Fabrication of composite adsorbents with exceptional fluorescence performance has attracted increasing attention. In this study, a nitrogen-doped graphene quantum dots (NGQDs)/poly(vinyl alcohol) (PVA) composite membrane (NGQDs-PVA) with high adsorption selectivity and fluorescence quenching for Ag + was prepared via simple cross-linking. The SEM characterization showed that the NGQDs were uniformly distributed in PVA, indicating that the material exhibited fluorescence characteristics of quantum dots. C−O, −COOH, −NH 2 , and −OH functional groups in NGQDs-PVA complexed with a great amount of Ag + , and −NH− reduced a small amount of Ag + to Ag 0 . The pseudo-firstorder kinetic and Langmuir models were used to describe the adsorption process of heavy metals using the composite. The maximum adsorption capacity was 317.35 mg/g (Langmuir model fitting, pH = 4, T = 40 °C). When the fluorescence of NGQDs-PVA was quenched as the number of Ag + adsorbed increased, the change in fluorescence intensity was used to qualitatively quantify the adsorption process.