This study addresses the challenge of removing Congo red (CR) from aqueous solutions using activated carbon (AC) derived from macadamia nutshells (MNS). A unique two-step carbonization and pyrolysis process was employed to produce MNS-AC with high surface area and porosity. Key experimental variables, including initial CR concentration, contact time, and pH, were systematically varied in batch mode. Results indicated that the modified AC achieved significantly higher removal percentages compared to unmodified charcoal. At pH 2.0 and an initial dye concentration of 50 mg L−1, CR removal reached 97.48 % for MNS-AC3. The maximum adsorption capacity (qmax) of 58.29 mg g−1 was observed at an initial dye concentration of 200 mg L−1. The pseudo-second-order kinetic model closely matched the experimental data, and equilibrium data analysis using Langmuir and Dubinin-Radushkevich (D-R) isotherm models provided excellent fits. This research demonstrates the potential of using industrial biomass waste to develop sustainable solutions for dye removal in wastewater treatment.