Cassava pulp is a major by-product produced in a cassava starch factory, containing 50–60% of starch (dry basis). Therefore, in this study we are considering its potential as a raw material substrate for the production of methane. To ensure sufficient amounts of nutrients for the anaerobic digestion process, the potential of co-digestion of cassava pulp (CP) with pig manure (PM) was further examined. The effect of the co-substrate mixture ratio was carried out in a semi-continuously fed stirred tank reactor (CSTR) operated under mesophilic condition (37 °C) and at a constant OLR of 3.5 kg VS m−3 d−1 and a HRT of 15 days. The results showed that co-digestion resulted in higher methane production and reduction of volatile solids (VS) but lower buffering capacity. Compared to the digestion of PM alone, the specific methane yield increased 41% higher when co-digested with CP in concentrations up to 60% of the incoming VS. This was probably due to an increase in available easily degradable carbohydrates as the CP ratio in feedstock increased. The highest methane yield and VS removal of 306 mL g−1 VSadded and 61%, respectively, were achieved with good process stability (VFA:Alkalinity ratio < 0.1) when CP accounted for 60% of the feedstock VS. A further increase of CP of the feedstock led to a decrease in methane yield and solid reductions. This appeared to be caused by an extremely high C:N ratio of the feedstock resulting in a deficiency of ammonium nitrogen for microbial growth and buffering capacity.