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

323381

Sigma-Aldrich

Hydrogen peroxide solution, contains ~200 ppm acetanilide as stabilizer, 3 wt. % in H₂O

45754

Sigma-Aldrich

Acetic acid solution, suitable for HPLC

349887

Sigma-Aldrich

Hydrogen peroxide solution, contains inhibitor, 35 wt. % in H₂O

534064

Sigma-Aldrich

Acetone, histological grade, ≥99.5%

472476

Sigma-Aldrich

Chloroform, contains amylenes as stabilizer, ACS reagent, ≥99.8%

455180

Sigma-Aldrich

Hydrogen chloride solution, 2.0 M in diethyl ether

366919

Sigma-Aldrich

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

415413

Sigma-Aldrich

Sodium hydroxide solution, 50% in H₂O

32211

Sigma-Aldrich

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

32201

Sigma-Aldrich

Acetone, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.5% (GC)

516813

Sigma-Aldrich

Hydrogen peroxide solution, 50 wt. % in H₂O, stabilized

345547

Sigma-Aldrich

Hydrogen chloride solution, 4.0 M in dioxane

484024

Sigma-Aldrich

Sodium hydroxide, reagent grade, 97%, flakes

24229

Sigma-Aldrich

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

676764

Sigma-Aldrich

Tetrahydrofuran, ACS reagent, ≥99.0%, contains 200-400 ppm BHT as inhibitor

757527

Sigma-Aldrich

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

06203

Sigma-Aldrich

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

132950

Sigma-Aldrich

Chloroform, ReagentPlus^®, ≥99.8%, contains 0.5-1.0% ethanol as stabilizer

676780

Sigma-Aldrich

Methanol, ACS reagent, ≥99.8%

695092

Sigma-Aldrich

Acetic acid, glacial, ACS reagent, ≥99.7%

M1775

Sigma-Aldrich

Methanol, Absolute - Acetone free

S8045

Sigma-Aldrich

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

05211

Sigma-Aldrich

Sodium hydroxide solution, purum, ≥32%

179124

Sigma-Aldrich

Acetone, ACS reagent, ≥99.5%

07102

Sigma-Aldrich

Hydrochloric acid, meets analytical specification of Ph. Eur., BP, NF, fuming, 36.5-38%

07104

Sigma-Aldrich

Hydrochloric acid, puriss., 24.5-26.0%

179973

Sigma-Aldrich

Acetone, Laboratory Reagent, ≥99.5%

655104

Sigma-Aldrich

Sodium hydroxide, reagent grade, 97%, powder

33209

Sigma-Aldrich

Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%

319988

Sigma-Aldrich

Chloroform, contains ethanol as stabilizer, ACS reagent, ≥99.8%