Abstract
The production of cellulose nanocrystals (CNC) from biomass involves pretreatment, CNC synthesis, and post-synthesis purification. Information on quality variation during the different stages of pretreatment and CNC synthesis is well documented; however, the post-synthesis purification stage has received little attention. In this study, characteristic variations of CNC during the post-synthesis purification process were investigated. The stages in the process were washing (first and second), neutralization, and centrifugation. CNC’s yield decreased after the second washing and neutralization. Cellobiose and cellotriose were detected in the supernatants after the first and second washings. After neutralization, CNC showed a higher colloidal dispersion compared to the first and the second washings. The dimension, morphological, and structural properties were moderately altered during the purification process. Crystallinity increased while crystallite size reduced as CNC purification progressed. The CtCBD3 bound to CNC’s surface reduced by 24.27% after the second washing and increased by 47.44% after neutralization. The results in this study provide comprehensive information regarding the overall changes in CNC’s characteristics during its purification.
Similar content being viewed by others
Data and materials availability
All data generated or analyzed during this study are included in this article.
References
Shaghaleh H, Xu X, Wang S (2018) Current progress in production of biopolymeric materials based on cellulose, cellulose nanofibers, and cellulose derivatives. RSC Adv 8:825–842
Thomas B, Raj MC, Athira KB, Rubiyah MH, Joy J, Moores A, Drisko GL, Sanchez C (2018) Nanocellulose, a versatile green platform: from biosources to materials and their applications. Chem Rev 118:11575–11625
Catori DM, Fragal EH, Messias I, Garcia FP, Nakamura CV, Rubira AF (2021) Development of composite hydrogel based on hydroxyapatite mineralization over pectin reinforced with cellulose nanocrystal. Int J Biol Macromol 167:726–735
Chinta ML, Velidandi A, Pabbathi NPP, Dahariya S, Parcha SR (2021) Assessment of properties, applications and limitations of scaffolds based on cellulose and its derivatives for cartilage tissue engineering: a review. Int J Biol Macromol 175:495–515
Huang S, Tao R, Ismail A, Wang Y (2020) Cellulose nanocrystals derived from textile waste through acid hydrolysis and oxidation as reinforcing agent of soy protein film. Polymers 12:958
Vanderfleet OM, Cranston ED (2020) Production routes to tailor the performance of cellulose nanocrystals. Nat Rev Mater 6:124–144
Brinkmann A, Chen M, Couillard M, Jakubek ZJ, Leng T, Johnston LJ (2016) Correlating cellulose nanocrystal particle size and surface area. Langmuir 32:6105–6114
Cheng M, Qin Z, Hu J, Liu Q, Wei T, Li W, Ling Y, Liu B (2020) Facile and rapid one–step extraction of carboxylated cellulose nanocrystals by H2SO4/HNO3 mixed acid hydrolysis. Carbohydr Polym 231:115701
So BR, Yeo HJ, Lee JJ, Jung YH, Jung SK (2021) Cellulose nanocrystal preparation from Gelidium amansii and analysis of its anti-inflammatory effect on the skin in vitro and in vivo. Carbohydr Polym 254:117315
Gupta GK, Shukla P (2020) Lignocellulosic biomass for the synthesis of nanocellulose and its eco-friendly advanced applications. Front Chem 8:601256
Benito-Gonzalez I, Lopez-Rubio A, Gavara R, Martınez-Sanz M (2019) Cellulose nanocrystal-based films produced by more sustainable extraction protocols from Posidonia oceanica waste biomass. Cellulose 26:8007–8024
Grishkewich N, Mohammed N, Tang J, Tam KC (2017) Recent advances in the application of cellulose nanocrystals. Curr Opin Colloid Interface Sci 29:32–45
Tang J, Sisler J, Grishkewich N, Tam KC (2017) Functionalization of cellulose nanocrystals for advanced applications. J Colloid Interface Sci 494:397–409
Xiao Y, Kang S, Liu Y, Guo X, Li M, Xu H (2021) Effect and mechanism of calcium ions on the gelation properties of cellulose nanocrystals-whey protein isolate composite gels. Food Hydrocoll 111:106401
Hernandez CC, Ferreira FF, Rosa DS (2018) X-ray powder diffraction and other analyses of cellulose nanocrystals obtained from corn straw by chemical treatments. Carbohydr Polym 193:39–44
Luzi F, Puglia D, Sarasini F, Tirillò J, Maffei G, Zuorro A, Lavecchia R, Kenny JM, Torre L (2019) Valorization and extraction of cellulose nanocrystals from North African grass: Ampelodesmos mauritanicus (Diss). Carbohydr Polym 209:328–337
Wang J, Xu J, Zhu S, Wu Q, Li J, Gao Y, Wang B, Li J, Gao W, Zeng J, Chen K (2021) Preparation of nanocellulose in high yield via chemi-mechanical synergy. Carbohydr Polym 251:117094
Duan CJ, Huang MY, Pang H, Zhao J, Wu CX, Feng JX (2017) Characterization of a novel theme C glycoside hydrolase family 9 cellulase and its CBM-chimeric enzymes. Appl Microbiol Biotechnol 101:5723–5737
Liu T, Zhang Y, Lu X, Wang P, Zhang X, Tian J, Wang Q, Song J, Jin Y, Xiao H (2021) Binding affinity of family 4 carbohydrate binding module on cellulose films of nanocrystals and nanofibrils. Carbohydr Polym 251:116725
Oliveira C, Romani A, Gomes D, Cunha JT, Gama FM, Domingues L (2018) Recombinant family 3 carbohydrate-binding module as a new additive for enhanced enzymatic saccharification of whole slurry from autohydrolyzed Eucalyptus globulus wood. Cellulose 25:2505–2514
Maharjan A, Alkotaini B, Kim BS (2018) Fusion of carbohydrate binding modules to bifunctional cellulase to enhance binding affinity and cellulolytic activity. Biotechnol Bioprocess Eng 23:79–85
Kim IJ, Ko HJ, Kim TW, Nam KH, Choi IG, Kim KH (2013) Binding characteristics of a bacterial expansin (BsEXLX1) for various types of pretreated lignocellulose. Appl Microbiol Biotechnol 97:5381–5388
Kim IJ, Ko H, Kim T, Choi CI, Kim KH (2013) Characteristics of the binding of a bacterial expansin (BsEXLX1) to microcrystalline cellulose. Biotechnol Bioeng 110:401–407
Hashimoto H (2006) Recent structural studies of carbohydrate-binding modules. Cell Mol Life Sci 63:2954–2967
Nishida Y, Suzuki K, Kumagai Y, Tanaka H, Inoue A, Ojima T (2007) Isolation and primary structure of a cellulase from the Japanese sea urchin strongylocentrotus nudus. Biochimie 89:1002–1011
Gong J, Li J, Xu J, Xiang Z, Mo L (2017) Research on cellulose nanocrystals produced from cellulose sources with various polymorphs. RSC Adv 7:33486–33493
Pandi N, Sonawane SH, Kishore KA (2021) Synthesis of cellulose nanocrystals (CNCs) from cotton using ultrasound-assisted acid hydrolysis. Ultrason Sonochem 70:105353
Wu Q, Xu J, Zhu S, Kuanga Y, Wang B, Gao W (2020) Crystalline stability of cellulose III nanocrystals in the hydrothermal treatment and NaOH solution. Carbohydr Polym 249:11682
Jiang H, Wu Y, Han B, Zhang Y (2017) Effect of oxidation time on the properties of cellulose nanocrystals from hybrid poplar residues using the ammonium persulfate. Carbohydr Polym 174:291–298
Jung YH (2017) Trends and prospects of microfibrillated cellulose in bio-industries. Microbiol Biotechnol Lett 45:1–11
Melikoğlu AY, Bilek SE, Cesur S (2019) Optimum alkaline treatment parameters for the extraction of cellulose and production of cellulose nanocrystals from apple pomace. Carbohydr Polym 215:330–337
Qiao C, Chen G, Zhang J, Yao J (2016) Structure and rheological properties of cellulose nanocrystals suspension. Food Hydrocoll 55:19–25
Park S, Baker JO, Himmel ME, Parilla PA, Johnson DK (2010) Cellulose crystallinity index: measurement techniques and their impact on interpreting cellulase performance. Biotechnol Biofuels 3:10
El-Achaby M, Kassab Z, Aboulkas A, Gaillard C, Barakat A (2018) Reuse of red algae waste for the production of cellulose nanocrystals and its application in polymer nanocomposites. Int J Biol Macromol 106:681–691
Aguayo MG, Perez AF, Reyes G, Oviedo C, Gacitúa W, Gonzalez R, Uyarte O (2018) Isolation and characterization of cellulose nanocrystals from rejected fibers originated in the kraft pulping process. Polymers 10:1145
Chieng BW, Lee SH, Ibrahim NA, Then YY, Loo YY (2017) Isolation and characterization of cellulose nanocrystals from oil palm mesocarp fiber. Polymers 9:355
Lamaming J, Hashim R, Leh CP, Sulaiman O, Sugimoto T, Nasir M (2015) Isolation and characterization of cellulose nanocrystals from parenchyma and vascular bundle of oil palm trunk (Elaeis guineensis). Carbohydr Polym 134:534–540
Acknowledgments
This work was supported by the National Research Foundation of Korea (NRF) grant funded by Korean government (Ministry of Science and ICT, MSIT; No 2020R1C1C1005251).
Author information
Authors and Affiliations
Contributions
HJY performed most experiments, conducted statistical analysis and contributed in writing the draft manuscript. OEA performed statistical analysis, interpreted data and wrote the draft manuscript. MDK, HSO, and HSP performed part of the experiments. MS conducted statistical analysis and performed part of the experiment. DHK reviewed and revised the draft manuscript. YHJ conceived the idea, acquired fund, supervised the project, reviewed, and revised the manuscript. All authors read and approved the final manuscript.
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that they have no known competing financial interest or personal relationship that could have influenced the findings reported in this paper.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Rights and permissions
About this article
Cite this article
Yeo, H.J., Adedeji, O.E., Kang, M.D. et al. Tracing characteristic variations of cellulose nanocrystals during the post-synthesis purification process. Polym. Bull. 80, 1531–1544 (2023). https://doi.org/10.1007/s00289-022-04121-5
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00289-022-04121-5