adsorbent Croton bonplandianus Baill. biochar. Its adsorption capacity was further enhanced by loading magnetic composites on it, which makes it an efficient medium for the adsorption of dyes. Two azo dyes, Basic Brown 1 (BB 1 ) and Basic Orange 2 (BO 2 ), were studied for their effective adsorption from aqueous media. A comprehensive characterization was performed by using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) to study the properties of Fe 2 O 3 -loaded C. bonplandianus Baill. biochar (FO-CBPBB). A series of batch experiments were conducted to optimize various parameters (pH, contact time, adsorbent amount, initial BB 1 and BO 2 concentrations, and temperature) for the maximum adsorption of BB 1 and BO 2 on the FO-CBPBB adsorbent. The percentage of BB 1 and BO 2 dyes that adsorb to FO-CBPBB under the best experimental circumstances (pH of solution 7, contact time 80 min, temperature of solution 40 °C, initial BB 1 and BO 2 dye concentrations 80 mg L −1 , and adsorbent dose 1 g L −1 ) was 93 and 95%, respectively. The best adsorption of BB 1 and BO 2 was accomplished by optimizing the effects of several factors, including the starting dye concentration, contact time, and temperature, based on the central composite design. The Freundlich and Langmuir isotherm models were used to examine the equilibrium data. The Langmuir isotherm with the greatest adsorption capacity and R 2 value effectively captured the experimental results. When kinetic parameters were investigated, it was found that pseudo-second-order was appropriate, reflecting the fact that the dye−adsorbent interaction was the rate-controlling factor in this study. The sorption process was endothermic and spontaneous, as shown by the thermodynamic variables. Based on the interaction between the adsorbent and azo dyes, it was concluded that the adsorption process was electrostatic in nature. Adsorbents that have been synthesized can effectively remove azo dyes from wastewater. Excellent regeneration efficiency was exhibited by FO-CBPBB, which makes it an ecofriendly and cost-effective alternative to other costly techniques applied for water purification.