Properties of NaBH4 hydrolysis reaction using Co-P-B/FeCrAlloy catalyst and the catalyst durability were studied. Co-P-B/FeCrAlloy catalyst showed low activation energy such as 25.2 kJ/mol in 5 wt% NaBH4 solution, which was similar that of noble metal catalyst. The activation energy increased as the NaBH4 concentration increased. Formation of gel at high concentration of NaBH4 seriously affected hydrogen evolution rate and the catalyst durability. The catalyst loss decreased as reaction temperature increased due to lower gel formation when the concentration of NaBH4 was over 20 wt%. Considering hydrogen generation rate and durability of catalyst, the catalyst supported with FeCrAlloy heat-treated at 1000 ℃ without ultra vibration during dipping and calcination after catalyst dipping was best catalyst. To use catalyst more than three times in 25 wt% NaBH4 solution, it should be reacted at higher temperature than 60 ℃.