Efficient, low-cost and safe new systems are still needed for the storage and usage of hydrogen energy, which is considered the most important energy source of the future. For this reason, the aim of this study was to prepare Co-0, Ni-0, and Cu-0 composite catalysts with fly ash (FA) formed by combustion of coal in thermal power plants to be used for the dehydrogenation of ethylenediamine bisborane (EDAB) as a hydrogen source. In the hydrolysis reactions of EDAB, parameters such as metal type, catalyst concentration, temperature, and EDAB concentration were investigated. The FA-Cu-0 composite catalyst was determined to be an effective catalyst system for hydrogen production by hydrolysis of EDAB from among the FA-M-0 composite catalysts. Besides, FA can be used as an effective support material in order to prevent agglomeration of metal particles. (C) 2020 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.