The synthesis and characterization of ZnO/Kaolin nanocomposites for adsorption processes, particularly in bleaching palm oil, have been comprehensively investigated. Various techniques including X-ray diffraction (XRD), scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) and BET analysis were employed to characterize the nanocomposites. The results indicate successful synthesis and activation of ZnO/Kaolin nanocomposites, with notable changes in structural, morphological, and chemical properties compared to raw materials. The adsorption capacity of the nanocomposites, evaluated through iodine value determination as a response parameter, revealed significant variations based on calcination temperature, time, and kaolin-ZnO ratios. Statistical analysis using ANOVA and Design of Experiment (DOE) highlighted the significance of these factors in optimizing adsorption efficiency.