Cellulose Nanocrystals Isolated from Bean Seed Hulls: Acetylation and Characterization

Ebele Joy Morah *

Department of Pure and Industrial Chemistry, Nnamdi Azikiwe University, P.M.B 5025, Awka Anambra State, Nigeria.

David Okechukwu Okeke

Department of Applied Biochemistry, Nnamdi Azikiwe University, Awka, Nigeria.

Ozioma Juliana Anekwe-Nwekeaku

Department of Pure and Industrial Chemistry, Nnamdi Azikiwe University, P.M.B 5025, Awka Anambra State, Nigeria.

Chidinma Malinda Muobike

Department of Pure and Industrial Chemistry, Nnamdi Azikiwe University, P.M.B 5025, Awka Anambra State, Nigeria.

Uchechukwu Joachin Ezenyeaka

Department of Pure and Industrial Chemistry, Nnamdi Azikiwe University, P.M.B 5025, Awka Anambra State, Nigeria.

*Author to whom correspondence should be addressed.


Bean seed hulls is an agro-waste with abundant content of lignocellulosic materials but are being wasted due to its underutilization. Cellulose nanocrystals (CNCs) were successfully extracted from bean seed hulls using alkali treatment, bleaching and sulphuric acid hydrolysis. Cellulose triacetate (CTA) was obtained from CNCs by acetylation using acetic anhydride with sulphuric acid as catalyst. CNCs is neutral pH whereas CTA is slightly acidic. CNCs was sparingly soluble in ethanol but CTA was completely soluble in ethanol. CTA has a higher melting point than CNCs. The density of both CNCs and CTA is approximately equal to the density of water. SEM analysis revealed that CNCs is irregular and fragmented in nature and has both more large surface area and porosity than CTA. FTIR analysis showed the presence of the dominant functional groups such as O-H stretch, N-H stretch, C-H stretch, C-O stretch and C-N stretch in both CNCs and CTA. GC-MS analysis revealed the presence of the prevalent organic compounds such as alkanes, alcohols, phenols, alkanones, phthalates, carboxylic acids, esters and triterpene in both CNCs and CTA. Therefore, the isolation of CNCs from bean seed hulls suggests great efficacy to recover the under-utilized agro-wastes thereby preventing air pollution.

Keywords: Bean seed hulls, Isolation, cellulose nanocrystals, cellulose triacetate, Characterization

How to Cite

Morah, E. J., Okeke , D. O., Anekwe-Nwekeaku , O. J., Muobike , C. M., & Ezenyeaka , U. J. (2023). Cellulose Nanocrystals Isolated from Bean Seed Hulls: Acetylation and Characterization. Asian Journal of Applied Chemistry Research, 14(4), 54–76. https://doi.org/10.9734/ajacr/2023/v14i4276


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Nsude OP, Orie KJ. Thermodynamic and adsorption analysis of corrosion inhibition of mild steel in 0.5m hcl medium via ethanol extracts of phyllanthus mellerianus. American Journal of Applied Chemistry. 2022;10(3):67-75.

Auffhaminer M, Ramanathan V, Vincent J. Proceedings of the National Academy of Science. 2006;5(52):19668-19672.

Agarwal B. Gender and forest conservation: The impact of women’s participation in community forest governance. Ecological Economies. 2009;68(11):2785-2799.

Nwajiobi CC, Otaigbe J, Oriji O. Isolation and characterization of microcrystalline cellulose from papaya stem. Der Pharma Chemica. 2019;11(3):19-26.

Nsude OP, Orie KJ, Udeozo PI, Ogbobe O, Chime CC. Isolation, physicochemical and bet analysis of cellulose from pentaclethra macrophylla benth (oil bean). Pod Biomass Wastes International Research Journal of Pure and Applied Chemistry. 2022;23(5):9-22. DOI:10.9734/IRJPAC/2022/v23i530474.

Aridi AS, Yusuf YA, Nyuk LC, Ishak NA, Mohammad Yusuf YNN. Isolation of cellulose from leucaena, leucocephia mature pods and how different bleaching agents affect its characterization. Materials Performance and Characterization. 2022;11(1):236-243.

Onuegbu TC. Improving fuel wood efficiency in rural Nigeria: Briquette technology chemistry in Nigeria. A National Magazine in the Chemical Society of Nigeria. 2010;4(3):35-39.

Saha BC. Hemicellulose bioconversion. Journal of Industrial Microbiology and Biotechnology. 2003;30:279-291.

Candido RG, Godoy GG, Goncalves AR. Study on sugarcane bagasse pretreatment with sulphuric acid as a step of obtaining cellulose. WASET. 2012;61:101-105.

Bello A, Isa MT, Aderemi BO, Mukhtar B. Acetylation of cotton stalk for cellulose acetate production. American Scientific Research Journal for Engineering, Technology and Sciences (ASRJETS). 2016;15(1):137-150.

Malladi R, Nagalakshmaiah M, Robert M, Elkoun S. Importance of agricultural and industrial waste in the field of nanocellulose and recent industrial developments of wood based nanocellulose: A review. ACS Sustainable Chemistry & Engineering. 2018;1-70. DOI:10.1021/acssuschemeng.7b03437

Klemm D, Kramer F, Moritz S, Lindstrom T, Ankerfors M, Gray D, Dorris A. Nanocelluloses: A new family of nature-based materials. Angew. Chem. Int. Ed. 2011;50(24):5438-5466. DOI:10:1002/ anie.201001273

Finar IL. Organic chemistry: Stereochemistry and the chemistry of natural products. Vol 2, 5th Edition. Pearson Education Limited. 2014;350-353.

De Souza Lima MM, Borsali RR. Cellulose microcrystals: Structure, properties and applications. macromol. Rapid Commun. 2004;25(7):771-789. DOI: 10.1002/marc.200300268

Sheltami RM, Abdullah T, Ahmad I, Dufresne A, Kargarzadeh H. Extraction of cellulose nanocrystals from mengkuang leaves (Pananus tectorius). Carbohydrate Polymers. 2012;88(2):772-779. Available: https://doi.org/10.1016/j.carbpol.2012.01.062

Habibi Y, Lucia L, Rojas O. Cellulose nanocrystals: Chemistry self-assembling and applications chemical reviews. 2010;110(6):3479-3500. DOI:10.1021/cr900339w

He X, Luzi F, Yang W, Xiao Z, Torre L, Xie Y, Puglia D. Citric acid as green modifier for tuned hydrophilicity of surface modified cellulose and lignin nanoparticles. ACS Sustainable Chemistry and Engineering. 2018;6(8):9966-9978. Available: https://doi.org/10.1021/acssuschemeng.8b01202.

Plackett D, Sodergard A. Natural fibres, biopolymers and biocomposites. CRC Press, Boca Raton. 2005;569.

Yang W, Fortunate E, Luzi F, Kenny JM, Torre L, Puglia D. Lignocellulosic /based bionanocomposites for different industrial applications. Current Organic Chemistry. 2018;22(12):1205-1221. Available: https://doi.org/10.2174/1385272822666180515120948

Morrison RT, Boyd RN, Bhattacharjee SK. Organic chemistry. 8th Edition, Dorling Kindersley (India) Pvt. Ltd. 2018;1267:1274-1276.

Lamaming J, Hashim R, Leh CP, Sulaiman O, Sugimoto T, Nasir M. Isolation and characterization of cellulose nanocrystals from parenchyma and vascular bundle of oil palm trunk (Elaeis guineensis). Carbohydrate Polymers. 2012;88(2):772-779.

Luzi F, Puglia D, Sarasini F, Tirillo J, Maffei G, Zuorro A, Lavecchia R, Kenny JM, Torre L. Volarization and extraction of cellulose nanocystals from North African grass: Ampellodesmos mauritanicus (DISS). Carbohydrate Polymers. 2019;209:328-337. Available: https://doi.org/10.1016/j.carbpol.2019.01.048

Sacui IA, Nieuwendaal RC, Burnett DJ, Stranick SJ, Jorfi M, Weder C, Johan FE, Olsson RT, Gilman JW. Comparison of the properties of cellulose nanocrystals and cellulose nanofibrils isolated from bacteria, tunicate and wood processed using acid, enzymatic, mechanical and oxidative methods. ACS Applied Materials and Interfaces. 2014;6(9):6127- 6138. Available: https://doi.org/10.1021/am500359f

Matos RM, Cavaillé JY, Dufresne A, Gerard JF, Graillat C. Processing and characterization of new thermoset nanocomposites based on cellulose whiskers. Composite Interfaces. 2000;7(2):117-131. Available: https://doi.org/10.1163/156855400300184271

Neus Anglés M, Dufresne A. Platicized starch/ tunicin whiskers, nanocomposite materials.2. Mechanical Behaviours. Macromolecules. 2001;34(9):2921-2931. Available: https://doi.org/10.1021/MA001555H

simple.m.wikipedia.org > wiki > File: Cellulose triacetate structure.jpg. Retrieved on Sunday 14 January 2024, 11:59 am WAT.

Akpuaka MU. Essentials of natural products chemistry. 1st Edition. Mason Publishers Enugu, Nigeria. 2009;25-30.

www.vedantu.com>chemisy>us... Retrieved on the 1st of August 2023 at 03:20am West Central African Time.

Badea GI, Radu GL. Introductory chapter: Carboxylic acids-keyrole in life sciences; 2018. Available: https://dx.doi.org/10.5772/intechopen.77021

Kalgutkar AS, Daniels JS. Carboxylic acids and their bioisosteres. In: Metabolism, pharmacokinetics and toxicity of functional groups: Impact of the building blocks of medicinal chemistry on ADMET. London: Royal Society of Chemistry. 2010;99-167.

Pfaff AR, Beltz J, King E, Ercal N. Medicinal thiols: Current status and new perspectives Mini Rev. Med. Chem. 2020;20(6):513-529. DOI:10.2174/1389557519666191119144100

Smith A. Nova Biomedical: The importance of ketones from a clinical and medical perspective. News-Medical; 2023. Available:https://www.newsmedical.net/news/20230308/The-importance-of-ketones-from-a-clinical-and-medical-perspective.aspx>.

Carter A, Jewel T. What are the medical and health uses of phenol? An overview. Healthcare; 2019.

Al Mamari HH. Phenolic compounds: Classification, chemistry and updated techniques of analysis and synthesis. Chapter metrics overview. Open access peer-reviewed chapter. Healthline media; 2021. DOI:10.5772/intechopen-98958.

Haminiuk CW, Maciel GM, Plata-Oviedo MSV, Peralta RM. Phenolic compounds in fruits- an overview. Food Sci. Technol. Int. 2012;47:2022-2044. Available: https://doi.org/10.1111/j.13652621.2012.03067.x

Das S, Das J, Samadder A, Khuda- Bukhsh AR. Dihydroxy –isosteviol methyl ester from pulsatilla nigricans induces apostosis in Hela cells: Its cytoxicity and interaction with calf thymus DNA. Phototherapy Research. 2012;27(5):664-673. Available: https://doi.org/10.1002/ptr.4768

Wang Y, Qian H. Pthalates and their impacts on human health. Healthcare. 2021;9(5):603. DOI:1.3390/healthcare9050603

Ericson-Neilsen W, Kaye AD. Steroids: Pharmacology, complications and practice delivery issues. The Ochsner Journal. 2014;14(2):203-207.

Sharma S, Anand N. Approaches to design and synthesis of antiparasitic drugs. Pharmacochemistry Library. 1997;25:296-324. Available: https://doi.org/10.1016/S0165-7208(97)80034-7

Negi BYS. Studies on cellulose nanocrystals isolated from groundnut shells. Carbohydrate Polymers. 2017;157:1041-1049.

Carreón T, Herrick RL. Aliphatic hydrocarbons. Wiley Online Library; 2012. Available:https://doi.org/10.1002/0471435139.tox049.pub2

www.google.com. Retrieved on the1st of August 2023 at 2:30am West Central African Time

Dumonteil G, Berteina-Rabolo S. Synthesis of conjugated dienes in natural compounds. Journals Catalysts. 2022;12 (1):86. DOI.org/10.3390/catal12010086

Rani A, Jain S, Kumar R, Kumar A. 1,5-Bis (2-hydroxyphenyl) pent-1,4-diene-3-one: A lead compound for the development of broad-spectrum anti-bacterial agents. S. Afr. J. Chem. 2010;63:31-35. Available: htpps://journals.sabinet.co.zalsajchem/>

Xiao Y, Liu Y, Wang X, Li M, Lei H, Xu H. Cellulose nanocrystals prepared from wheat bran: Characterization and cytoxicity assessment. International Journal of Biological Macromolecules. 2019;140:225-233.

Kassab Z, Abdellaoui Y, Salim MH, El Achaby M. Cellulosic Materials from Pealpisum sativum and broad beans (vicia faba) pods agro-industrial residues. Material Letters. 2022;280:128539. Available:https://doi.org/10.1016(j.matlet.2020.128539

Furniss BS, Hannaford AJ, Smith PWG, Tatchell AR. Vogel’s textbook of practical organic chemistry. 5th Edition. Pearson Education limited, England. 1196-1204, 1225, 1289-1398.

ASTM International. ASTM D792-17 Standard test methods for density, specific gravity (Relative Density of plastics by displacement), cellulose, lignin, hemicellulose, moisture content and melting point. West Conshohocken, PA: ASTM International; 2017.

American Oil Chemists' Society (AOAC). Official methods and recommended practices of the AOCS (7th ed.). AOCS Press; 2017.

ASTM International. ASTM E70-18 Standard Test for pH of aqueous solutions with the glass electrode. West Conshohocken, PA: ASTM International; 2015.

www.quora.com. Retrieved from Google scholar on Tuesday, 9 January, 2024 at 3:48am WAT.

Azogu CI, Laboratory Organic Chemistry: Techniques, qualitative analysis, organic preparations and spectroscopy. 2nd Edition. Maybinson Book Publishers, New Jersey, USA. 2010;153-200.

Ajayi IA, Oderinde RA, Kajogbola DO, Uponi JI. Oil content and fatty acid composition of some underutilized legumes from Nigeria. Journal of Food Chemistry. 2006;99:115-120. DOI:10.1016/j.foodchem.2005.06.045.

Ibourki M, Azouguigh F, Jadouali S, Saka E, Bijla L, Majourhat K, Gharby S, Laknifli A. Physical fruit traits, nutritional composition and seed oil fatty acid profiling in the main date palm (Phoenix dactylifera L.) varieties grown in Morocco. Hindawi Journal of Food Quality. Article ID5138043, 2021;12. Available:https://doi.org/10.1155/2021/5138043.

Alkinjokun A, Petrik LF, Ogunfowokan J, Ajao J, Ojumu TV. Isolation and characterization of nanocrystalline cellulose from cocoa pod husk (CPH) biomass wastes. Heliyon. 2021;7(4):e06680.

Alhaji MH, Oparah EN, Yakubu MK, Maju CC, Suleiman H, Akawu I, Musa TAD, Aliyu S. Production, properties and applications of cellulose/waste leather buff composite (WLB) for environmental sustainability and recyclability. Journal of Chemical Society of Nigeria. 2021;46(3):610-617. Available: htpps://doi.org/10.46602/jcsn.v46i3.634

Danbature WL, Shehu Z, Joshua J, Adam MM. Moringa oleifera root-mediated synthesis of nanosilver particles and the antibacterial applications. Journal of Chemical Society of Nigeria. 2021;46(3): 504-516. Available:https://doi.org/10.46602/jcsn.v446i3.626

Ekeoma MO, Okoye PAC, Ajiwe VIE, Hameed BH. Modified coconut shell as active heterogeneous catalyst for the transesterification of waste cooking oil. J. Chem. Soc. Nigeria. 2020;45(2): 360-368.

Pam AA, Adeyi AA, Obiyenwa GK, Yinusa I, Salawu OW. Adsorption of methylene blue from aqueous solution using iminodiacetic acid supported montmorillonite adsorbent. J. Chem. Soc. Nigeria. 2020;45(2):288-297.

Saravanan R, Ravikumar I. The use of new chemically modified cellulose for heavy metal ion adsorption and antimicrobial activities. Journal of Water Resources and Protection. 2015;7:530-545.

Williams DH, Fleming I. Spectroscopic methods in organic chemistry. 3rd Edition. McGraw-Hill Book Company (UK) Limited England, 1980;47-73.

Flauzino NWP, Silverio HA, Dantas NO, Pasquini D. Extraction and characterization of cellulose nanocrystals from agro-industrial residue-soy hulls, Ind. Crop Prod. 2013;42:480-488.

George J, SN S. Cellulose nanocrystals: Synthesis, functional properties and applications. Nanotechnology Sci. Appl; 2015. DOI: 10.2147/NSA.S64386