In this work, methanol is used as an alternative to water. Preparation and characterization of Co-Cu-B catalysts in methanol for hydrogen generation from catalytic hydrolysis of sodium borohydride are studied. In addition, the plasma treated Co-Cu-B catalyst prepared in methanol for the hydrogen generation from catalytic hydrolysis of sodium borohydride is investigated. Process parameters including plasma gases, plasma time, NaOH and sodium borohydride concentrations and reaction temperature affecting the hydrolysis reaction of sodium borohydride in the presence of plasma treated Co-Cu-B catalysts are investigated. The maximum hydrogen generation rates of Co-Cu-B catalysts in water and methanol toward sodium borohydride hydrolysis are 734.4 and 3998 mL/g/min, respectively. Cold plasma treated Co-Cu-B catalyst for sodium borohydride hydrolysis is exhibited a hydrogen generation rate of about 4972 mL/g/min. The activation energy of the catalytic hydrolysis reaction of sodium borohydride with the plasma treated Co-Cu-B catalyst for first-order of is found at 17.38 kJ/mol. Copyright (c) 2015, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.