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

606766

Sigma-Aldrich

Acetic acid-¹²C₂, 99.9 atom % ¹²C

717975

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Methanol, NMR reference standard

W530574

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2104

Supelco

Hydrochloric acid solution, volumetric, 0.1 M HCl (0.1N), endotoxin free

H1758

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431362

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439126

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Acetone, suitable for HPLC, ≥99.9%

186562

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Tetrahydrofuran, anhydrous, contains 250 ppm BHT as inhibitor, ≥99.9%

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Acetic acid, natural, ≥99.5%, FG

401757

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Tetrahydrofuran, anhydrous, ≥99.9%, inhibitor-free

W332607

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Acetone, ≥99%, meets FCC analytical specifications

288306

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Chloroform, anhydrous, ≥99%, contains 0.5-1.0% ethanol as stabilizer

72068

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Acetic acid, ≥99.5%, FCC, FG

322415

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S8045

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Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)

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Acetone, ACS reagent, ≥99.5%

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Methanol, Absolute - Acetone free

27225

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Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%

221465

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Sodium hydroxide, ACS reagent, ≥97.0%, pellets

338826

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Acetic acid, glacial, ≥99.99% trace metals basis

366919

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Chloroform, ACS spectrophotometric grade, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer

323381

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496189

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Chloroform, contains 100-200 ppm amylenes as stabilizer, ≥99.5%

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