Microwave-Assisted Alkali (MAA) pretreatment of corncob biomass was optimized for maximum fermentable sugar yield using dilute sulfuric acid hydrolysis. A Central Composite Design (CCD) investigated the effects of microwave power (450–9000 W), NaOH concentration (1.5 to 4.5% wt./v), and irradiation time (10–20 min) on lignin removal. The optimal MAA pretreatment conditions were found to be 691.73 W, 3.4% NaOH, and 15.5 min, resulting in the selective removal of 73.36% lignin with high retention of cellulose (71.69%) and hemicellulose (22.14%). Characterization techniques (FTIR, SEM, XRD, TGA) confirmed substantial changes in surface morphology, functional groups, crystallinity, and thermal stability of the pretreated corncobs. Dilute sulfuric acid hydrolysis (0.5–2.5%, 110130 °C, 3060 min) of the optimized sample yielded a maximum reducing sugar output of 537.42 mg/g, achieved at 0.534% H2SO4, 122.3 °C, for 58 min. Optimizing Microwave-Assisted Alkali pretreatment process for corncobs could boost biofuel production efficiency, sustainably utilize agricultural waste, and advance a more sustainable energy landscape.
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