At present, carbon nanotube supported monometallic Ru at 3 wt% Ru loading (3% Ru/CNT) per gram support and bimetallic RuMo at 3 wt% Ru loading per gram support (3% Ru-Mo/CNT) at varying Ru:Mo atomic ratios are synthesized via sodium borohydride (NaBH4) reduction method to investigate their performance towards NaBH4 hydrolysis. These monometallic Ru/CNT and bimetallic Ru:Mo/CNT catalysts prepared at varying Ru:Mo atomic ratios are characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX), and transmission electron microscopy (TEM). Characterization results reveal that Mo addition to Ru alters the electronic state of the catalysts. The NaOH concentration, the amount of catalyst, the NaBH4 concentration and the temperature parameters that affect the hydrolysis rate of this synthesized and developed catalyst were examined. The kinetic calculations of these parameters related to the order of the reaction were determined. Under optimum conditions catalyst hydrogen production rate was found to be 82,758.43 ml H-2 g(cat)(-1) min(-1). The reaction order (n) and activation energy (E-a) are determined as 0.42 and 35.11 kJ mol(-1). Ru:Mo/CNT catalyst is a novel and promising catalyst for hydrogen generation from NaBH4.