Heavy metal contamination in water is a serious environmental issue due to the toxicity of metals like lead. This study developed zeolite and multi-walled carbon nanotube (MWCNT) incorporated polyacrylonitrile (PAN) nanofibers via needleless electrospinning and examined their potential for lead ion adsorption from aqueous solutions. The adsorption process was optimized using response surface methodology (RSM) and artificial neural network (ANN) modeling approaches. The adsorbent displayed efficient lead removal of 84.75% under optimum conditions (adsorbent dose (2.21 g), adsorption time (207 min), temperature (48 °C), and initial concentration (62 ppm)). Kinetic studies revealed that the adsorption followed pseudo-first-order kinetics governed by interparticle diffusion. Isotherm analysis indicated Langmuir monolayer adsorption with improved 5.90 mg g⁻¹ capacity compared to pristine PAN nanofibers. Thermodynamic parameters suggested the adsorption was spontaneous and endothermic. This work demonstrates the promise of electrospun zeolite/MWCNT nanofibers as adsorbents for removing lead from wastewater.