This study focused on the degradation of cornstalk and recovery of reducing sugars and volatile fatty acids (VFAs) at different hydrothermal treatment severity (HTS) (4.17-8.28, 190-320 degrees C). The highest recovery of reducing sugars and VFAs reached 92.39% of aqueous products, equal to 34.79% based on dry biomass (HTS, 6.31). GC-MS and HPLC identified that the aqueous contained furfural (0.35-2.88 g/L) and 5-hydroxymethyl furfural (0-0.85 g/L) besides reducing sugars and VFAs. Hemicellulose and cellulose were completely degraded at a HTS of 5.70 and 7.60, respectively. SEM analysis showed that cornstalk was gradually changed from rigid and highly ordered fibrils to molten and grainy structure as HTS increased. FT-IR and TGA revealed the significant changes of organic groups for cornstalk before and after hydrothermal treatment at different HTS. Hydrothermal treatment might be promising for providing feedstocks suitable for biohythane production. (C) 2015 Elsevier Ltd. All rights reserved.