Chlorine-free extraction and structural characterization of cellulose nanofibers from waste husk of millet (Pennisetum glaucum)

Int J Biol Macromol. 2022 May 1:206:92-104. doi: 10.1016/j.ijbiomac.2022.02.078. Epub 2022 Feb 22.

Abstract

This study aims to extract cellulose nanofibers (CNFs) from a sustainable source, i.e. millet husk, which is an agro-waste worthy of consideration. Pre-treatments such as mercerisation, steam explosion, and peroxide bleaching (chlorine-free) were applied for the removal of non-cellulosic components. The bleached millet husk pulp was subjected to acid hydrolysis (5% oxalic acid) followed by homogenization to extract CNFs. The extracted CNFs were characterized using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Transmission electron microscopy (TEM), Dynamic Light Scattering (DLS), Energy Dispersive X-ray Spectroscopy (EDX), Thermogravimetry (TG and DTG), Differential scanning calorimetry (DSC), and Solid state 13C nuclear magnetic resonance spectroscopy (solid state 13C NMR). The isolated CNFs show a typical cellulose type-I structure with a diameter of 10-12 nm and a crystallinity index of 58.5%. The appearance of the specific peak at 89.31 ppm in the solid state 13C NMR spectra validates the existence of the type-I cellulose phase in the prepared CNFs. The prepared CNFs had a maximum degradation temperature (Tmax) of 341 °C, that was 31 °C greater than raw millet husk (RMH). The outcome of the study implies that the nanofibers are prominent alternatives for synthetic fibers for assorted potential applications, especially in manufacturing green composites.

Keywords: Cellulose nanofibers; Millet husk; Steam explosion.

MeSH terms

  • Cellulose / chemistry
  • Millets
  • Nanofibers* / chemistry
  • Pennisetum*
  • Spectroscopy, Fourier Transform Infrared
  • Thermogravimetry

Substances

  • Cellulose