A hydrazone-linked COF (DvDf-C3XJ-COF) with hydrogen-bond reinforcement and abundant coordination sites was synthesized, exhibiting strong fluorescence and high sensitivity/selectivity for Hg2+ detection, with a detection limit of 1.65 × 10-6 M. The fluorescence quenching for Hg2+ is attributed to coordination interactions, which occur through a dynamic quenching process.