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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

Phenolphthalein solution, 1 % (w/v), pH 7.8-10.0

Sigma-Aldrich

Sodium hydroxide-¹⁶O solution, 20 wt. % in H₂¹⁶O, 99.9 atom % ¹⁶O

Sigma-Aldrich

Ethyl alcohol, Pure, 200 proof, anhydrous, ≥99.5%

Sigma-Aldrich

Dimethyl sulfoxide, JIS special grade, ≥99.0%

Sigma-Aldrich

Phenolphthalein solution, 0.1 % (w/v), pH 7.8-10.0

Sigma-Aldrich

Toluene, SAJ first grade, ≥99.0%

Sigma-Aldrich

Phenolphthalein, JIS special grade, ≥98.0%

Sigma-Aldrich

Ethanol, ≥99.5%, SAJ super special grade

Sigma-Aldrich

Ethanol, ≥99.5%, suitable for absorption spectrum analysis

Sigma-Aldrich

Toluene, JIS 300, suitable for residue analysis, ≥99.8%

Sigma-Aldrich

Phenolphthalein, SAJ first grade, ≥97.0%

Sigma-Aldrich

Ethanol, ≥99.5%, suitable for fluorescence

Sigma-Aldrich

Dimethyl sulfoxide, SAJ first grade, ≥99.0%

Sigma-Aldrich

Ethanol, ≥99.5%

Sigma-Aldrich

Dimethyl sulfoxide solution, 50 wt. % in H₂O

Sigma-Aldrich

Dimethyl sulfoxide, ≥99.5%

Sigma-Aldrich

Toluene, JIS special grade, ≥99.5%

Sigma-Aldrich

Pyridine, suitable for hydroxyl value determination, ≥99.5%

Sigma-Aldrich

Ethanol, JIS 300, ≥99.5%, suitable for residue analysis

Sigma-Aldrich

Ethanol, JIS 1000, ≥99.5%, suitable for residue analysis

Sigma-Aldrich

Dimethyl sulfoxide, ≥99.0%, suitable for absorption spectrum analysis

Sigma-Aldrich

Phenolphthalein solution, 0.04 % (w/v), pH 7.8-10.0

Sigma-Aldrich

Ethanol, ≥99.5%, suitable for HPLC

Sigma-Aldrich

Pyridine, JIS special grade, ≥99.5%

Sigma-Aldrich

Toluene, JIS 1000, suitable for residue analysis, ≥99.8%

Sigma-Aldrich

Dimethyl sulfoxide, suitable for HPLC

Sigma-Aldrich

Dimethyl sulfoxide, ≥99.6%, ReagentPlus^®

Sigma-Aldrich

Pyridine, anhydrous, 99.8%

Sigma-Aldrich

Ethyl alcohol, Pure, 190 proof, ACS spectrophotometric grade, 95.0%

Sigma-Aldrich

Hydrogen chloride, ReagentPlus^®, ≥99%