Two-dimensional (2D) transition metal carbides and nitrides (MXenes) have drawn considerable attention for application in the field of environmental remediation. In this study, we report the simultaneous reductive–adsorption behavior of Ti3CNTx for toxic metal ion Hg2+ ion in the aqueous phase. 2D Ti3CNTx and Ti3C2Tx MXene nanosheets were synthesized by exfoliation of Ti3AlCN and Ti3AlC2 MAX phases, respectively. Various characteristics analysis confirmed the successful fabrication of MAX phases and their exfoliation into MXenes. The fabricated MXene nanosheets were used to investigate their Hg2+ removal, Hg2+ intercalation, and surface interaction mechanism efficiencies. Both MXenes were found to adsorb and reduce a large amount of Hg2+. Analytical techniques such as X-ray powder diffraction, field emission transmission electron microscopy, zeta-potential analyses, and X-ray photoelectron spectroscopy were used to investigate the material characteristics and structural changes after uptake of Hg2+. The quantitative investigation confirmed the interaction of bimetal and hydroxyl groups with Hg2+ using electrostatic interactions and adsorption-coupled reduction. In addition, both MXenes exhibited extraordinary Hg ion removal capabilities in terms of fast kinetics with an excellent distribution coefficient (KdHg) up to 1.36 × 10+9. Based on batch adsorption results, Ti3C2Tx and Ti3CNTx exhibited removal capacities of 5473.13 and 4606.04 mg/g, respectively, for Hg2+, which are higher than those of previous Hg adsorbents.