In this study, a Co/MMT catalyst was synthesized by pillaring method using montmorillonite (MMT) as a support material for hydrogen production by hydrolysis reaction from sodium borohydride (NaBH4) solution. N2 sorption, XRD, SEM-EDS, and FTIR spectroscopy techniques were used for catalyst characterization. To optimize the amount of hydrogen obtained as a result of the hydrolysis reaction, the NaBH4 concentration (0.3-0.5 M), the sodium hydroxide (NaOH) concentration (0.3-0.5 M), the amount of catalyst (20-50 mg) and the reaction temperature (30-50 C-degrees) were investigated. The optimal conditions obtained from the Box-Behnken analysis were 50 C-degrees, 0.33 M NaBH4, 39 mg catalyst, 0.46 M NaOH, and the maximum reaction rate (hydrogen production) was 2328 mL min( -1) gcat (-1 )at standard temperature and pressure (298K,1atm). According to the analysis of variance, it was found that all parameters had a significant effect on the hydrogen production rate.