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A high-sensitivity electrochemical sensor for heavy metal ions (HMIs) was prepared by associating Ti3C2Txwith protonated carbon nitride (H–C3N4/Ti3C2Tx). Due to the electrostatic interaction, massive H–C3N4was distributed on the surface of Ti3C2Txand served as coating material. H–C3N4/Ti3C2Txcomposite showed great conductivity derived from Ti3C2Tx, and H-C3N4was with abundant electroactive deposition sites for the deposition of HMIs. In addition, the stability of H–C3N4/Ti3C2Txcomposite was enhanced due to the protective H–C3N4coating. The H–C3N4/Ti3C2Txelectrode exhibited remarkable sensitivities for the simultaneous detection of Cd2+(0.05 ∼ 1.50 μM) and Pb2+(0.05 ∼ 1.50 μM) and the detection limit of Cd2+and Pb2+were 0.001 and 0.0006μM, respectively. Notably, sensor based on H–C3N4/Ti3C2Txcomposite showed excellent selectivity for Cd2+and Pb2+in the presence of interfere ions and molecules (K+, Na+, Ca2+, Hg2+, Cr2+, Cu2+, Cl−, NO3−, PO4−, ascorbic acid, uric acid, acetaminophen, glucose and nicotinamide). Besides that, distinguished stability and reproductivity of H–C3N4/Ti3C2Txelectrode indicate that this sensor is promising for HMIs in wastewater and other commercial applications.