This study aimed at characterising, hydrolysing and mechanically pressing a mixture of fibrous biomass materials (cassava, yam and plantain peels) from Africa. It comparatively evaluates the biomethane potential from these mixtures and their press waters and cakes, using the Hohenheim Biogas Technology (HBT) at a temperature of 27 ℃ and an inoculum produced at a mesophilic temperature of 37 ℃ but adapted to a psychrophilic temperature of 27 ℃. The studied materials conform to biowaste, with energetic values relevant for biogas generation. The biomethane potentials of the materials pre-treated using hydrolysis is about 60% more than the biomethane potential of the non-treated form. Press waters and press cakes from these materials (both pre-treated and non-pre-treated) proved to have valuable biogas potentials, useful for energy purposes. In this study, the primary materials contained a mixture of different waste materials in a form that mimics the practically occurring generation pattern in Africa, unlike most studies, which considered single materials waste resources.