Even though the Brazilian ethanol and sugar production system (based on sugarcane industry) have been providing large amounts of bioenergy, the extensive amounts of organic wastes generated cannot be ignored when it comes to sustainability. Using these biomasses to produce biomethane through anaerobic digestion has been proven as a promising way to tackle this issue. This study investigated the biomethane potential of the co-digestion of these biomasses: SF (sugarcane straw : filter cake = 8:2), SFV (sugarcane straw : filter cake : vinasse = 1:4:45), and D (digestate separated from AD of SFV). Three treatments autoclaving (AU), alkaline (AL) treatment using 6% (w/w) NaOH and the combination of these two (AUAL) were then conducted on SF and SFV as pre-treatments; on D as post- treatments. In the biomethane potential tests of untreated material, the highest methane yield was achieved by SFV with 275.28 ± 11 N ml CH4/g VS, followed by SF with 223.25 ± 10 N ml CH4 g-1 VS, substrate D also resulted in a methane potential of 144.69 ± 2 N ml CH4 g-1 VS. As pre-treatments, AL and AUAL both showed increase in methane yield (between 36.0% and 49.1%) and methane production rate. As post-treatments, AU, AL and AUAL showed distinctive results in methane production, with 33.8%, 99.8% and 128.8% increase, respectively. In comparison with pre-treatment, post-treatment showed a better performance in increasing methane production. The following feeding experiments performed in continuous stirred-tank reactors showed that AL treatment led to an average of 248% increase in methane yield. / Sugarcane waste: towards a zero C emission in the Brazilian bioenergy sector