Photocatalytic degradation is one of the environmentally friendly methods used in treat-ing dye wastewater. In this study, a series of MXene/g-C3N4 heterostructure photocatalysts with different loading amounts of MXene (1, 4, 8, and 12 wt.) were successfully synthesized via the wet impregnation method and their photocatalytic activity was evaluated via the degradation of methylene blue under visible-light irradiation. As such, the 1 wt. MXene/g-C3N4 heterostructure photocatalyst achieved a high degradation of methylene blue compared to the pure g-C3N4 under visible-light illumination of 180 min. This significant improvement was attributed to the intimate interfacial contact, evidently from the FESEM analysis, which allows the smooth photocharge carriers to transport between g-C3N4 and MXene. Additionally, the larger BET surface area demonstrated by the 1 wt. MXene/g-C3N4 heterostructure allowed this sample to have higher adsorption of dye molecules and provided a higher number of reactive sites, which was beneficial for the enhancement of the photocatalytic activity. Nevertheless, it was found that the excessive loading of MXene can substantially impede photocatalytic activity. This was attributed to the decrease in the active sites, as well as the weakened crystallinity of the MXene/g-C3N4 heterostructure photocatalyst, evident from the FTIR and XRD analysis. All in all, this study has shown the potential of the MXene/g-C3N4 photocatalyst as a promising photocatalyst for highly efficient wastewater treatment applications. © 2022 by the authors. Licensee MDPI, Basel, Switzerland.