A laboratory experimental campaign was carried out in order to assess the optimal configuration for the anaerobic digestion of a mixture of sweet corn and ensiled maize. Batch hydrolysis tests were conducted at 35 and 55 °C and at four different particle sizes (2, 5, 20 and 50 mm) obtained by manual chopping and sieving. Chemical pre-treatment by 24 h incubation at various acid and alkaline pH was also considered for its potential to increase the maize methane yield. Results suggest that the hydrolytic phase proceeds significantly faster under thermophilic conditions. Significant differences in the solubilization rate were also observed when comparing coarse (20-50 mm) with fine (2-5 mm) particles, while 2 and 5 mm particles were solubilized at similar rates. No advantages from the chemical pre-treatment, in terms of solubilization efficiency and biomethanization potential were observed. According to these preliminary results, a two-stage semi-continuous laboratory plant consisting of a thermophilic hydrolytic reactor followed by a mesophilic methanogenic reactor was operated for 110 days. Steady state loading parameters were: influent concentration (maize mixture diluted in tap water) of 46 g VS/L, hydraulic retention time of 31 d, organic loading rate of 1.5 g VS/L/d. Alkalinity was dosed to the methanogenic reactor to avoid pH drops. Collected data allowed the average biodegradation efficiency to be estimated at around 60-65%.