The impact of Ni nanoparticles (NPs) and Ni-graphene nanocomposite (Ni-Gr NC) on hydrogen production from industrial wastewater containing mono-ethylene glycol (MEG) via anaerobic digestion was investigated. Batch reactors were supplemented with different dosages of Ni NPs and Ni-Gr NC ranging from 0 to 100mg/L. Maximum hydrogen yields (HYs) of 24.73±1.12 and 41.28±1.69mL/gCODinitial were achieved at a dosage of 60mg/L for Ni NPs and Ni-Gr NC, respectively. Substantial improvements of 23% and 105% in hydrogen production were registered at an optimum dosage of 60mg/L for Ni NPs and Ni-Gr NC, respectively, compared with the control without nanomaterials addition. However, increasing the dosage of Ni NPs and Ni-Gr NC to 100mg/L resulted in a significant decrease in HY to 20.80±1.12 and 24.24±1.13mL/gCODinitial, respectively. A non-linear regression model revealed that the higher maximum hydrogen production (129% improvement) could be achieved at a dosage of 50mg/L Ni-Gr NC and an initial pH of 5.0. Economic and environmental revenues due to bioenergy recovery from MEG-containing wastewater were also estimated.