<p>The generation of hydrogen gas through the catalytic hydrolysis of sodium borohydride (NaBH₄) has garnered significant interest in recent years. The primary research challenge remains the development of effective and reusable catalysts. This research details the development of Co/MnFe₂O₄ catalysts aimed at facilitating the hydrolysis of sodium borohydride (NaBH₄), employing MnFe₂O₄ as the support material. The support was synthesized through a co-precipitation method, while the catalysts were produced via an impregnation-chemical reduction technique. The characterization of the catalysts was performed using X-ray diffraction, field emission scanning electron microscopy, X-ray fluorescence, vibrating sample magnetometry, and nitrogen adsorption–desorption measurements. The study initially explored the effects of calcination temperature of the supports and the amount of loaded cobalt on the hydrogen generation process. Notably, catalysts supported on MnFe₂O₄ calcined at 400&#xa0;°C demonstrated greater activity, with 30% Co/MF-400 catalyst yielding 3533&#xa0;mL.min⁻¹.g_cat⁻¹of hydrogen during NaBH₄ hydrolysis. The enhanced catalytic performance of the MF-400 supported catalysts was attributed to their small crystallite size or prominent number of defects and high magnetic properties. In addition, 30Co-MF400 showed high specific surface area of 120.1 m².g⁻¹. Subsequently, various parameters were examined over 30Co/MF-400, including catalyst dosage (10–25&#xa0;mg), concentrations of NaOH (1–7 wt.%), temperature (25–45&#xa0;°C), and catalyst reusability. The activation energy (E_a) for the 30% Co/MF-400 catalyst was found to be 27.1&#xa0;kJ/mol, as determined through the application of the rate expression and the Arrhenius equation. The 30% Co/MF-400 catalyst showed a 44% decline in catalytic performance after being used for four cycles.</p>