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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

Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)

Sigma-Aldrich

Acetic acid-¹²C₂, 99.9 atom % ¹²C

Supelco

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

Sigma-Aldrich

Methanol, NMR reference standard

Sigma-Aldrich

Hydrochloric acid solution, ~6 M in H₂O, for amino acid analysis

Sigma-Aldrich

Hydrochloric acid solution, 32 wt. % in H₂O, FCC

Sigma-Aldrich

Ethanol, JIS special grade, 94.8-95.8%

Sigma-Aldrich

Sodium hydroxide solution, 1.0 N, BioReagent, suitable for cell culture

Sigma-Aldrich

Hydrogen peroxide solution, 30 % (w/w) in H₂O, contains stabilizer

Sigma-Aldrich

Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture

Supelco

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

Sigma-Aldrich

Hydrochloric acid, 36.5-38.0%, BioReagent, for molecular biology

Sigma-Aldrich

Chloroform, ≥99%, PCR Reagent, contains amylenes as stabilizer

Sigma-Aldrich

Acetyl bromide, 99%

Sigma-Aldrich

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

Sigma-Aldrich

Hydroxylamine hydrochloride, 99.999% trace metals basis

Sigma-Aldrich

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

Sigma-Aldrich

Acetic acid, natural, ≥99.5%, FG

Sigma-Aldrich

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

Sigma-Aldrich

Acetone, ≥99%, meets FCC analytical specifications

Sigma-Aldrich

Hydroxylamine hydrochloride, 99.995% trace metals basis

Sigma-Aldrich

Acetone, natural, ≥97%

Sigma-Aldrich

Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H₂O

Sigma-Aldrich

Acetic acid, ≥99.5%, FCC, FG

Sigma-Aldrich

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

Sigma-Aldrich

Hydrogen peroxide solution, 34.5-36.5%

Sigma-Aldrich

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

Sigma-Aldrich

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

Sigma-Aldrich

Acetone, ACS reagent, ≥99.5%

Sigma-Aldrich

Methanol, ACS reagent, ≥99.8%