MXenes are promising candidates for the removal of pollutants from aqueous solutions. Their application, however, is restricted by the lack of surface-active sites. This study examined the effect of NZVI intercalated MXene on the removal of polycyclic aromatic hydrocarbons from wastewater. XPS spectra, FTIR analysis, SEM images, and N2 adsorption-desorption isotherms characterizations indicated that the functional groups on the MXene surface aided in the introduction and stabilization of NZVI into the inter-layer and surface of MXene. The adsorption parameters (pH, dosage and contact time) were optimized using response surface methodology (RSM) in design expert software. The optimum operating conditions for the removal of naphthalene, fluorene and phenanthrene using NZVI intercalated MXene (named N-MXene-3) were pH of 3, dosage of 101.5 mg/L and contact time of 40.5 min. The use of synthesized N-MXene-3 to extract naphthalene, fluorene, and phenanthrene from oil and gas industry wastewater samples validates the usefulness of the proposed method in testing actual wastewater samples. Over 80 of the three polycyclic aromatic hydrocarbons in wastewater were removed by the adsorbent. N-MXene-3 was shown to be an effective, and promising material for wastewater treatment. © 2024 Elsevier Ltd