ABSTRACT Initially, the carboxylated-acryl amido propane sulfonic acid (C-AMPSA) was synthesized through the thiol-ene reaction using 2-acrylamido-2-methylpropane sulfonic acid and 3-mercapto propane sulfonic acid monomers. The C-AMPSA was cross-linked with polyvinyl alcohol to create a non-perfluorinated membranes were of these acid group-containing monomers. Using a cross-linking technique, a poly vinyl alcohol cross-linked C-AMPSA (PVA-C-AMPSA) polymer was prepared. Following that, the MoS2 nanosheets (NSs) were synthesized through the one-pot hydrothermal method, and their phase purity, functionality, and morphology were evaluated by p-XRD, FT-IR, and FE-SEM analyses. These nanosheets were then incorporated into PVA-C-AMPSA polymer nanocomposite membranes at various concentrations (0%, 1%, 2%, 3%, and 5% by weight). In addition, the physicochemical properties of bare and MoS2 nanosheets incorporated PVA-C-AMPSA polymer nanocomposite membranes were assessed, including water uptake, swelling ratio, and ion-exchange capacity. Remarkably, the membrane with 5% of MoS2 NSs in PVA-C-AMPSA displayed an ion-exchange capacity of 1.13 mmol g−1 and a proton conduction of 1.8 × 10−3 S cm−1 at 110°C. The Arrhenius plot indicated that the proton transport was involved in both Grotthuss and vehicular mechanisms. In the fuel cell testing, the PVA-C-AMPSA polymer nanocomposite membrane containing MoS2 NSs demonstrated superior performance, achieving a peak power density (PD) exceeding 0.7 W cm−2 and an open-circuit voltage (OCV) surpassing 0.93 V at 110°C. In contrast, the pure PVA-C-AMPSA membrane exhibited a peak PD of over 0.4 W cm−2 and an OCV of around 0.6 V at the same temperature. Additionally, the 5% of MoS2 NSs incorporated PVA-C-AMPSA polymer nanocomposite membrane exhibited outstanding oxidative stability with 87.7% of degradation when exhibited to a Fenton reagent at 80°C for 8 h.