Acid mine drainage (AMD) is a widespread environmental problem associated with coal mining, characterized by water with high acidity and metal content. This study investigates the potential of fly ash, a coal combustion by-product, as a treatment agent for AMD. Our objectives were to neutralize AMD acidity, measure pH, electrical conductivity (EC), oxidation-reduction potential (ORP), and sulfate concentrations, and characterize the properties of fly ash before and after treatment. We conducted batch experiments, treating AMD with varying doses of fly ash and monitoring the physicochemical parameters over time. The results showed a significant increase in pH, from acidic to near-neutral levels, upon treatment with fly ash. Concurrently, EC and ORP measurements indicated a reduction in soluble metal ions, and sulfate concentrations decreased, suggesting precipitation of metal sulfates. The characterization of fly ash before and after treatment using FTIR, scanning electron microscopy (SEM), and X-ray diffraction (XRD) revealed changes in its mineralogical and morphological features, evidencing its reactivity and metal-binding capacity. The findings confirm that fly ash can effectively remediate AMD, providing insights into its role in immobilizing contaminants. The study underscores the potential of fly ash to improve water quality in mine-affected areas and recommends further research to optimize application methods for environmental rehabilitation.