Synergistic Effects of Double Oxidation on the Extraction and Characterization of Crystalline Nanocellulose from Rattan Waste and Kenaf Fiber
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Keywords:
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Nanocellulose, AFM, Oxidation, FTIR, Rattan, Kenaf
Abstract
This study investigates the potential of rattan fiber, a by-product of the furniture industry, as a feedstock for nanocellulose production. Cellulose nanocrystals (CNC) were extracted using a double oxidation process that combined bleaching with ammonium persulfate (APS) treatment. The effects of APS reaction time, pre-treatment with and without bleaching, on the crystallinity and morphology of CNC were evaluated. Additionally, the feasibility of applying this extraction method to agro-industrial kenaf fiber was assessed. Fourier transform infrared (FTIR) spectroscopic confirmed the removal of lignin and hemicellulose, while the X-ray diffraction (XRD) analysis showed a gradual increase in the crystallinity index (Crl) of CNCs extracted from rattan and kenaf, achieving 73.40% and 72.40, respectively. Scanning Electron Microscope (SEM) revealed fiber disintegration and Transmission Electron Microscopy (TEM) confirmed the spherical CNCs of rattan and kenaf having a diameter of 61.51 ± 6.46 nm and 31.76 ± 6.34 nm, respectively. Atomic force microscopy (AFM) further indicated smaller CNC sizes in kenaf compared to rattan. These findings suggest that rattan fiber is a promising renewable feedstock for producing nanocellulose, with potential application in various industries.
References
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Khalil, H. P. S. A., A. F. I. Yusra, A. H. Bhat, and M. Jawaid (2010). Cell Wall Ultrastructure, Anatomy, Lignin Distribution, and Chemical Composition of Malaysian Cultivated Kenaf Fiber. Industrial Crops and Products, 31(1); 113–121
Khanjanzadeh, H. and B. D. Park (2020). Characterization of Carboxylated Cellulose Nanocrystals from Recycled Fiberboard Fibers Using Ammonium Persulfate Oxidation. Journal of the Korean Wood Science and Technology, 48(2); 231–244
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Nechyporchuk, O., M. N. Belgacem, and J. Bras (2016). Production of Cellulose Nanofibrils: A Review of Recent Advances. Industrial Crops and Products, 93; 2–25
Oun, A. A. and J.-W. Rhim (2017). Characterization of Carboxymethyl Cellulose-Based Nanocomposite Films Reinforced with Oxidized Nanocellulose Isolated Using Ammonium Persulfate Method. Carbohydrate Polymers, 174; 484–492
Padzil, F. N. M., S. H. Lee, Z. M. A. Ainun, C. H. Lee, and L. C. Abdullah (2020). Potential of Oil Palm Empty Fruit Bunch Resources in Nanocellulose Hydrogel Production for Versatile Applications: A Review. Materials, 13(5); 1245
Rahmatullah, R., R. W. Putri, M. Rendana, U. Waluyo, and T. Andrianto (2022). Effect of Plasticizer and Concentration on Characteristics of Bioplastic Based on Cellulose Acetate from Kapok (Ceiba pentandra) Fiber. Science and Technology Indonesia, 7(1); 73–83
Rana, A. K., E. Frollini, and V. K. Thakur (2021). Cellulose Nanocrystals: Pretreatments, Preparation Strategies, and Surface Functionalization. International Journal of Biological Macromolecules, 182; 1554–1581
Razab, M. K. A. A., R. S. M. Ghani, F. A. M. Zin, N. A. A. N. Yusoff, and A. M. Noor (2022). Isolation and Characterization of Cellulose Nanofibrils from Banana Pseudostem, Oil Palm Trunk, and Kenaf Bast Fibers Using Chemicals and High-Intensity Ultrasonication. Journal of Natural Fibers, 19(13); 5537–5550
Sabaruddin, F. A., P. M. Tahir, S. M. Sapuan, R. A. Ilyas, S. H. Lee, K. Abdan, N. Mazlan, A. S. M. Roseley, and H. P. S. A. Khalil (2021). The Effects of Unbleached and Bleached Nanocellulose on the Thermal and Flammability of Polypropylene-Reinforced Kenaf Core Hybrid Polymer Bionanocomposites. Polymers, 13(1); 1–19
Samat, N., R. F. Nasrudin, and N. S. Engliman (2022). Fabrication of Poly(vinyl) Alcohol-Cellulose Nanocrystal Hybrid Aerogel. Materials Science Forum, 1074; 11–16
Samat, N., M. A. Sulaiman, Z. Ahmad, and H. Anuar (2021). A Comparative Study on the Desiccant Effect of Polypropylene and Polylactic Acid Composites Reinforced with Different Lignocellulosic Fibres. Journal of Applied Science and Engineering, 24(2); 223–231
Segal, L., J. J. Creely, A. E. Martin Jr, and C. M. Conrad (1959). An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-Ray Diffractometer. Textile Research Journal, 29(10); 786–794
Shanmugam, K., N. Chandrasekar, and R. Balaji (2023). Barrier Performance of Spray Coated Cellulose Nanofibre Film. Micro, 3(1); 192–207
Song, Y., W. Jiang, Y. Zhang, H. Wang, F. Zou, K. Yu, and G. Han (2018). A Novel Process of Nanocellulose Extraction from Kenaf Bast. Materials Research Express, 5(8); 085032
Sulaiman, S., M. N. Mokhtar, M. N. Naim, A. S. Baharuddin, M. A. M. Salleh, and A. Sulaiman (2015). Study on the Preparation of Cellulose Nanofibre (CNF) from Kenaf Bast Fibre for Enzyme Immobilization Application. Sains Malaysiana, 44(11); 1541–1550
Syazwani, N. S., M. N. E. Efzan, C. K. Kok, and M. J. Nurhidayatullaili (2022). Analysis on Extracted Jute Cellulose Nanofibers by Fourier Transform Infrared and X-Ray Diffraction. Journal of Building Engineering, 48; 103744
Toni, N. M. M. and S. Mahzan (2021). Influences of Chemical Treatment on Mechanical Properties of Rattan. Research Progress in Mechanical and Manufacturing Engineering, 2(2); 590–598
Vu, A. N., L. H. Nguyen, K. Yoshimura, T. D. Tran, and H. V. Le (2024). Cellulose Nanocrystals Isolated from Sugarcane Bagasse Using the Formic/Peroxyformic Acid Process: Structural, Chemical, and Thermal Properties. Arabian Journal of Chemistry, 17(8); 105841
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Wahib, S. A., D. A. Da’na, and M. A. Al-Ghouti (2022). Insight into the Extraction and Characterization of Cellulose Nanocrystals from Date Pits. Arabian Journal of Chemistry, 15(3); 103650
Zhang, K., P. Sun, H. Liu, S. Shang, J. Song, and D. Wang (2016). Extraction and Comparison of Carboxylated Cellulose Nanocrystals from Bleached Sugarcane Bagasse Pulp Using Two Different Oxidation Methods. Carbohydrate Polymers, 138; 237–243
Zuraida, A., T. Maisarah, A. Zahurin, A. M. Luqman, R. Wan Yussof, W. Wan Shazlin Maisarah, and A. Marjan (2015). Structural Examination and Elemental Composition Analysis of Rattan Waste Fibers for Binderless Board Application. Malaysian Journal of Microscopy, 11; 39–44
Al-Dulaimi, A. A. and W. D. Wan Rosli (2017). Isolation and Characterization of Nanocrystalline Cellulose from Totally Chlorine Free Oil Palm Empty Fruit Bunch Pulp. Journal of Polymers and the Environment, 25(2); 427–437
Astari, L., S. Sudarmanto, S. S. Kusumah, F. Akbar, and K. W. Prasetiyo (2019). Quality of Particleboard Made from Rattan Waste. In IOP Conference Series: Earth and Environmental Science, volume 374. page 012009
Balakrishnan, P., S. Gopi, V. G. Geethamma, N. Kalarikkal, and S. Thomas (2018). Cellulose Nanofiber vs Nanocrystals from Pineapple Leaf Fiber: A Comparative Study on Reinforcing Efficiency on Starch Nanocomposites. Macromolecular Symposia, 380(1); 1800102
Cheng, M., Z. Qin, Y. Liu, Y. Qin, T. Li, L. Chen, and M. Zhu (2014). Efficient Extraction of Carboxylated Spherical Cellulose Nanocrystals with Narrow Distribution Through Hydrolysis of Lyocell Fibers by Using Ammonium Persulfate as an Oxidant. Journal of Materials Chemistry A, 2(1); 251–258
Ding, L., X. Han, L. Cao, Y. Chen, Z. Ling, J. Han, S. He, and S. Jiang (2022). Characterization of Natural Fiber from Manau Rattan (Calamus manan) as a Potential Reinforcement for Polymer-Based Composites. Journal of Bioresources and Bioproducts, 7(3); 190–200
Dungani, R., M. I. Bakshi, T. Z. Hanifa, M. Dew, F. A. Syamani, M. Mahardika, and W. Fatriasari (2024). Isolation and Characterization of Cellulose Nanofiber (CNF) from Kenaf (Hibiscus cannabinus) Bast Through the Chemo-Mechanical Process. Journal of Renewable Materials, 12(6); 1057–1069
Khalil, H. P. S. A., A. F. I. Yusra, A. H. Bhat, and M. Jawaid (2010). Cell Wall Ultrastructure, Anatomy, Lignin Distribution, and Chemical Composition of Malaysian Cultivated Kenaf Fiber. Industrial Crops and Products, 31(1); 113–121
Khanjanzadeh, H. and B. D. Park (2020). Characterization of Carboxylated Cellulose Nanocrystals from Recycled Fiberboard Fibers Using Ammonium Persulfate Oxidation. Journal of the Korean Wood Science and Technology, 48(2); 231–244
Megashah, L. N., H. Ariffin, M. R. Zakaria, and M. A. Hassan (2018). Properties of Cellulose Extract from Different Types of Oil Palm Biomass. IOP Conference Series: Materials Science and Engineering, 368(1); 012049
Mikulcová, V., R. Bordes, A. Minarík, and V. Kašpárková (2018). Pickering Oil-In-Water Emulsions Stabilized by Carboxylated Cellulose Nanocrystals—Effect of the pH. Food Hydrocolloids, 80; 60–67
Mi’rajunnisa, H. S., H. Suryadi, Sutriyo, and Y. P. I. Lestari (2023). Isolation of Cellulase from Selected Fungal Strains and Its Use for Manufacture Microcrystal Cellulose from Kapuk Cortex (Ceiba pentandra (L.) Gaertn). Science and Technology Indonesia, 8(2); 227–234
Montoya-Escobar, N., D. Ospina-Acero, J. A. Velásquez-Cock, C. Gómez-Hoyos, A. S. Guerra, P. F. G. Rojo, L. M. V. Acosta, J. P. Escobar, N. Correa-Hincapié, O. Triana-Chávez, R. Z. Gallego, and P. M. Stefani (2022). Use of Fourier Series in X-Ray Diffraction (XRD) Analysis and Fourier-Transform Infrared Spectroscopy (FTIR) for Estimation of Crystallinity in Cellulose from Different Sources. Polymers, 14(23); 5199
Nascimento, D. M. D., J. S. Almeida, M. do S. Vale, R. C. Leitão, C. R. Muniz, M. C. B. de Figueirêdo, J. P. S. Morais, and M. de F. Rosa (2016). A Comprehensive Approach for Obtaining Cellulose Nanocrystal from Coconut Fiber. Part I: Proposition of Technological Pathways. Industrial Crops and Products, 93; 66–75
Nasrudin, R. F., N. Samat, N. A. Mokhtar, and N. Yacob (2022). Production of Cellulose Nanocrystals from Oil Palm Empty Fruit Bunch and Pineapple Leaf Fibre Using Double Oxidation Approach. Jurnal Teknologi, 84(5); 73–81
Nechyporchuk, O., M. N. Belgacem, and J. Bras (2016). Production of Cellulose Nanofibrils: A Review of Recent Advances. Industrial Crops and Products, 93; 2–25
Oun, A. A. and J.-W. Rhim (2017). Characterization of Carboxymethyl Cellulose-Based Nanocomposite Films Reinforced with Oxidized Nanocellulose Isolated Using Ammonium Persulfate Method. Carbohydrate Polymers, 174; 484–492
Padzil, F. N. M., S. H. Lee, Z. M. A. Ainun, C. H. Lee, and L. C. Abdullah (2020). Potential of Oil Palm Empty Fruit Bunch Resources in Nanocellulose Hydrogel Production for Versatile Applications: A Review. Materials, 13(5); 1245
Rahmatullah, R., R. W. Putri, M. Rendana, U. Waluyo, and T. Andrianto (2022). Effect of Plasticizer and Concentration on Characteristics of Bioplastic Based on Cellulose Acetate from Kapok (Ceiba pentandra) Fiber. Science and Technology Indonesia, 7(1); 73–83
Rana, A. K., E. Frollini, and V. K. Thakur (2021). Cellulose Nanocrystals: Pretreatments, Preparation Strategies, and Surface Functionalization. International Journal of Biological Macromolecules, 182; 1554–1581
Razab, M. K. A. A., R. S. M. Ghani, F. A. M. Zin, N. A. A. N. Yusoff, and A. M. Noor (2022). Isolation and Characterization of Cellulose Nanofibrils from Banana Pseudostem, Oil Palm Trunk, and Kenaf Bast Fibers Using Chemicals and High-Intensity Ultrasonication. Journal of Natural Fibers, 19(13); 5537–5550
Sabaruddin, F. A., P. M. Tahir, S. M. Sapuan, R. A. Ilyas, S. H. Lee, K. Abdan, N. Mazlan, A. S. M. Roseley, and H. P. S. A. Khalil (2021). The Effects of Unbleached and Bleached Nanocellulose on the Thermal and Flammability of Polypropylene-Reinforced Kenaf Core Hybrid Polymer Bionanocomposites. Polymers, 13(1); 1–19
Samat, N., R. F. Nasrudin, and N. S. Engliman (2022). Fabrication of Poly(vinyl) Alcohol-Cellulose Nanocrystal Hybrid Aerogel. Materials Science Forum, 1074; 11–16
Samat, N., M. A. Sulaiman, Z. Ahmad, and H. Anuar (2021). A Comparative Study on the Desiccant Effect of Polypropylene and Polylactic Acid Composites Reinforced with Different Lignocellulosic Fibres. Journal of Applied Science and Engineering, 24(2); 223–231
Segal, L., J. J. Creely, A. E. Martin Jr, and C. M. Conrad (1959). An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-Ray Diffractometer. Textile Research Journal, 29(10); 786–794
Shanmugam, K., N. Chandrasekar, and R. Balaji (2023). Barrier Performance of Spray Coated Cellulose Nanofibre Film. Micro, 3(1); 192–207
Song, Y., W. Jiang, Y. Zhang, H. Wang, F. Zou, K. Yu, and G. Han (2018). A Novel Process of Nanocellulose Extraction from Kenaf Bast. Materials Research Express, 5(8); 085032
Sulaiman, S., M. N. Mokhtar, M. N. Naim, A. S. Baharuddin, M. A. M. Salleh, and A. Sulaiman (2015). Study on the Preparation of Cellulose Nanofibre (CNF) from Kenaf Bast Fibre for Enzyme Immobilization Application. Sains Malaysiana, 44(11); 1541–1550
Syazwani, N. S., M. N. E. Efzan, C. K. Kok, and M. J. Nurhidayatullaili (2022). Analysis on Extracted Jute Cellulose Nanofibers by Fourier Transform Infrared and X-Ray Diffraction. Journal of Building Engineering, 48; 103744
Toni, N. M. M. and S. Mahzan (2021). Influences of Chemical Treatment on Mechanical Properties of Rattan. Research Progress in Mechanical and Manufacturing Engineering, 2(2); 590–598
Vu, A. N., L. H. Nguyen, K. Yoshimura, T. D. Tran, and H. V. Le (2024). Cellulose Nanocrystals Isolated from Sugarcane Bagasse Using the Formic/Peroxyformic Acid Process: Structural, Chemical, and Thermal Properties. Arabian Journal of Chemistry, 17(8); 105841
Wahab, R., N. Mokhtar, R. S. Mohd Ghani, and M. S. Sulaiman (2019). An Overview of Rattan Industry Status and Its Economic Aspect in Setting Up Rattan-Based Industry in Malaysia. e-BANGI: Jurnal Sains Sosial dan Kemanusiaan, 16(3); 1–10
Wahib, S. A., D. A. Da’na, and M. A. Al-Ghouti (2022). Insight into the Extraction and Characterization of Cellulose Nanocrystals from Date Pits. Arabian Journal of Chemistry, 15(3); 103650
Zhang, K., P. Sun, H. Liu, S. Shang, J. Song, and D. Wang (2016). Extraction and Comparison of Carboxylated Cellulose Nanocrystals from Bleached Sugarcane Bagasse Pulp Using Two Different Oxidation Methods. Carbohydrate Polymers, 138; 237–243
Zuraida, A., T. Maisarah, A. Zahurin, A. M. Luqman, R. Wan Yussof, W. Wan Shazlin Maisarah, and A. Marjan (2015). Structural Examination and Elemental Composition Analysis of Rattan Waste Fibers for Binderless Board Application. Malaysian Journal of Microscopy, 11; 39–44
Authors
Samat, N., Roshidi, M. A. R. M. ., Onn, D. N. A. D. R. ., Hatta, M. A. M. ., & Sabaruddin, F. A. . (2025). Synergistic Effects of Double Oxidation on the Extraction and Characterization of Crystalline Nanocellulose from Rattan Waste and Kenaf Fiber. Science and Technology Indonesia, 10(2), 411–419. https://doi.org/10.26554/sti.2025.10.2.411-419
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