Isolation and Characterization of Cellulose Nanofibrils (CNF) from Dates by-Product via Citric Acid Hydrolysis
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Keywords:
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Cellulose Nanofibrils , Citric Acid , Concentration , Dates by-Product , Hydrolysis
Abstract
Industrial residues that are not optimally utilized are removed by burning, landfilling, or dumping, which can threaten the environment and health. In fact, part of this agro-industrial waste still has content that has the potential to become raw material for value-added other industries. Dates by-product as residue of the fiber-rich fruit industry have the potential to be a source of nanocellulose. This study aims to obtain nanofibril cellulose (CNF) isolates from dates by-product via citric acid hydrolysis, and investigate the effect of acid concentration on the unknown dates by-product CNF isolate characteristics. Pretreatment such as delignification and bleaching is needed to obtain cellulose isolate with high purity. Furthermore, acid hydrolysis, centrifugation, and sonication are performed to obtain CNF. CNF isolates are characterized by the analysis of particle size distribution, morphology, and crystallinity. Analysis of functional groups and lignocellulose content test confirm that lignin and hemicellulose are degraded during isolation. The particle size distribution measurement shows that the greater the acid concentration, the smaller the CNF size and the better the size uniformity. The morphology of the CNF obtained is net-like fibers. The degree of crystallinity shown decreases with increasing acid concentration. This study revealed that different citric acid concentrations can result in different characteristics of CNF isolates.
References
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Ghnimi, S., S. Umer, A. Karim, and A. Kamal-Eldin (2017). Date Fruit (Phoenix dactylifera L.): An Underutilized Food Seeking Industrial Valorization. NFS Journal, 6; 1–10.
Ginting, S. K. and R. Mohadi (2017). Adsorption of Congo Red Using Kaolinite-Cellulose Adsorbent. Science and Technology Indonesia, 2(2); 29–36.
Hosseini, M., H. Z. Dizaji, M. Taghavi, and A. A. Babaei (2018). Extraction of Cellulose Nanofibril (CNF) from Agricultural Residues. In Proceedings of the 7th International Conference on Nanostructures (ICNS7).
Jadaun, S., U. Sharma, R. Khapudang, and S. Siddiqui (2023). Biodegradable Nanocellulose Reinforced Biocomposites for Food Packaging – A Narrative Review and Future Perspective. Journal of Water and Environmental Technology, 8(3); 293–319.
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Klemm, D., B. Phillipp, T. Heinze, and W. Wagenknecht (1998). Comprehensive Cellulose Chemistry: Fundamentals and Analytical Methods. Wiley.
Lestari, Y. P. I., Y. Falya, U. Chasanah, D. W. Kusumo, and M. Bethasari (2022). Isolation of α-Cellulose, Manufacture & Characterization of Microcrystalline Cellulose (MCC) from Baby Orange Peel Waste (Citrus sinensis). Pharmaceutical and Pharmacology Magazine, 26(3); 119–123.
Liu, C., H. Du, G. Yu, Y. Zhang, Q. Kong, B. Li, and X. Mu (2017). Simultaneous Extraction of Carboxylated Cellulose Nanocrystals and Nanofibrils via Citric Acid Hydrolysis – A Sustainable Route. Paper and Biomaterial, 2(4); 19–26.
Lynch, J., Cain, M., Frame, D., & Pierrehumbert, R. (2021). Agriculture’s Contribution to Climate Change and Role in Mitigation is Distinct From Predominantly Fossil CO2-Emitting Sectors. Frontiers in Sustainable Food Systems, 4(518039), 1–9.
Malachowska, E., Dubowik, M., Lipkiewicz, A., Przybysz, K., & Przybysz, P. (2020). Analysis of Cellulose Pulp Characteristics and Processing Parameters for Efficient Paper Production. Sustainability, 12(17), 7219.
Mariño, M. A., Cypriano, D., & Tasic, L. (2021). Agroindustry Residues as a Source for Cellulose Nanofibers Production. Journal of Brazilian Chemical Society, 32(4), 878–888.
Mirzaee, N., Nikzad, M., Battisti, R., & Araghi, A. (2023). Isolation of Cellulose Nanofibers from Rapeseed Straw via Chlorine-Free Purification Method and its Application as Reinforcing Agent in Carboxymethyl Cellulose-Based Films. International Journal of Biological Macromolecules, 251, 126405.
Mrabet, A., Hammadi, H., Rodríguez-Arcos, R., Jimenez-Araujo, A., & Sindic, M. (2019). Date Palm Fruits as a Potential Source of Functional Dietary Fiber: A Review. Food Science and Technology Research, 25(1), 1–10.
Mrabet, A., Rodríguez-Arcos, R., Guillen-Bejarano, R., Chaira, N., Frechichi, A., & Jimenez-Araujo, A. (2012). Dietary Fiber from Tunisian Common Date Cultivars (Phoenix dactylifera L.): Chemical Composition, Functional Properties, and Antioxidant Capacity. Journal of Agricultural and Food Chemistry, 60, 3658–3664.
Pavalaydon, K., Ramasawmy, H., & Surroo, D. (2022). Comparative Evaluation of Cellulose Nanocrystals from Bagasse and Coir Agro Wastes for Reinforcing PVA Based Composites. Environment, Development and Sustainability, 24, 9963–9984.
Pinto, E., Aggrey, W. N., Boakye, P., Amenuvor, G., Sokama-Neuyam, Y., Fokuo, M. K., Karimaie, H., Sarkodie, K., Adenutsi, C. D., Erzuah, S., & Rockson, M. A. D. (2022). Cellulose Processing from Biomass and its Derivatization into Carboxymethylcellulose: A Review. Scientific African, 15, e01078.
Prasetia, I. G. N. J. A., Deviana, S., Damayanti, T., Cahyadi, A., & Wirasuta, I. M. A. G. (2018). The Effect of NaOH Concentration in Delignification Process on Microcrystalline Cellulose from Green Algae (Cladophora sp.) as the Renewable Marine Product. Journal of Pharmaceutical Science and Society, 15(2), 68–71.
Rahmatullah, R., Putri, K., Rendana, M., Waluyo, U., & Andrianto, T. (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, M. S., Rahim, M. A., Mosharraf, M. P., Tipu, M. F. K., Chowdhury, J. A., Haque, M. R., Kabir, S., Amran, M. S., & Chowdhury, A. A. (2023). Morphological, Spectroscopic and Thermal Analysis of Cellulose Nanocrystals Extracted from Waste Jute Fiber by Acid Hydrolysis. Polymers, 15, 1530.
Santhi, M., Arnata, I. W., & Wrasiati, L. P. (2022). Isolation of Cellulose from Coconut Fiber (Cocos nucifera L.) at Variation of Temperature and Time of Bleaching Process with Peracetic Acid. Journal of Agroindustrial Engineering and Management, 10(3), 248–258.
Segal, L., Creely, J. J., Martin, A. E. J., & Conrad, C. M. (1959). An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-Ray Diffractometer. Textile Research Journal, 29, 786–794.
Sena, P. W., Putra, G. P. G., & Suhendra, L. (2021). Characterization of Cellulose from the Skin of Cocoa Fruit (Theobroma Cacao L.) at Various Concentrations of Hydrogen Peroxide and Bleaching Process Temperatures. Journal of Agroindustrial Engineering and Management, 9(3), 288–299.
Tang, P., & Sun, G. (2017). Generation of Hydroxyl Radicals and Effective Whitening of Cotton Fabrics by H2O2 Under UVB Irradiation. Carbohydrate Polymers, 160, 153–162.
Umaningrum, D., Nurmasari, R., Astuti, M. D., Mardhatillah, M., Mulyasuryani, A., & Mardiana, D. (2018). Isolation of Cellulose from Rice Straw Using Variations in Base Concentration. Journal of Science and Applied Chemistry, 12(1), 25.
Van Soest, P. J., Robertson, J. B., & Lewis, B. A. (1991). Methods for Dietary Fiber Neutral Detergent Fiber, and Nonstarch Polysaccharides in Relation to Animal Nutrition. Journal Dairy Science, 74, 3583–3597.
Wang, T., Jung, J., & Zhao, Y. (2022). Isolation, Characterization, and Applications of Holocellulose Nanofibers From Apple and Rhubarb Pomace Using Eco-Friendly Approach. Food and Bioproducts Processing, 136, 166–175.
Widiarto, S., Pramono, E., Suharso, Rochliadi, A., & Arcana, I. M. (2019). Cellulose Nanofibers Preparation from Cassava Peels via Mechanical Disruption. Fibers, 7(5), 44.
Wu, Q., Meng, Y., Wang, S., Li, Y., Fu, S., Ma, L., & Harper, D. (2014). Rheological Behavior of Cellulose Nanocrystal Suspension: Influence of Concentration and Aspect Ratio. Journal of Applied Polymer Science, 131(15), 40525.
Wu, Y., Wu, J., Yang, F., Tang, C., & Huang, Q. (2019). Effect of H2O2 Bleaching Treatment on the Properties of Finished Transparent Wood. Polymers, 11(5), 776.
Yu, M., Yang, R., Huang, L., Cao, X., Yang, F., & Liu, D. (2012). Preparation and Characterization of Bamboo Nanocrystalline Cellulose. BioResources, 7(2), 1802–1812.
Yurdacan, H. M., & Sari, M. M. (2021). Sustainable Materials for Transitional and Alternative Energy. Gulf Professional Publishing.
Yuwono, S. D., Nahrowi, R., Setiawan, A., Juliasih, N. L. G. R., Sukmana, I., Simajuntak, W., & Hadi, S. (2022). Synthesis of Cellulose–Polylactic Acid Microcapsule as a Delivery Agent of Rifampicin. Science and Technology Indonesia, 7(3), 263–268.
Amorim, J. D. P., H. A. Nascimento, C. J. G. S. Junior, A. D. M. Medeiros, I. D. L. Silva, A. F. S. Costa, G. M. Vinhas, and L. A. Sarubbo (2021). Obtainment of Bacterial Cellulose with Added Propolis Extract for Cosmetic Applications. Polymer Engineering and Science, 62(2); 565–575.
Arnata, I. W., S. Suprihatin, F. Fahma, N. Richana, and T. C. Sunarti (2020). Cationic Modification of Nanocrystalline Cellulose From Sago Fronds. Cellulose, 27(6); 3121–3141.
Attia, A. I., F. M. Reda, A. K. Patra, S. S. Elnesr, Y. A. Attia, and M. Alagawany (2021). Date (Phoenix dactylifera L.) By-Products: Chemical Composition, Nutritive Value And Applications In Poultry Nutrition, An Updating Review. Animals, 1(4); 1133.
Azeredo, H. M. C., L. H. C. Mattoso, D. Wood, T. G. Williams, R. J. Avena-Bustillos, and T. H. McHugh (2009). Nanocomposite Edible Films from Mango Puree Reinforced with Cellulose Nanofibers. Journal of Food Science, 74(5); 31–35.
Barbash, V. A., O. V. Yaschenko, S. V. Alushkin, A. S. Kondratyuk, O. Y. Posudievsky, and V. G. Koshechko (2016). The Effect of Mechanochemical Treatment of the Cellulose on Characteristics of Nanocellulose Films. Nanoscale Research Letters, 11; 410.
Blanco, A., M. C. Monte, C. Campano, A. Balea, N. Merayo, and C. Negro (2018). Nanocellulose for Industrial Use: Cellulose Nanofibers (CNF), Cellulose Nanocrystals (CNC), and Bacterial Cellulose (BC). In Handbook of Nanomaterials for Industrial Applications. Elsevier.
Bondancia, T. J., J. de Aguiar, G. Batista, A. J. G. Cruz, J. M. Marconcini, L. H. C. Mattoso, and C. S. Farinas (2020). Production of Nanocellulose Using Citric Acid in a Biorefinery Concept: Effect of the Hydrolysis Reaction Time and Techno-Economic Analysis. Industrial & Engineering Chemistry Research, 59(25); 11505–11516.
Bruel, C., T. S. Davies, P. J. Carreau, J. R. Tavares, and M. C. Heuzey (2020). Self-assembly Behaviors of Colloidal Cellulose Nanocrystals: A Tale of Stabilization Mechanisms. Journal of Colloid and Interface Science, 574; 399–409.
Capanoglu, E., E. Nemli, and F. Tomas-Barberan (2022). Novel Approaches in the Valorization of Agricultural Wastes and their Applications. Journal of Agricultural and Food Chemistry, 70(23); 6787–6804.
Chen, L., Y. Wu, Y. Guo, X. Yan, W. Liu, and S. Huang (2024). Preparation and Characterization of Soluble Dietary Fiber Edible Packaging Films Reinforced by Nanocellulose from Navel Orange Peel Pomace. Polymers, 16(3); 315.
Coelho, C. C. S., M. Michelin, M. A. Cerqueira, C. Goncalves, R. V. Tonon, L. M. Pastrana, O. Freitas-Silva, A. A. Vicente, L. M. C. Cabral, and J. A. Teixeira (2018). Cellulose Nanocrystals from Grape Pomace: Production, Properties and Cytotoxicity Assessment. Carbohydrate Polymers, 195; 327–336.
Danaei, M., M. Dehghankhold, S. Ataei, F. H. Davarani, R. Javanmard, A. Dokhani, S. Khorasani, and M. R. Mozafari (2018). Impact of Particle Size and Polydispersity Index on the Clinical Applications of Lipidic Nanocarrier Systems. Pharmaceutics, 10(2); 57.
Dutra, E. D., F. A. Santos, B. R. A. Alencar, A. L. S. Reis, R. F. R. de Souza, K. A. S. Aquino, M. A. M. Jr, and R. S. C. Menezes (2017). Alkaline Hydrogen Peroxide Pretreatment of Lignocellulosic Biomass: Status and Perspectives. Biomass Conversion and Biorefinery, 8(1); 1–10.
Fan, J., S. Zhang, F. Li, and J. Shi (2020). Cellulose-based Sensors for Metal Ions Detection. Cellulose, 27; 5477–5507.
Food and Agriculture Organization of the United Nations (2022). World Food and Agriculture - Statistical Yearbook 2022.
France, K. J. D., T. Hoare, and E. D. Cranston (2017). Review of Hydrogels and Aerogels Containing Nanocellulose. Chemistry of Materials, 29; 4609–4631.
Ghnimi, S., S. Umer, A. Karim, and A. Kamal-Eldin (2017). Date Fruit (Phoenix dactylifera L.): An Underutilized Food Seeking Industrial Valorization. NFS Journal, 6; 1–10.
Ginting, S. K. and R. Mohadi (2017). Adsorption of Congo Red Using Kaolinite-Cellulose Adsorbent. Science and Technology Indonesia, 2(2); 29–36.
Hosseini, M., H. Z. Dizaji, M. Taghavi, and A. A. Babaei (2018). Extraction of Cellulose Nanofibril (CNF) from Agricultural Residues. In Proceedings of the 7th International Conference on Nanostructures (ICNS7).
Jadaun, S., U. Sharma, R. Khapudang, and S. Siddiqui (2023). Biodegradable Nanocellulose Reinforced Biocomposites for Food Packaging – A Narrative Review and Future Perspective. Journal of Water and Environmental Technology, 8(3); 293–319.
Jakubek, Z. J., M. Chen, M. Couillard, T. Leng, L. Liu, S. Zou, U. Baxa, J. D. Clogston, W. Y. Hamad, and L. J. Johnston (2018). Characterization Challenges for a Cellulose Nanocrystal Reference Material: Dispersion and Particle Size Distributions. Journal of Nanoparticle Research, 20(98); 1–16.
Khorairi, A. N. S. A., N. Sofian-Seng, R. Othaman, H. A. Rahman, N. S. M. Razali, S. J. Lim, and W. A. W. Mustapha (2021). A Review on Agro-industrial Waste as Cellulose and Nanocellulose Source and Their Potentials in Food Applications. Food Reviews International, 39(2); 663–688.
Klemm, D., B. Phillipp, T. Heinze, and W. Wagenknecht (1998). Comprehensive Cellulose Chemistry: Fundamentals and Analytical Methods. Wiley.
Lestari, Y. P. I., Y. Falya, U. Chasanah, D. W. Kusumo, and M. Bethasari (2022). Isolation of α-Cellulose, Manufacture & Characterization of Microcrystalline Cellulose (MCC) from Baby Orange Peel Waste (Citrus sinensis). Pharmaceutical and Pharmacology Magazine, 26(3); 119–123.
Liu, C., H. Du, G. Yu, Y. Zhang, Q. Kong, B. Li, and X. Mu (2017). Simultaneous Extraction of Carboxylated Cellulose Nanocrystals and Nanofibrils via Citric Acid Hydrolysis – A Sustainable Route. Paper and Biomaterial, 2(4); 19–26.
Lynch, J., Cain, M., Frame, D., & Pierrehumbert, R. (2021). Agriculture’s Contribution to Climate Change and Role in Mitigation is Distinct From Predominantly Fossil CO2-Emitting Sectors. Frontiers in Sustainable Food Systems, 4(518039), 1–9.
Malachowska, E., Dubowik, M., Lipkiewicz, A., Przybysz, K., & Przybysz, P. (2020). Analysis of Cellulose Pulp Characteristics and Processing Parameters for Efficient Paper Production. Sustainability, 12(17), 7219.
Mariño, M. A., Cypriano, D., & Tasic, L. (2021). Agroindustry Residues as a Source for Cellulose Nanofibers Production. Journal of Brazilian Chemical Society, 32(4), 878–888.
Mirzaee, N., Nikzad, M., Battisti, R., & Araghi, A. (2023). Isolation of Cellulose Nanofibers from Rapeseed Straw via Chlorine-Free Purification Method and its Application as Reinforcing Agent in Carboxymethyl Cellulose-Based Films. International Journal of Biological Macromolecules, 251, 126405.
Mrabet, A., Hammadi, H., Rodríguez-Arcos, R., Jimenez-Araujo, A., & Sindic, M. (2019). Date Palm Fruits as a Potential Source of Functional Dietary Fiber: A Review. Food Science and Technology Research, 25(1), 1–10.
Mrabet, A., Rodríguez-Arcos, R., Guillen-Bejarano, R., Chaira, N., Frechichi, A., & Jimenez-Araujo, A. (2012). Dietary Fiber from Tunisian Common Date Cultivars (Phoenix dactylifera L.): Chemical Composition, Functional Properties, and Antioxidant Capacity. Journal of Agricultural and Food Chemistry, 60, 3658–3664.
Pavalaydon, K., Ramasawmy, H., & Surroo, D. (2022). Comparative Evaluation of Cellulose Nanocrystals from Bagasse and Coir Agro Wastes for Reinforcing PVA Based Composites. Environment, Development and Sustainability, 24, 9963–9984.
Pinto, E., Aggrey, W. N., Boakye, P., Amenuvor, G., Sokama-Neuyam, Y., Fokuo, M. K., Karimaie, H., Sarkodie, K., Adenutsi, C. D., Erzuah, S., & Rockson, M. A. D. (2022). Cellulose Processing from Biomass and its Derivatization into Carboxymethylcellulose: A Review. Scientific African, 15, e01078.
Prasetia, I. G. N. J. A., Deviana, S., Damayanti, T., Cahyadi, A., & Wirasuta, I. M. A. G. (2018). The Effect of NaOH Concentration in Delignification Process on Microcrystalline Cellulose from Green Algae (Cladophora sp.) as the Renewable Marine Product. Journal of Pharmaceutical Science and Society, 15(2), 68–71.
Rahmatullah, R., Putri, K., Rendana, M., Waluyo, U., & Andrianto, T. (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, M. S., Rahim, M. A., Mosharraf, M. P., Tipu, M. F. K., Chowdhury, J. A., Haque, M. R., Kabir, S., Amran, M. S., & Chowdhury, A. A. (2023). Morphological, Spectroscopic and Thermal Analysis of Cellulose Nanocrystals Extracted from Waste Jute Fiber by Acid Hydrolysis. Polymers, 15, 1530.
Santhi, M., Arnata, I. W., & Wrasiati, L. P. (2022). Isolation of Cellulose from Coconut Fiber (Cocos nucifera L.) at Variation of Temperature and Time of Bleaching Process with Peracetic Acid. Journal of Agroindustrial Engineering and Management, 10(3), 248–258.
Segal, L., Creely, J. J., Martin, A. E. J., & Conrad, C. M. (1959). An Empirical Method for Estimating the Degree of Crystallinity of Native Cellulose Using the X-Ray Diffractometer. Textile Research Journal, 29, 786–794.
Sena, P. W., Putra, G. P. G., & Suhendra, L. (2021). Characterization of Cellulose from the Skin of Cocoa Fruit (Theobroma Cacao L.) at Various Concentrations of Hydrogen Peroxide and Bleaching Process Temperatures. Journal of Agroindustrial Engineering and Management, 9(3), 288–299.
Tang, P., & Sun, G. (2017). Generation of Hydroxyl Radicals and Effective Whitening of Cotton Fabrics by H2O2 Under UVB Irradiation. Carbohydrate Polymers, 160, 153–162.
Umaningrum, D., Nurmasari, R., Astuti, M. D., Mardhatillah, M., Mulyasuryani, A., & Mardiana, D. (2018). Isolation of Cellulose from Rice Straw Using Variations in Base Concentration. Journal of Science and Applied Chemistry, 12(1), 25.
Van Soest, P. J., Robertson, J. B., & Lewis, B. A. (1991). Methods for Dietary Fiber Neutral Detergent Fiber, and Nonstarch Polysaccharides in Relation to Animal Nutrition. Journal Dairy Science, 74, 3583–3597.
Wang, T., Jung, J., & Zhao, Y. (2022). Isolation, Characterization, and Applications of Holocellulose Nanofibers From Apple and Rhubarb Pomace Using Eco-Friendly Approach. Food and Bioproducts Processing, 136, 166–175.
Widiarto, S., Pramono, E., Suharso, Rochliadi, A., & Arcana, I. M. (2019). Cellulose Nanofibers Preparation from Cassava Peels via Mechanical Disruption. Fibers, 7(5), 44.
Wu, Q., Meng, Y., Wang, S., Li, Y., Fu, S., Ma, L., & Harper, D. (2014). Rheological Behavior of Cellulose Nanocrystal Suspension: Influence of Concentration and Aspect Ratio. Journal of Applied Polymer Science, 131(15), 40525.
Wu, Y., Wu, J., Yang, F., Tang, C., & Huang, Q. (2019). Effect of H2O2 Bleaching Treatment on the Properties of Finished Transparent Wood. Polymers, 11(5), 776.
Yu, M., Yang, R., Huang, L., Cao, X., Yang, F., & Liu, D. (2012). Preparation and Characterization of Bamboo Nanocrystalline Cellulose. BioResources, 7(2), 1802–1812.
Yurdacan, H. M., & Sari, M. M. (2021). Sustainable Materials for Transitional and Alternative Energy. Gulf Professional Publishing.
Yuwono, S. D., Nahrowi, R., Setiawan, A., Juliasih, N. L. G. R., Sukmana, I., Simajuntak, W., & Hadi, S. (2022). Synthesis of Cellulose–Polylactic Acid Microcapsule as a Delivery Agent of Rifampicin. Science and Technology Indonesia, 7(3), 263–268.
Authors
Aisy, L. A. R., Kemala, T., Suryanegara, L., & Purwaningsih, H. (2024). Isolation and Characterization of Cellulose Nanofibrils (CNF) from Dates by-Product via Citric Acid Hydrolysis. Science and Technology Indonesia, 9(4), 818–827. https://doi.org/10.26554/sti.2024.9.4.818-827
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