The efficient pretreatment
of lignocellulosic biomass
is essential
for cellulose valorization. This work investigated the fractionation
efficiency of the pretreatment process based on natural acidic deep
eutectic solvent (NADES) for isolating cellulose-rich materials (CRM)
from coffee parchment (CP). The results showed that NADES, composed
of choline chloride, oxalic acid, and water in a 2:2:1 molar ratio,
was the most efficient solvent for CP fractionation. The sequential
pretreatment using NADES under microwave heating (MW-NADES) at 130
°C for 15 min, followed by a two-step alkaline hydrogen peroxide
(AHP) process, could maximize the removals of hemicellulose (99.6%)
and lignin (97.7%) from CP, leading to production of the CRM with
86.1% cellulose content. This process generated a rough, fractured
surface and promoted microfibril disassembly observed in the pretreated
fibers. As a result, the CRM exhibited a highly crystalline structure
and good thermal stability. Furthermore, the results also highlighted
the successful transformation of the isolated CRM to nanofibril networks
having a diameter of less than 10 nm and a length of several hundred
nanometers. Overall, this work suggests that the sequential MW-NADES
and AHP pretreatment could be considered an effective approach in
isolating high-purity cellulose from CP, potentially a sustainable
source for nanocellulose production.