This study focuses on establishing the kinetic parameters for the catalytic dehydrogenation process of NaBH4. This reaction occurs in the presence of a co-catalyst derived from metallic sources of Co and Ni. For this purpose, a heterogeneous catalyst was synthesized using metal-organic frameworks (MOFs) as the supporting material. CoF2 and NiF2 for cobalt and nickel were the active metal sources, respectively. Metal organic framework (MOF), MIL-101 (Cr), was chosen because it has a larger specific surface area than other materials (2504 m2g-1). The reaction rate constants and rate order were calculated via the differential method. As a result, zero-order kinetics was proved by using the experimental data. After that, the activation energy was calculated as 51.06 kJ/mol through the slope of the graph of lnk versus 1/T for the hydrolysis reaction. The dehydrogenation index of NaBH4 was calculated as 2150 mL H2/g NaBH4 according to the amount of NaBH4 in the aqueous solution. There is no doubt MOFs are promising novel materials synthesized for various aims. Here, we tried to indicate its different usage areas in catalytic reactions.