In this study, organic waste sources (spent coffee ground (SCG)) is used as metal-free catalyst in comparison with conventional noble-metal catalyst materials for hydrogen generation based on the methanolysis of sodium borohydride solution. Spent coffee ground (SCG) is used as a metal-free catalyst for the first time as treated with different chemicals. The aim is to synthesize the metal-free catalyst that can be used for the production of hydrogen, a renewable energy source. SCG, which was collected from coffee shops, was used for preparing the catalyst. To produce hydrogen by sodium borohydride (NaBH4) methanolysis, SCG is pretreated with different chemical agents (H3PO4, KOH, ZnCl2). According to the acid performances, the choice of phosphoric acid was evaluated at different mixing ratios (10%, 20%, 30%, 40%, 50%, 100%) (w/w), different temperatures (200, 300 and 400 degrees C) and burning times (30, 45, 60 and 90 min) for the optimization of SCG-catalyst. A detailed characterization of the samples were carried out with the aid of FTIR, SEM, XRD and BET analysis. In this study, the experiments were generally carried out effectively under ambient temperature conditions in10 ml methanol solution containing 0.025 g NaBH4 and 0.1 g of the catalyst. The hydrogen obtained in the experimental studies was determined volumetrically by the gas measurement system. When evaluating the hydrogen volume, different NaBH4 concentrations, catalyst amount and different temperature effects were investigated. The effect of the amount of NaBH4 was investigated with 1%, 2.5%, 5%, and 7.5% ratio of NaBH4 while the influence of the concentration of catalyst was carried-out at 0.05, 0.1, 0.15, and 0.25 g catalysts. Four different temperatures were tested (20, 30, 40, 50 and 60 degrees C) to explore the performance of the catalyst under different temperatures. The experiments by using SCG-catalyst treated with H3PO4 reveal that the best acid ratio was 100% H3PO4. The maximum hydrogen production rate with the use of SCG-catalyst for the methanolysis of NaBH(4 )was found to be 8335.5 mL min(-1) gcat(-1). Also, the activation energy was determined to be 9.81 kJ mol(-1). Moreover, it was discovered that there was no decline in the percentage of converted catalyst material. (C) 2019 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.