The central composite rotatable design (CCD) of response surface methodology (RSM) was used to optimize aluminum dispersed bamboo activated carbon preparation. The independent variables selected for optimization are activating agent (AlCl3) concentration (mol/L), activation temperature (°C), and activation time (min.). The independent variable's response change was observed through the percentage adsorption efficiency of Ciprofloxacin hydrochloride (CIP) antibiotics. The maximum CIP adsorption efficiency was found to be 93.6 ± 0.36% (13.36 mg/g) for the adsorbent prepared at AlCl3 concentration 2.0 mol/L, activation temperature 900 °C, and activation time 120 min. The adsorption efficiency was recorded at the natural pH (7.9) of the adsorbent (3 g/L)-adsorbate (50 mL solution of 50 ppm) mixture. The Al-dispersed bamboo activated carbon was characterized for its surface morphology, surface elemental compositions, molecular crystallinity, surface area, pore morphology, and surface functional groups. The mechanism of adsorbent surface formation and CIP adsorption sites were explored. The characterization data and mechanism study will help in deciding possible future applications in other fields of study.