The ubiquity of diclofenac (DCF) in the environment has raised significant concerns. Diclofenac is a non-steroidal anti-inflammatory drug that has been found in various environmental matrices at minimum concentrations that are harmful to aquatic and terrestrial organisms. Traditional wastewater treatment plants (WWTPs) are not fully equipped to remove a range of pharmaceuticals, and that explains the continued ubiquity of DCF in surface waters. In this study, an Fe
3O
4/SiO
2 nanocomposite prepared from acid mine drainage and coal fly ash was applied for the removal of DCF from wastewater. Major functional groups (Si–O–Si and Fe–O) were discovered from FTIR. TEM revealed uniform SiO
2 nanoparticle rod-like structures with embedded dark spherical nanoparticles. SEM-EDS analysis discovered a sponge-like structure fused with Fe
3O
4 nanoparticles that had significant Si, O, and Fe content. XRD demonstrated the crystalline nature of the nanocomposite. The surface properties of the nanocomposite were evaluated using BET and were 67.8 m
2/g, 0.39 cm
3/g, and 23.2 nm for surface area, pore volume, and pore size, respectively. Parameters that were suspected to be affecting the removal process were evaluated, including pH, nanocomposite dosage, and sample volume. The detection of DCF was conducted on high-performance liquid chromatography with diode-array detection (HPLC-DAD). Under optimum conditions, the adsorption process was monolayer, and physisorption was described using the Langmuir and Dubinin-Radushkevich (D-R) isotherm models. The kinetic data best fitted the pseudo-first order kinetic model, indicating a physisorption adsorption process. The thermodynamic experimental data confirmed that the adsorption process was spontaneous. The results obtained from real water samples showed 95.28% and 97.44% removal efficiencies from influent and effluent: 94.83% and 88.61% from raw sewage and final sewage, respectively. Overall, this work demonstrated that an Fe
3O
4/SiO
2 nanocomposite could be successfully prepared from coal fly ash and acid mine drainage and could be used to remove DCF in wastewater.
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