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Issue 14, 2017
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The Hy-MASS concept: hydrothermal microwave assisted selective scissoring of cellulose for in situ production of (meso)porous nanocellulose fibrils and crystals

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Abstract

The hydrothermal microwave-assisted selective scissoring (Hy-MASS) of depectinated orange peel residues (OPR), produced via conventional acid hydrolysis and acid-free microwave processing, to yield (meso)porous nanocellulose fibrils and crystals simultaneously in the absence of additional auxiliary reagents and/or mechanical treatment is reported. In the stepwise microwave hydrothermal treatment (MHT) of OPR from 120 °C–200 °C at 20 °C intervals, release of residual pectins and hemicelluloses is observed up to 180 °C producing nanocellulose fibrils (3–15 × 500–2000 nm). Beyond 180 °C, selective leaching/hydrolysis of amorphous regions occur to yield nanocellulose crystals (200–400 × 40–50 nm) and crystallites (5–15 × 40–50 nm). This selective, step-wise scissoring process is termed Hy-MASS Concept. Structure, morphology and properties of (meso)porous nanocellulose are strongly influenced by pectin extraction methodology employed. With acid depectinated OPR, deconstruction of the lignocellulosic matrix via microwave is hastened by approx. 20 °C with respect to acid-free microwave depectinated OPR. Td of acid depectinated nanocelluloses (CMC) is ca. 350 °C compared to microwave depectinated nanocelluloses (MMC, Td, varies 342–361 °C). Nanocellulose produced via microwave pre-treatment is (meso)porous: BJH pore size 5–35 nm; BET surface area, 1.5–107 m2 g−1, and; BJH pore volume, 0.01–0.27 cm3 g−1, when compared to acid pre-treated counterparts. The crystallinity index of CMC and MMC increases in two stages, 120–140 °C (ca. 8%) and at 180–200 °C (5–9%). XRD revealed presence of calciuim salts, most likely calcium oxalate. The hydration capacities of nanocelluloses (12–23 g water per g sample) are much higher than their precursors or literature citrus nanocellulose.

Graphical abstract: The Hy-MASS concept: hydrothermal microwave assisted selective scissoring of cellulose for in situ production of (meso)porous nanocellulose fibrils and crystals

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Publication details

The article was received on 09 May 2017, accepted on 14 Jun 2017 and first published on 23 Jun 2017


Article type: Paper
DOI: 10.1039/C7GC01378G
Citation: Green Chem., 2017,19, 3408-3417
  • Open access: Creative Commons BY-NC license
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    The Hy-MASS concept: hydrothermal microwave assisted selective scissoring of cellulose for in situ production of (meso)porous nanocellulose fibrils and crystals

    E. M. de Melo, J. H. Clark and A. S. Matharu, Green Chem., 2017, 19, 3408
    DOI: 10.1039/C7GC01378G

    This article is licensed under a Creative Commons Attribution-NonCommercial 3.0 Unported Licence. Material from this article can be used in other publications provided that the correct acknowledgement is given with the reproduced material and it is not used for commercial purposes.

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