In this work, methanol was used as an alternative to water. Our objective is to study the influence of the using of methanol instead of water in the preparation of Co-B-TiO2 catalyst. It is also expected to improve the activity of Co-B-TiO2 catalyst by plasma treatment for the hydrogen generation from hydrolysis of NaBH4. The prepared catalysts were characterized using BET (N-2 adsorption), SEM (scanning electron microscopy), XRD (X-ray diffraction) and FTIR (Fourier transform infrared) methods. The Co-B-TiO2 catalyst prepared in methanol shows maximum hydrogen generation rate, which is about 3.0 times higher than that obtained for Co-B-TiO2 catalyst prepared in water. The maximum hydrogen generation rates for the Co-B-TiO2 catalysts prepared in water and methanol were 1017 and 3031 mL/min/g, respectively. In addition, the maximum hydrogen generation rates for the plasma treated Co-B-TiO2 catalysts prepared in water and methanol were 1320 and 2656 mL/min/g, respectively. The activation energies of nth-order reaction model for the hydrogen production from hydrolysis of NaBH4 with the plasma treated Co-B/TiO2 catalyst prepared in methanol and Co-B/TiO2 catalyst prepared in methanol can be obtained from the slope and intercept of the regression line, being 41.29 and 36.24 kJ/mol, respectively. Copyright (C) 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.