Springer Nature is making SARS-CoV-2 and COVID-19 research free. View research | View latest news | Sign up for updates

Effects of hydrolysis conditions on the morphology, crystallinity, and thermal stability of cellulose nanocrystals extracted from kenaf bast fibers

  • 4972 Accesses

  • 310 Citations

Abstract

Cellulose nanocrystals (CNC) were first isolated from kenaf bast fibers and then characterized. The raw fibers were subjected to alkali treatment and bleaching treatment and subsequent hydrolysis with sulfuric acid. The influence of the reaction time on the morphology, crystallinity, and thermal stability of CNC was investigated. Fourier transform infrared spectroscopy showed that lignin and hemicellulose were almost entirely removed during the alkali and bleaching treatments. The morphology and dimensions of the fibers and acid-released CNC were characterized by field emission scanning electron microscopy and transmission electron microscopy. X-Ray diffraction analysis revealed that the crystallinity first increases upon hydrolysis and then decreases after long durations of hydrolysis. The optimal extraction time was found to be around 40 min during hydrolysis at 45 °C with 65% sulfuric acid. The thermal stability was found to decrease as the hydrolysis time increased. The electrophoretic mobility of the CNC suspensions was measured using the zeta potential, and it ranged from −8.7 to −95.3 mV.

This is a preview of subscription content, log in to check access.

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

References

  1. Ahmad I, Mosadeghzad Z, Daik R, Ramli A (2008) The effect of alkali treatment and filler size on the properties of sawdust/UPR composites based on recycled PET wastes. J Appl Polym Sci 109:3651–3658

  2. Alemdar A, Sain M (2008) Isolation and characterization of nanofibres from agricultural residues-wheat straw and soy hulls. Bioresor Technol 99:1664–1671

  3. Angellier H, Putaux JL, Molina-Boisseau S, Dupeyre D, Dufresne A (2005) Starch nanocrystal fillers in a acrylic polymer matrix. Macromol Symp 221:95–104

  4. Araki J, Wada M, Kuga S, Okano T (1998) Low properties of microcrystalline cellulose suspension prepared by acid treatment of native cellulose. Colloid Surface A 142:75–82

  5. Ashori A, Jalaluddin H, Raverty WD, Mohd Nor MY (2006) Chemical and morphological characteristics of Malaysia Cultivated kenaf (Hibiscuse cannabinus) fiber. Polym Plast Technol 45:131–134

  6. Beck-Candanedo S, Roman M, Gray DG (2005) Effect of reaction conditions on the properties and behavior of wood cellulose nanocrystal suspensions. Biomacromolecules 6:1048–1054

  7. Bendahou A, Habibi Y, Kaddami H, Dufresne A (2009) Physico-chemical characterization of palm from Phoenix Dactylifera–L, preparation of cellulose whiskers and natural rubber—based nanocomposites. J Biobas Mat Bioenergy 3:81–90

  8. Bismarck A, Mishra S, Lampke T (2005) Plant fiber as reinforcement for green composites. In: Mohanty AK, Misra M, Drzal LT (eds) Natural fiber biopolymers, and biocomposites. CRC Press, Boca Raton, vol 2, pp 37–108

  9. Bledzki AK, Gassan J (1999) Composites reinforced with cellulose based fiber. Prog Polym Sci 24:221–274

  10. Bondeson D, Mathew A, Oksman K (2006) Optimization of the isolation of nanocrystal from microcrystalline cellulose by acid hydrolysis. Cellulose 13:171–180

  11. Chen Y, Liu C, Chang PR, Cao X, Anderson DP (2009) Bionanocomposites based on pea starch and cellulose nanowhiskers hydrolyzed from pea hull fibre: effect of hydrolysis time. Carbohyd Polym 76:607–615

  12. Cherian BM, Leão AL, de Souza SF, Thomas S, Pothan LA, Kottaisamy M (2010) Isolation of nanocellulose from pineapple leaf fibres by steam explosion. Carbohyd Polym 81:720–725

  13. de Souze Lima MM, Borsali R (2004) Rodlike cellulose microcrystals: structure, properties, and applications. Macromol Rapid Comm 25:771–787

  14. Dong XM, Revol JF, Gray DG (1998) Effect of microcrystallite preparation conditions on the formation of colloid crystals of cellulose. Cellulose 5:19–32

  15. Dufresne A (2008) Cellulose-based composites and nanocomposites. In: Gandini A, Belgacem MN (eds) Monomers, polymers and composites from renewable resources. Elsevier, Oxford, vol 19, pp 401–418

  16. Elanthikkal S, Gopalakrishnapanicker U, Varghese S, Guthrie JT (2010) Cellulose microfibres produced from banana plant wastes: isolation and characterization. Carbohyd Polym 80:852–859

  17. Fahma F, Iwamoto S, Hori N, Iwata T, Takemura A (2010) Isolation, preparation, and characterization of nanofibers from oil palm empty-fruit-bunch (OPEFB). Cellulose 17:977–985

  18. Fahma F, Iwamoto S, Hori N, Iwata T, Takemura A (2011) Effect of pre-acid-hydrolysis treatment on morphology and properties of cellulose nanowhiskers from coconut husk. Cellulose 18:443–450

  19. Favier V, Chanzy H, Cavaille JY (1995) Polymer nanocomposites reinforced by cellulose whiskers. Macromolecules 28:6365–6367

  20. Garcia de Rodriguez NLG, Thielemans W, Dufresne A (2006) Sisal cellulose whiskers reinforced poly(vinyl acetate) nanocomposite. Cellulose 13:261–270

  21. Hunter RJ (1981) Zeta potential in colloids science. Academic Press, New York

  22. Jonoobi M, Harun J, Shakeri A, Misra M, Oksman K (2009) Chemical composition, crystallinity, and thermal degradation of bleached and unbleached kenaf bast (Hibiscus cannabinus) pulp and nanofibres. Bioresour 4:626–639

  23. Li R, Fei J, Cai Y, Li Y, Feng J, Yao J (2009) Cellulose whiskers extracted from mulberry: A novel biomass production. Carbohyd Polym 76:94–99

  24. Lu P, Hsieh YL (2010) Preparation and properties of cellulose nanocrystals: rods, spheres, and network. Carbohyd Polym 82:329–336

  25. Martínez-Sanz M, Lopez-Rubio A, Lagaron JM (2011) Optimization of the nanofabrication by acid hydrolysis of bacterial cellulose nanowhiskers. Carbohyd Polym 85:228–236

  26. Mohd Edeerozey AM, Hazizan MA, Azhar AB, Zainal Ariffin MI (2007) Chemical modification of kenaf fibers. Mater Lett 61:2023–2025

  27. Morán JI, Alvarez VA, Cyras VP, Vázquez A (2008) Extraction of cellulose and preparation of nanocellulose from sisal fibres. Cellulose 15:149–159

  28. Pääkkö M, Ankerfors M, Kosonen H, Nykänen A, Ahola S, Österberg M, Ruokolainen J, Laine J, Larsson PT, Ikkala O, Lindström T (2007) Enzymatic hydrolysis combined with mechanical shearing and high-pressure homogenization for nanoscale cellulose fibrils and strong gels. Biomacromolecules 8:1934–1941

  29. Roman M, Winter WT (2004) Effect of sulphated groups from sulphuric acid hydrolysis on the thermal degradation behavior of bacterial cellulose. Biomacromolecules 5:1048–1054

  30. Rosa MF, Medeiros ES, Malmonge JA, Gregorski KS, Wood DF, Mattoso LHC, Glenn G, Orts WJ, Imam SH (2010) Cellulose nanowhiskers from coconut husk fibres: effect of preparation conditions on their thermal and morphological behavior. Carbohyd Polym 81:83–92

  31. Rowell RM, Han JS, Rowell JS (2000) Characterization and factors effecting fiber properties. In: Frollini E, Leão AL, Mattoso LHC (eds) Natural polymers and agrofibers composites. Embrapa Instrumentação Agropecuária, São Carlos, pp 115–134

  32. Sain M, Panthapulakkal S (2006) Bioprocess preparation of wheat straw fibres and their characterization. Ind Crops Prod 2:1–8

  33. Segal L, Greely JJ, Martin AE, Conrad CM (1959) An empirical method for estimating the degree of crystallinity of native cellulose using X-ray diffractometer. Text Res J 29:786–794

  34. Shebani AN, van Reenen AJ, Meincken M (2008) The effect of wood extractives on the thermal stability of different wood species. Thermochim Acta 471:43–50

  35. Siqueira G, Abdillahi H, Bras J, Dufresne A (2010) High reinforcing capability cellulose nanocrystals extracted from syngonanthus nitens (Capim Dourado). Cellulose 17:289–298

  36. Swingle RS, Urias AR, Doyle JC, Voigt RL (1978) Chemical composition of kenaf forage and its digestibility by lambs and in vitro. J Anim Sci 46:1346–1350

  37. Troedec M, Sedan D, Peyratout C, Bonnet J, Smith A, Guinebretiere R, Gloaguen V, Krausz P (2008) Influence of various chemical treatment on the composition and structure of hemp fibres. Compos Part A 39:514–522

  38. Wang N, Ding E, Cheng R (2007) Thermal degradation behavior of spherical cellulose nanocrystals with sulfate groups. Polymer 48:3486–3493

  39. Yang HP, Yan R, Hen HP, Lee DH, Zheng CG (2007) Characteristics of hemicelluloses, cellulose and lignin pyrolysis. Fuel 86:1781–1788

  40. Zuluaga R, Putaux JL, Velez J, Mondragon I, Gañán P (2009) Cellulose microfibrils from banana rachis: effect of alkaline treatments on structural and morphological features. Carbohyd Polym 76:51–59

Download references

Acknowledgments

The authors acknowledge the financial support from the Ministry of Higher Education (MOHE) and Universiti Kebangsaan Malaysia (UKM) under FRGS grant UKM-ST-07-FRGS0041-2009 and UKM-DLP-2011-013. In addition, we wish to thank the French Embassy in Kuala Lumpur and Universiti Kebangsaan Malaysia (UKM) for providing financial support (French Scholars in Malaysia).

Author information

Correspondence to Ishak Ahmad.

Rights and permissions

Reprints and Permissions

About this article

Cite this article

Kargarzadeh, H., Ahmad, I., Abdullah, I. et al. Effects of hydrolysis conditions on the morphology, crystallinity, and thermal stability of cellulose nanocrystals extracted from kenaf bast fibers. Cellulose 19, 855–866 (2012). https://doi.org/10.1007/s10570-012-9684-6

Download citation

Keywords

  • Kenaf fibers
  • Purification
  • Cellulose nanocrystals
  • Hydrolysis conditions