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Cocoa pod husks are a type of biomass that is still poorly explored. This work was carried out as part of the optimization of the delignification process for this residue with potassium hydroxide, to maximize the reducing sugars content. Screening for potentially influencing factors showed that the biomass to solvent ratio and the temperature had the greatest effect on the delignification process. Optimization of these factors using a composite central plan revealed that the quadratic model was the most suitable for predicting the rate of delignification. The predicted R² (0.815) was in good agreement with the adjusted R² (0.906). The correlation coefficient (R2 = 0.945) between the predicted and experimental results confirmed the fit of the model. The optimal conditions were a biomass to solvent ratio of 9.14% and a temperature of 128 °C, which resulted in a maximum degree of delignification of 93.9%, with 80% of the solids recovered. This study found that the removal of extractables before the pretreatment considerably improved the delignification of cocoa pod husks and the production of reducing sugars, which increased from 3.15 ± 0.006 mg/mL to 5.33 ± 0.143 mg/mL. Scanning electron microscopy and X-ray diffraction confirmed physicochemical changes in the biomass after pretreatment.

Optimization of the autoclave-assisted alkaline delignification of cocoa (Theobroma cacao) pod husks using KOH to maximize reducing sugars