Abstract Oil palm mesocarp fiber is a promising lignocellulosic biomass as a raw material for valorizing biomass into more valuable products such as second-generation biofuels, biocomposites, or bioenergy. However, the lignin composition present in lignocellulosic biomass provides resistance to the valorization process and protects the cellulose composition, thereby limiting the conversion of cellulose into more valuable products. The hybrid ozonation-ultrasonic method as a lignin-degrading method is starting to be considered an effective method. Additionally, a Box-Behnken Design (BBD) was employed to investigate each independent variable's effect on pretreatment process conditions using the response surface methodology (RSM), namely reaction time (30-90) min, reaction temperature (20 -40) oC and ozone flow rate (1-3) L/min to the response of the percentage of lignin degradation (%). The optimum condition of the pretreatment process is determined using the desirability function graph. The results showed that reaction time, reaction temperature, and ozone flow rate had a significant effect on lignin degradation (p <0.05). The optimum conditions obtained the highest percentage of lignin degradation, namely 92.08% at a reaction temperature of 30 oC with an ozone flow rate of 2 L/min for 60 minutes reaction time. The decrease in lignin absorption peaks at 1638 cm-1 and 1427 cm-1 was supported by the results of the analysis of increased crystallinity in the sample after the pretreatment of lignin degradation to 80.20% and was validated by changes in the morphology of the mesocarp fiber after the pretreatment process indicating that the lignin compound had been successfully degraded from cellulose products of mesocarp fibers.
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