A mesoporous Zr-G-Csub.3Nsub.4 nanomaterial was synthesized by a succinct-step ultrasonication technique and used for Cusup.2+ ion uptake in the aqueous phase. The adsorption of Cusup.2+ was examined by varying the operating parameters, including the initial metal concentration, contact time, and pH value. Zr-G-Csub.3Nsub.4 nanosorbent displays graphitic carbon nitride (g-Csub.3Nsub.4) and ZrOsub.2 peaks with a crystalline size of ~14 nm, as determined by XRD analysis. The Zr-G-Csub.3Nsub.4 sorbent demonstrated a BET-specific surface area of 95.685 msup.2/g and a pore volume of 2.16 × 10sup.−7 msup.3·gsup.−1. Batch mode tests revealed that removing Cu (II) ions by the mesoporous Zr-G-Csub.3Nsub.4 was pH-dependent, with maximal removal achieved at pH = 5. The adsorptive Cusup.2+ ion process by the mesoporous nanomaterial surface is well described by the Langmuir isotherm and pseudo-second-order kinetics model. The maximum adsorption capacity of the nanocomposite was determined to be 2.262 mol·kgsup.−1 for a contact time of 48 min. The results confirmed that the fabricated mesoporous Zr-G-Csub.3Nsub.4 nanomaterial is effective and regenerable for removing Cusup.2+ and could be a potent adsorbent of heavy metals from aqueous systems.