A Co-B-based catalyst was prepared under microwave irradiation for hydrogen generation by hydrolysis of NaBH4 solution. The activity of Co-B catalyst for hydrogen generation was studied in comparison with another Co-B catalyst prepared by the known methods. The results show that Co-B catalyst reduced prepared under microwave irradiation was quick and was completed in only 17 min, while the Co-B catalyst produced in a known method was slow and was completed in 27 min. The hydrogen generation from the hydrolys of NaBH4 with Co-B catalyst was investigated depending on NaBH4 and NaOH concentrations in solution, temperature, microwave applying time, and microwave applying power. Hydrolysis kinetics of NaBH4 were investigated at a temperature range of 30-50 degrees C and zero-order kinetics were applied to the obtained data.