Supercritical water treatment for cello-oligosaccharide production from microcrystalline cellulose

• Supercritical water can dissolve cellulose to water-soluble cello-oligosaccharides.
• The yield and molar mass distribution was controlled via treatment time.
• 42% yield of cello-oligosaccharides was achieved in 0.4 s at 380 °C.
• Fragmentation and dehydration products were identified in oligosaccharides.

Microcrystalline cellulose was treated in supercritical water at 380 °C and at a pressure of 250 bar for 0.2, 0.4, and 0.6 s. The yield of the ambient-water-insoluble precipitate and its average molar mass decreased with an extended treatment time. The highest yield of 42 wt % for DP2-9 cello-oligosaccharides was achieved after the 0.4 s treatment. The reaction products included also 11 wt % ambient-water-insoluble precipitate with a DPw of 16, and 6.1 wt % monomeric sugars, and 37 wt % unidentified degradation products. Oligo- and monosaccharide-derived dehydration and retro-aldol fragmentation products were analyzed via a combination of HPAEC-PAD–MS, ESI-MS/MS, and GC–MS techniques. The total amount of degradation products increased with treatment time, and fragmented (glucosyln-erythrose, glucosyln-glycolaldehyde), and dehydrated (glucosyln-levoglucosan) were identified as the main oligomeric degradation products from the cello-oligosaccharides.

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