The hydrothermolysis variables temperature (150 -210 °C) and time (10 -20 minutes) were assessed to improve hydrolysis e ciency of brewery spent grain (BSG) for renewable energy generation. The intensi cation of the pretreatment was expressed by the severity variation (2.8 -4.5) and the process was optimized with methane production of 411.6 ± 7.2 mL. g -1 STV (severity 4.2). The fermentationmethanogenesis of BSG and hydrolysate resulting from BSG hydrothermolysis process under severity of 4.2 (210 o C for 10 min.) was evaluated by central composite design (CCD) with the variables operation temperature (30 -60 °C), BSG concentration (7.3 -20.7 g.L -1 ) and hydrolysate (0 -12.4 mL). The higher methane production observed was 305.8 mL.g -1 STV, with 14 g.L -1 of BSG, without hydrolysate at 45 °C.The main soluble metabolites were acetic acid (233.17 mg.L -1 ) and butyric acid (156.0 mg.L -1 ). On other hand, the lower methane production (108.5 ± 2.0 mL. g -1 STV) veri ed was 14 g.L -1 of BSG, 6.5 mL of hydrolysate at 60 °C, which revealed that in this condition propionic acid (947.4 mg.L -1 ) and acetic acid (599.2 mg.L -1 ) were expressive. In the optimal fermentation-methanogenic condition of pretreated BSG, Macellibacteroides and Sphaerochaeta (15.9 and 14.7%, respectively) were identi ed, as well as archaea similar to Methanosaeta (80.4%), favoring the acetoclastic methanogenic pathway.