Isolation and Characterization of Cellulose Nanocrystals from Different Lignocellulosic Residues: A Comparative Study

Abstract

Recently, cellulose nanocrystals (CNCs) have captured the interest of researchers and industries. In this study, CNCs were isolated from four abundant lignocellulosic byproducts: teff (Eragrostis tef, Poaceae) straw, enset (Ensete ventricosum, Musaceae) fiber (EF), sugarcane (Saccharum officinarum, Poaceae) bagasse and coffee (Coffea arabica, Rubiaceae) hull (CH). Cellulose fibers were obtained using chlorine-free extraction with 5% sodium hydroxide pretreatment followed by delignification (with formic acid, acetic acid and hydrogen peroxide) and bleaching (with alkaline hydrogen peroxide). CNCs were then isolated following hydrolysis of the cellulose fibers with 64% sulfuric acid. The as-obtained CNCs were investigated and characterized in terms of yield, crystallinity, chemical functionality, morphology, particle size, zeta potential (ZP) and thermal stability. The CNCs displayed a typical crystal lattice of Iβ-type based on XRD patterns, d-spacings and Z-values. The highest yield (~ 70%), CrI (~ 86%), and crystal size (~ 6 nm) were observed in EF–CNCs, and the least in CH–CNCs (yield: ~ 25%, CrI: ~ 77%, crystal size: ~ 4 nm). FTIR spectra of all CNCs indicated typical chemical composition of cellulose. TEM observations revealed that the CNCs were needle-shaped nanoscale structures with different aspect ratios (17.32–36.67) and dimensions (average length: 154.28–193.06 nm; diameter: 5.16–11.79 nm), while the DLS measurements provided the hydrodynamic sizes, 96.96–184.90 nm. The thermal studies by TGA/DTG revealed the CNCs had a two-step decomposition process at Tmax 215–225 °C and 340–355 °C. This study showed that the CNCs isolated exhibited high crystallinity, aspect ratio, colloidal and thermal stability although differences were observed due to variations in cellulose sources.

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Abbreviations

C1 and C2:

Cellulose fibres extracted with extraction Conditions 1 and 2, respectively

CC:

Commercial cellulose

CC-CNCs:

Cellulose nanocrystals isolated from commercial cellulose

CH:

Coffee hull

CNCs-C1 and CNCs-C2:

Cellulose nanocrystals isolated from C1 and C2, respectively

CrI(s):

Crystallinity index/indexes

DLS:

Dynamic light scattering

DTG:

Differential thermo gravimetry

EF:

enset Fiber

FTIR:

Fourier-Transform Infrared spectroscopy

HA:

Hermans et al. approach

SA:

Segal et al. approach

SB:

Sugarcane bagasse

TEM:

Transmission electron microscopy

TGA:

Thermogravimetric analysis

TS:

teff Straw

X200 :

The proportion of crystallite interior chains for the 200 plane

XRD:

X-ray diffraction

ZP:

Zeta potential

Δd/d200 :

The fractional variation in the plane spacing for the 200 plane

τ200 :

Average thickness (size) of cellulose crystallites for the 200 plane

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Acknowledgements

The authors would like to acknowledge Addis Ababa University, Ethiopia for sponsoring the PhD study of TG, and Martin Luther University, Germany for providing access to laboratory space and facilities such as TEM and DLS. This research was partly supported by the Ministry of Innovation and Technology, Ethiopia, and Tri-Sustain (Economic, Ecological and Therapeutic Sustainability) Project in the development of phytopharmaceuticals for Sub-Saharan Africa, funded by the German Ministry of Research and Education (BmBF) (Grant No. 01DG17008B) and German Academic Exchange Service (DAAD) (Grant No. 57369155), Germany.

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Conceptualization, Methodology, Investigation, Visualization, original draft Writing, Software: TG. Writing—review & editing, Formal analysis: AB. Software, Methodology, Writing—review & editing: GH. Funding acquisition, Project administration, Writing—review & editing: RN. Conceptualization, Investigation, Supervision, Visualization, Writing—review & editing, Funding acquisition: TG-M.

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Correspondence to Tsige Gebre-Mariam.

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Gabriel, T., Belete, A., Hause, G. et al. Isolation and Characterization of Cellulose Nanocrystals from Different Lignocellulosic Residues: A Comparative Study. J Polym Environ (2021). https://doi.org/10.1007/s10924-021-02089-3

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Keywords

  • Cellulose nanocrystals
  • Teff straw
  • Enset fiber
  • Sugarcane bagasse
  • Coffee hull