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Investigating the effects of hemicellulose pre-extraction on the production and characterization of loblolly pine nanocellulose

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Abstract

Production of nanocellulosic materials from loblolly pine (Pinus taeda) kraft pulp provides an opportunity to diversify the portfolio of traditional pulp and paper industries. In this study, pinewood was first subjected to dilute acid pre-extraction with 0.5% sulfuric acid in order to fractionate the hemicellulose, followed by kraft pulping and elemental chlorine free bleaching in order to obtain up to 97% pure cellulose fractions. CNCs (cellulose nanocrystals) were prepared by hydrolyzing the bleached kraft pulp with 64% sulfuric acid at 45 °C for 30 min; the resultant unhydrolyzed solid residues were homogenized using a microfluidizer in order to produce cellulose nanofibers (CNFs). The dilute acid pre-extraction step resulted in complete hydrolysis of galactan and arabinan from pinewood, as well as in partial removal of mannan (80%) and xylan (58%). As a result of pre-extraction, the CNC yield and crystallinity improved by 44% and 11%, respectively, from the corresponding kraft pulps. CNCs produced from the pre-extracted materials also exhibited 16% reduction in particle size, but a 70% increase in sulfur content as well as 20% increase in zeta potential. Higher purity of kraft pulps resulted in higher exposure of cellulose crystalline domains to sulfuric acid thereby resulting in the observed changes. Thus, pulp purity was found to play a significant role in determining the quantity and quality of nanocellulosic materials derived from loblolly pine.

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Acknowledgments

This project was supported by the Center for Advanced Surface Engineering (CASE) under the National Science Foundation (NSF) Grant Number OIA-1457888 and the Arkansas EPSCoR program, ASSET III. We would like to thank B.A. Babst and W.L. Headlee from the University of Arkansas, Monticello for providing the pine biomass, and A. Kuchuk and E. Martin at the Institute for Nanoscience and Engineering, University of Arkansas, Fayetteville for assisting with XRD analysis and TEM imaging, respectively. We would also like to thank C. Hamilton for conducting the ICP-OES analysis at the Center for Renewable Carbon, University of Tennessee, Knoxville.

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Correspondence to Jin-Woo Kim.

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Rajan, K., Djioleu, A., Kandhola, G. et al. Investigating the effects of hemicellulose pre-extraction on the production and characterization of loblolly pine nanocellulose. Cellulose (2020). https://doi.org/10.1007/s10570-020-03018-8

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Keywords

  • Loblolly pine
  • Hemicellulose pre-extraction
  • Dilute-acid pretreatment
  • Cellulose nanocrystals
  • Cellulose nanofibers
  • CNC yield
  • CNC crystallinity