A novel RHA/PFA/CFA composite adsorbent was synthesized from rice husk ash (RHA), palm oil fuel ash (PFA), and coal fly ash (CFA) by modified sol-gel method. Effect of different parameters such as adsorbent dosage, contact time, and pH were studied using batch experiment to optimize the maximum zinc (Zn2+) and nickel (Ni2) adsorption conditions. Results showed that the maximum adsorption condition occurred at adsorbent amount of 10 g/L, contact time of 60 min, and pH 7. At this condition, the removal efficiencies were 81% and 61% for Zn2+ and Ni2+, in which the adsorption capacities (qmax) were 21.74 mg/g and 17.85 mg/g, respectively. Adsorption behavior of RHA/PFA/CFA composite adsorbent was studied through the various isotherm models at different adsorbent amounts. The results indicated that the Freundlich isotherm model gave an excellent agreement with the experimental conditions. Based on the results obtained from the kinetic studies, pseudo-second-order was suitable for the adsorption of Ni2+ and Zn2+, compared to the pseudo-first-order model. The results presented in this study showed that RHA/PFA/CFA composite adsorbent successfully adsorbed Zn2+ and Ni2.