<p>This study introduces CS NPs–MWCNT@NiFe₂O₄, a novel and recyclable hybrid nanocomposite, as an efficient nanocatalyst for the sustainable synthesis of 1,4-disubstituted 1,2,3-triazoles. The catalyst comprises chitosan nanoparticles (CS NPs) crosslinked and anchored to magnetic multi-walled carbon nanotubes (MWCNTs) decorated with nickel ferrite (NiFe₂O₄). XRD, FT-IR, EDX-Map, TGA-DTA, VSM, and BET techniques were used to identify the structure of the magnetic nanocomposite. This design facilitates a one-pot, three-component reaction utilizing readily available benzyl bromides, sodium azide, and alkynes in water at a mild 50 °C, aligning with green chemistry principles. The magnetic properties of the nanocomposite enable facile separation and reuse of the catalyst. Furthermore, the synergistic effect of integrating chitosan and MWCNTs enhances catalytic activity and stability. Consistently high yields (90–98%) of the desired triazoles were achieved over seven cycles, demonstrating the catalyst’s robustness. These results position CS NPs–MWCNT@NiFe₂O₄ as a promising, eco-friendly, and robust alternative to traditional catalysts in click chemistry applications.</p> Graphical Abstract <p></p>