Co/Al2O3 nanopowder was used as a catalyst to investigate the effect of catalyst support, reduction temperature, sodium borohydride (NaBH4) concentration, sodium hydroxide (NaOH) concentration, and reaction temperature on the characteristics of NaBH4 hydrolysis. The Co/Al2O3 nanopowder showed a high catalytic activity among various catalysts. Catalyst reduction at 250℃ exhibited a relatively good activity. The activity decreased with an increase in the NaBH4 concentration. Conversely, the activity increased and then decreased with an increase in the NaOH concentration. Additionally, the activity increased with an increase in the reaction temperature. The value of apparent activation energy was 40.81 kJ/mol, which was lower than the other Co-based catalysts. Thus, Co/Al2O3 nanopowder catalyst can be widely used for NaBH4 hydrolysis owing to its superior catalytic activity.