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Metallic Co NPs@poly(vinylidene fluoride-co- hexafluoropropylene) nanofibers (PVFH NFs) were successfully synthesized with the help of electrospinning and in situ reduction of Co²⁺ ions onto the surface of PVFH membrane. Synthesis of PVFH NFs containing 10, 20, 30, and 40 wt% of cobalt acetate tetrahydrate was achieved. Physiochemical techniques were used to confirm the formation of metallic Co@PVFH NFs. High catalytic activity of Co@PVFH NFs in the dehydrogenation sodium borohydride (SBH) was demonstrated. The formulation with 40 wt% Co proved to have the greatest performance in comparison to the others. Using 1 mmol of SBH and 100 mg of Co@PVFH NFs, 110 mL of H₂ was produced in 19 min at a temperature of 25 °C, but only 56, 73, and 89 mL were produced using 10, 20, and 30 wt% Co, respectively. With the rise of catalyst concentration and reaction temperature, the amount of hydrogen generated increased. By raising the temperature from 25 to 55 °C, the activation energy was lowered to be 35.21 kJ mol⁻¹ and the yield of H₂ generation was raised to 100% in only 6 min. The kinetic study demonstrated that the reaction was pseudo-first order in terms of the amount of catalyst utilized and pseudo-zero order in terms of the SBH concentration. In addition, after six cycles of hydrolysis, the catalyst showed outstanding stability. The suggested catalyst has potential applications in H₂ generation through hydrolysis of sodium borohydride due to its high catalytic activity and flexibility of recycling. Full article