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Co-B catalyst, W-modified Co-B (Co-W-B) catalyst, and Mo-modified Co-W-B (Co-W-Mo-B) catalyst powders were synthesized via chemical reduction of metal salt solutions at room temperature. The optimal hydrogen production rate was obtained when the ratio of the reducing agent (NaBH4) to the metal solution was 4:1. Among the ternary catalysts, the Co0.1-W0.9-B catalyst showed the optimal hydrogen production rate when the content of W doping was 0.9. Furthermore, the hydrogen production rate of the quaternary catalyst was enhanced when the content of Mo doping was 0.075, denoted as Co0.1-W0.9-Mo0.075-B. The catalyst powders were characterized by SEM, XRD, XPS, and BET. The hydrogen production rates of the Co-B catalyst, Co0.1-W0.9-B catalyst, and Co0.1-W0.9-Mo0.075-B catalyst were investigated for the decomposition of alkaline sodium borohydride (NaBH4) in a water–ethanol mixture solution. The Co0.1-W0.9-Mo0.075-B catalyst exhibited the highest hydrogen production rate compared to Co-B and Co0.1-W0.9-B catalyst powders. The optimal hydrogen production rate of the Co0.1-W0.9-Mo0.075-B catalyst is 4600 ml·min−1·g−1, which is nearly 1.9 times higher than that of the Co-B catalyst. Moreover, the Co0.1-W0.9-Mo0.075-B catalyst exhibited good stability, retaining 73% of its catalytic activity after five cycles, and had a low apparent activation energy of 41.51 kJ·mol−1. [ABSTRACT FROM AUTHOR]