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. 2021 Oct 21;11(11):2778.
doi: 10.3390/nano11112778.

Facile Preparation and Characteristic Analysis of Sulfated Cellulose Nanofibril via the Pretreatment of Sulfamic Acid-Glycerol Based Deep Eutectic Solvents

Weidong Li  1 , Yu Xue  1   2 , Ming He  1 , Jiaqiang Yan  1 , Lucian A Lucia  1   3   4   5 , Jiachuan Chen  1 , Jinghua Yu  2 , Guihua Yang  1
Affiliations

Facile Preparation and Characteristic Analysis of Sulfated Cellulose Nanofibril via the Pretreatment of Sulfamic Acid-Glycerol Based Deep Eutectic Solvents

Weidong Li et al. Nanomaterials (Basel). .

Abstract

A deep eutectic solvent (DES) composed of sulfamic acid and glycerol allowed for the sustainable preparation of cellulose nanofibrils (CNF) with simultaneous sulfation. The reaction time and the levels of sulfamic acid demonstrated that fibers could be swelled and sulfated simultaneously by a sulfamic acid-glycerol-based DES and swelling also promoted sulfation with a high degree of substitution (0.12). The DES-pretreated fibers were further nanofibrillated by a grinder producing CNF with diameters from 10 nm to 25 nm. The crystallinity ranged from 53-62%, and CNF maintained the original crystal structure. DES pretreatment facilitated cellulose nano-fibrillation and reduced the energy consumption with a maximum reduction of 35%. The films prepared from polyvinyl alcohol (PVA) and CNF showed good UV resistance ability and mechanical properties. This facile and efficient method provided a more sustainable strategy for the swelling, functionalization and nano-fibrillation of cellulose, expanding its application to UV-blocking materials and related fields.

Keywords: cellulose nanofibril (CNF); characterization; deep eutectic solvent (DES); sulfamic acid-glycerol; sulfation.

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Conflict of interest statement

The authors declare no conflict of interest. The funders had no role in the design of the study; in the collection, analyses, or interpretation of data; in the writing of the manuscript, or in the decision to publish the results.

Figures

Figure 1
Figure 1
The preparation scheme of DES-untreated and DES-treated CNF.
Figure 2
Figure 2
FTIR spectra of original cellulose pulp (a), pulp-6-1 (b), pulp-6-1.5 (c), pulp-9-1 (d), pulp-9-1.5 (e), pulp-12-1 (f), and pulp-12-1.5 (g).
Figure 3
Figure 3
Water retention value (WRV, g/g) of CNF samples as a function of energy consumption (kWh/kg) in the supermasscolloider.
Figure 4
Figure 4
Schematic diagram for preparation of CNF through DES pretreatment.
Figure 5
Figure 5
AFM topography images, and diameter distribution histograms of (a) CNF, (b) CNF-6-1, (c) CNF-6-1.5, (d) CNF-9-1, (e) CNF-9-1.5, (f) CNF-12-1, and (g) CNF-12-1.5.
Figure 5
Figure 5
AFM topography images, and diameter distribution histograms of (a) CNF, (b) CNF-6-1, (c) CNF-6-1.5, (d) CNF-9-1, (e) CNF-9-1.5, (f) CNF-12-1, and (g) CNF-12-1.5.
Figure 6
Figure 6
X-ray diffraction curves of original fibers and DES-treated pulp after nano-fibrillation.
Figure 7
Figure 7
UV-Visible transmittance of neat PVA and PVA/CNF films.
Figure 8
Figure 8
Stress–strain curves of neat PVA and PVA/CNF films.
See this image and copyright information in PMC

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