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  • Ionic liquid-mediated technology to produce cellulose nanocrystals directly from wood.

Ionic liquid-mediated technology to produce cellulose nanocrystals directly from wood.

Carbohydrate polymers (2015-10-03)
Hatem Abushammala, Ingo Krossing, Marie-Pierre Laborie
ABSTRACT

We report for the first time the direct extraction of cellulose nanocrystals (CNCs) from wood by means of a 1-ethyl-3-methylimidazolium acetate ([EMIM][OAc]) treatment. A native cellulosic product could be recovered in 44% yield with respect to wood cellulose content. The product was analyzed for morphological (TEM, AFM, XRD), chemical (FTIR, (13)C CP/MAS NMR), thermal (DSC, TGA) and surface properties (Zeta potential, contact angle). These analyses evidenced the presence of partially acetylated (surface DS=0.28) nanocrystals of native cellulose I microstructure, with a crystallinity index of about 75% and aspect ratio of 65. Direct production of CNCs from wood is ascribed to the simultaneous capability of [EMIM][OAc] to (1) dissolve lignin in situ while only swelling cellulose, (2) decrease intermolecular cohesion in wood via acetylation, and (3) to catalyze cellulose hydrolysis.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, suitable for HPLC
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Acetone, for chromatography, ≥99.8%
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Tetrahydrofuran, JIS special grade, ≥99.5%
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Tetrahydrofuran, suitable for HPLC, contains no stabilizer
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Acetic acid, 99.5-100.0%
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Sodium hydroxide solution, 0.05 M
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Acetic acid, SAJ first grade, ≥99.0%
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Sodium hydroxide solution, 6 M
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Hydrochloric acid solution, 0.2 M
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Methanol, SAJ first grade, ≥99.5%
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Acetic acid, JIS special grade, ≥99.7%
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Hydrogen chloride – ethanol solution, 0.1 M in ethanol
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Hydrochloric acid, SAJ first grade, 35.0-37.0%
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Hydrochloric acid solution, 0.02 M
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Methanol, JIS 300, ≥99.8%, for residue analysis
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Acetone, for residue analysis, ≥99.5%
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Acetic acid, ≥99.7%
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Chloroform, SAJ first grade, ≥99.0%, contains 0.4-0.8% ethanol
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Chloroform, JIS 300, ≥99.0%, for residue analysis
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Hydrochloric acid solution, 0.05 M
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Hydrochloric acid solution, 2 M
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Acetic acid, ≥99.7%, suitable for amino acid analysis
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Ethanol, JIS special grade, 94.8-95.8%
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Tetrahydrofuran, SAJ first grade, ≥99.0%
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Chloroform, JIS special grade, ≥99.0%
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Hydrogen peroxide solution, SAJ first grade, ≥30.0%
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Acetone, JIS special grade, ≥99.5%
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Sodium hydroxide solution, 1 M
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Sodium hydroxide solution, 0.01 M
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Chloroform, suitable for HPLC