Anaerobic digestion of sugarcane press mud (PM) was carried out in 2000 mL Erlenmeyer flasks maintained at 40 ºC for 43 days. The effects of co-digestion with distillery wastewater (DW) and application of hot alkali-liquid pretreatment were determined and investigated. D5, the digester with pretreated feedstock (PM:DW of 2:1), obtained the maximum % CH4 content of 79.4%. The thermochemical pretreatment further enhanced the CH4 content by up to 9.45 times, considering equivalent volumes of PM and DW in the feedstock. The study findings also showed that pH fluctuations affected the stability of the anaerobic digestion process. On the other hand, a relationship between the biochemical oxygen demand (BOD), chemical oxygen demand (COD), total suspended solids (TSS), and volatile solids (VS) removal efficiency with the PM:DW feedstock ratio was observed, whereas lower DW content resulted to an enhanced degradation. Furthermore, applying hot alkali-liquid pre-treatment also resulted in an improved BOD, COD, TSS, and VS removal efficiency, attributed to accelerated hydrolysis leading to a more sustained substrate degradation. Total phosphorus (TP) decreased after digestion, but no relationships accounted for CH4 production and substrate degradation were found. Conversely, the trace elements of Ca, Cu, and Mn verified that they contributed to the efficiency of anaerobic digestion.