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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, NMR reference standard

Sigma-Aldrich

Acetic acid-¹²C₂, 99.9 atom % ¹²C

Sigma-Aldrich

Sodium hydroxide, ultra dry, powder or crystals, 99.99% trace metals basis

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Methanol, HPLC Plus, ≥99.9%, poly-coated bottles

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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%

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

Sigma-Aldrich

Hydroxylamine hydrochloride, 99.999% trace metals basis

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Acetic acid, natural, ≥99.5%, FG

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Chloroform, anhydrous, contains amylenes as stabilizer, ≥99%

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Hydroxylamine hydrochloride, 99.995% trace metals basis

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Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)

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Acetic acid, ≥99.5%, FCC, FG

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Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets

Supelco

Ethanol solution, certified reference material, 2000 μg/mL in methanol

Sigma-Aldrich

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

Sigma-Aldrich

Sodium hydroxide, puriss., meets analytical specification of Ph. Eur., BP, NF, E524, 98-100.5%, pellets

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Acetone, Laboratory Reagent, ≥99.5%

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Acetone, ACS reagent, ≥99.5%

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Sodium hydroxide, reagent grade, 97%, powder

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Methanol, ACS reagent, ≥99.8%

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Methanol, Absolute - Acetone free

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Acetic acid, glacial, ACS reagent, ≥99.7%

Sigma-Aldrich

Chloroform, puriss. p.a., reag. ISO, reag. Ph. Eur., 99.0-99.4% (GC)

Sigma-Aldrich

Acetone, puriss., meets analytical specification of Ph. Eur., BP, NF, ≥99% (GC)

Sigma-Aldrich

Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)

Sigma-Aldrich

Acetone, histological grade, ≥99.5%

Sigma-Aldrich

Acetic acid, glacial, ≥99.99% trace metals basis

Sigma-Aldrich

Methanol, ACS reagent, ≥99.8%

Sigma-Aldrich

Sodium hydroxide, reagent grade, 97%, flakes

Sigma-Aldrich

Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)