Abstract
Microcrystalline cellulose was obtained from agave bagasse by sequential alkaline hydrogen peroxide hydrolysis at low reagent concentrations, followed by dilute acid hydrolysis. The impact of reaction time, hydrogen peroxide concentration, and sulfuric acid hydrolysis on the physicochemical properties of the extracted crystalline cellulose was examined. Alkaline treatments efficiently produced porous crystalline cellulose and reduced its lignin and hemicellulose content. However, they were inadequate to remove the characteristic calcium oxalate crystals (COC) in agave bagasse cell walls. No significant differences in crystallinity degrees of the alkaline treated samples were detected in 62.8–5.2%, which increased to 69.4% after acid hydrolysis. X-ray diffractograms revealed the presence of type I cellulose as the primary domain, and FTIR confirmed the presence of COC and the removal of the non-cellulosic components during chemical treatments. In addition, morphological studies revealed the disruption of the lignocellulosic matrix and porous formation. The proposed method promises to produce porous crystalline cellulose in a short-term process, avoiding the complex and high-cost steps such as dewaxing and concentrated acid hydrolysis. Moreover, agave bagasse is a potential waste material for cellulose derivatives with interesting applications.
Graphical abstract
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Abu-Thabit NY, Judeh AB, Hakeem AS, Ul-Hamid A, Umar Y, Ahmad A (2020) Isolation and characterization of microcrystalline cellulose from date seeds (Phoenix dactylifera L.). Int J Biol Macromol 155:730–739. https://doi.org/10.1016/j.ijbiomac.2020.03.255
Aguirre-Fierro A, Ruiz HA, Cerqueira MA, Ramos-González R, Rodríguez-Jasso RM, Marques S, Lukasik RM (2020) Sustainable approach of high-pressure agave bagasse pretreatment for ethanol production. Renew Energy 155:1347–1354. https://doi.org/10.1016/j.renene.2020.04.055
Ahankari SS, Subhedar AR, Bhadauria SS, Dufresne A (2021) Nanocellulose in food packaging: a review. Carbohydr Polym 255:117479. https://doi.org/10.1016/j.carbpol.2020.117479
Akinjokun AI, Petrik LF, Ogunfowokan AO, Ajao J, Ojumu TV (2021) Isolation and characterization of nanocrystalline cellulose from cocoa pod husk (CPH) biomass wastes. Heliyon 7:e06680. https://doi.org/10.1016/j.heliyon.2021.e06680
Bai H, Chen J, Zhou X, Hu C (2020) Single and binary adsorption of dyes from aqueous solutions using functionalized microcrystalline cellulose from cotton fiber. Korean J Chem Eng 37:1926–1932. https://doi.org/10.1007/s11814-020-0621-3
Baruah J, Deka RC, Kalita E (2020) Greener production of microcrystalline cellulose (MCC) from Saccharum spontaneum (Kans grass): statistical optimization. Int J Biol Macromol 154:672–682. https://doi.org/10.1016/j.ijbiomac.2020.03.158
Benarbia A, Elidrissi A, Aqil M, Tabaght F, Tahani A, Ouassini K (2015) Kinetic thermal degradation of cellulose, polybutylene succinate and a green composite: comparative study. World J Environ Eng 3:95–110. https://doi.org/10.12691/wjee-3-4-1
Bernardino-Nicanor A, Teniente-Martínez G, Juarez-Goiz J, Filardo-Kerstupp S, Montañez-Soto J, González-Cruz L (2012) Changes in the concentration and characteristics of calcium oxalate crystals during development stages of Agave atrovirens. Adv Biores 3:22–28. https://doi.org/10.1093/humrep/det417
Borges de Oliveira F, Bras J, Borges Pimenta MT, da Silva Curvelo AA, Belgacem MN (2016) Production of cellulose nanocrystals from sugarcane bagasse fibers and pith. Ind Crops Prod 93:48–57. https://doi.org/10.1016/j.indcrop.2016.04.064
Cao J, Fei D, Tian X, Zhu Y, Wang S, Zhang Y, Mao Q, Sun M (2017) Novel modified microcrystalline cellulose-based porous material for fast and effective heavy metal removal from aqueous solution. Cellulose 24:5565–5577. https://doi.org/10.1007/s10570-017-1504-6
Carrillo-Varela I, Pereira M, Mendonca RT (2018) Determination of polymorphic changes in cellulose from Eucalyptus spp. Fibres after Alkalization Cellul 25:6831–6845. https://doi.org/10.1007/s10570-018-2060-4
Caspeta L, Caro-Bermúdez MA, Ponce-Noyola T, Martínez A (2014) Enzymatic hydrolysis at high-solids loadings for the conversion of agave bagasse to fuel ethanol. Appl Energy 113:277–286. https://doi.org/10.1016/j.apenergy.2013.07.036
Chen J, Wang X, Long Z, Wang S, Zhang J, Wang L (2020) Preparation and performance of thermoplastic starch and microcrystalline cellulose for packaging composites: extrusion and hot pressing. Int J Biol Macromol 165:2295–2302. https://doi.org/10.1016/j.ijbiomac.2020.10.117
Collazo-Bigliardi S, Ortega-Toro R, Boix AC (2018) Isolation and characterisation of microcrystalline cellulose and cellulose nanocrystals from coffee husk and comparative study with rice husk. Carbohydr Polym 191:205–215. https://doi.org/10.1016/j.carbpol.2018.03.022
Consejo Regulador Mezcal (2020) Informe estadístico 2020; Consejo Regulador Mezcal; Oaxaca, México
Couret L, Irle M, Belloncle C, Cathala B (2017) Extraction and characterization of cellulose nanocrystals from post-consumer wood fibreboard waste. Cellulose 24:2125–2137. https://doi.org/10.1007/s10570-017-1252-7
Debnath B, Haldar D, Purkait MK (2021) A critical review on the techniques used for the synthesis and applications of crystalline cellulose derived from agricultural wastes and forest residues. Carbohydr Polym 273:118537. https://doi.org/10.1016/j.carbpol.2021.118537
Espino E, Cakir M, Domenek S, Román-Gutiérrez AD, Belgacem N, Bras J (2014) Isolation and characterization of cellulose nanocrystals from industrial by-products of Agave tequilana and barley. Ind Crops Prod 62:552–559. https://doi.org/10.1016/j.indcrop.2014.09.017
French AD (2014) Idealized powder diffraction patterns for cellulose polymorphs. Cellulose 21:885–896. https://doi.org/10.1007/s10570-013-0030-4
Garba ZN, Lawan I, Zhou W, Zhang M, Wang L, Yuan Z (2020) Microcrystalline cellulose (MCC) based materials as emerging adsorbents for the removal of dyes and heavy metals – a review. Sci Total Environ 717:135070. https://doi.org/10.1016/j.scitotenv.2019.135070
Girisuta B, Janssen LBPM, Heeres HJ (2007) Kinetic study on the acid-catalyzed hydrolysis of cellulose to levulinic acid. Ind Eng Chem Res 46:1696–1708. https://doi.org/10.1021/ie061186z
Gómez-Guerrero AV, Valdez-Vazquez I, Caballero-Caballero M, Chiñas-Castillo F, Alavéz-Ramírez R, Montes-Bernabé JL (2019) Co-digestion of Agave angustifolia haw bagasse and vinasses for biogas production from mezcal industry. Rev Mex Ing Quim 18:1073–1083. https://doi.org/10.24275/uam/izt/dcbi/revmexingquim/2019v18n3/Gomez
Gómora-Hernández JC, Carreño-de-León MC, Flores-Alamo N, Hernández-Berriel MC, Fernández-Valverde SM (2020) Kinetic and thermodynamic study of corncob hydrolysis in phosphoric acid with a low yield of bacterial inhibitors. Biomass Bioenergy 143:105830. https://doi.org/10.1016/j.biombioe.2020.105830
Hafid HS, Omar FN, Zhu J, Wakisaka M (2021) Enhanced crystallinity and thermal properties of cellulose from rice husk using acid hydrolysis treatment. Carbohydr Polym 260:117789. https://doi.org/10.1016/j.carbpol.2021.117789
Hourlier D (2019) Thermal decomposition of calcium oxalate: beyond appearances. J Therm Anal Calorim 136:2221–2229. https://doi.org/10.1007/s10973-018-7888-1
Izatulina AR, Gurzhiy VV, Krzhizhanovskaya M, Kuz’mina MA, Leoni M, Frank-Kamenetskaya OV (2018) Hydrated calcium oxalates: crystal structures, thermal stability and phase evolution. Cryst Growth Des 18:5465–5478. https://doi.org/10.1021/acs.cgd.8b00826
Kale RD, Bansal PS, Gorade VG (2018) Extraction of microcrystalline cellulose from cotton Sliver and its comparison with commercial microcrystalline cellulose. J Polym Environ 26:355–364. https://doi.org/10.1007/s10924-017-0936-2
Kian LK, Jawaid M, Ariffin H, Alothman OY (2017) Isolation and characterization of microcrystalline cellulose from roselle fibers. Int J Biol Macromol 103:931–940. https://doi.org/10.1016/j.ijbiomac.2017.05.135
Kian LK, Saba N, Jawaid M, Fouad H (2020) Characterization of microcrystalline cellulose extracted from olive fiber. Int J Biol Macromol 156:347–353. https://doi.org/10.1016/j.ijbiomac.2020.04.015
Li J, Lu M, Guo X, Zhang H, Li Y, Han L (2018) Insights into the improvement of alkaline hydrogen peroxide (AHP) pretreatment on the enzymatic hydrolysis of corn stover: chemical and microstructural analyses. Bioresour Technol 265:1–7. https://doi.org/10.1016/j.biortech.2018.05.082
Liu Y, Liu A, Ibrahim SA, Yang H, Huang W (2018) Isolation and characterization of microcrystalline cellulose from pomelo peel. Int J Biol Macromol 111:717–721. https://doi.org/10.1016/j.ijbiomac.2018.01.098
Merci A, Urbano A, Grossmann MVE, Tischer CA, Mali S (2015) Properties of microcrystalline cellulose extracted from soybean hulls by reactive extrusion. Food Res Int 73:38–43. https://doi.org/10.1016/j.foodres.2015.03.020
Mongkhonsiri G, Anantpinijwatna A, Charoensuppanimit P, Arpornwichanop A, Gani R, Assabumrungrat S (2021) Novel biorefinery-integrated-Kraft-pulping network for sustainable development. Chem Eng Process Process Intensif 163:108373. https://doi.org/10.1016/j.cep.2021.108373
Monje PV, Baran EJ (2009) Characterization of calcium oxalate biominerals in Pereskia species (Cactaceae). Z Naturforsh 64c:763–766. https://doi.org/10.1515/znc-2009-11-1201
Owolabi AF, Mohamad-Haafiz MK, Sohrab-Hossain Md, Hazwan-Hussin M, Nurul-Fazita MR (2017) Influence of alkaline hydrogen peroxide pre-hydrolysis on the isolation of microcrystalline cellulose from oil palm fronds. Int J Biol Macromol 95:1228–1234. https://doi.org/10.1016/j.ijbiomac.2016.11.016
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. https://doi.org/10.1186/1754-6834-3-10
Pasaye-Anaya L, Vargas-Tah A, Martínez-Cámara C, Castro-Montoya AJ, Campos-García J (2019) Production of 2,3-butanediol by fermentation of enzymatic hydrolysed bagasse from agave mezcal-waste using the native Klebsiella oxytoca UM2-17 strain. J Chem Technol Biotechnol 94:3915–3923. https://doi.org/10.1002/jctb.6190
Pérez-Pimienta JA, Poggi-Varaldo HM, Ponce-Noyola T, Ramos-Valdivia AC, Chavez-Carvayar JA, Stavila V, Simmons BA (2016) Fractional pretreatment of raw and calcium oxalate-extracted agave bagasse using ionic liquid and alkaline hydrogen peroxide. Biomass Bioenergy 91:48–55. https://doi.org/10.1016/j.biombioe.2016.05.001
Prasanna NS, Mitra J (2020) Isolation and characterization of cellulose nanocrystals from Cucumis sativus peels. Carbohydr Polym 247:116706. https://doi.org/10.1016/j.carbpol.2020.116706
Rambo MKD, Ferreira MMC (2015) Determination of cellulose crystallinity of banana residues using near infrared spectroscopy and multivariate analysis. J Braz Chem Soc 26:1491–1499
Robles E, Fernández-Rodríguez J, Barbosa AM, Gordobil O, Carreño NLV, Labidi J (2018) Production of cellulose nanoparticles from blue agave waste treated with environmentally friendly processes. Carbohydr Polym 183:294–302. https://doi.org/10.1016/j.carbpol.2018.01.015
Robles-García MA, Del-Toro-Sánchez CL, Márquez-Ríos E, Barrera-Rodríguez A, Aguilar J, Aguilar JA, Reynoso-Marín FJ, Ceja I, Dórame-Miranda R, Rodríguez-Félix F (2018) Nanofibers of cellulose bagasse from Agave tequilana Weber var. azul by electrospinning: Preparation and characterization. Carbohydr Polym 192:69–74. https://doi.org/10.1016/j.carbpol.2018.03.058
Ruiz-Luna J, Velasco-Velasco VA, Maldonado-Peralta R, Enríquez-del Valle JR, Campos-Ángeles GV, Rodríguez-Ortiz G, Preciado-Rangel P (2012) Expression of nutrient deficiencies of nitrogen, phosphorus, potassium, sulfur and iron in agave angustifolia haw. Acta Hortic 947:339–345. https://doi.org/10.17660/ActaHortic.2012.947.43
Senthamaraikannan P, Kathiresan M (2018) Characterization of raw and alkali-treated new natural cellulosic fiber from Coccinia grandis L.. Carbohydr Polym 186:332–343. https://doi.org/10.1016/j.carbpol.2018.01.072
Septevani AA, Rifathin A, Sari AA, Sampora Y, Ariani GN, Sudiyarmanto SD (2020) Oil palm empty fruit bunch-based nanocellulose as a super-adsorbent for water remediation. Carbohydr Polym 229:115433. https://doi.org/10.1016/j.carbpol.2019.115433
Shao X, Wang J, Liu Z, Hu N, Liu M, Xu Y (2020) Preparation and characterization of porous microcrystalline cellulose from corncob. Ind Crops Prod 151:112457. https://doi.org/10.1016/j.indcrop.2020.112457
Sheng S, Meiling Z, Chen L, Wensheng H, Zhifeng Y (2018) Extraction and characterization of microcrystalline cellulose from waste cotton fabrics via hydrothermal method. Waste Manag 82:139–146. https://doi.org/10.1016/j.wasman.2018.10.023
Siripong P, Duangporn P, Takata E, Tsutsumi Y (2016) Phosphoric acid pretreatment of Achyranthes aspera and Sida acuta weed biomass to improve enzymatic hydrolysis. Bioresour Technol 203:303–308. https://doi.org/10.1016/j.biortech.2015.12.037
Solarte-Toro JC, Romero-García JM, Martínez-Patiño JC, Ruiz-Ramos E, Castro-Galiano E, Cardona-Alzate CA (2019) Acid pretreatment of lignocellulosic biomass for energy vectors production: a review focused on operational conditions and techno-economic assessment for bioethanol production. Renew Sustain Energ Rev 107:587–601. https://doi.org/10.1016/j.rser.2019.02.024
Tarchoun AF, Trache D, Klapötke TM (2019a) Microcrystalline cellulose from Posidonia oceanica brown algae: extraction and characterization. Int J Biol Macromol 138:837–845. https://doi.org/10.1016/j.ijbiomac.2019.07.176
Tarchoun AF, Trache D, Klapötke TM, Derradji M, Bessa W (2019b) Ecofriendly isolation and characterization of microcrystalline cellulose from giant reed using various acidic media. Cellulose 26:7635–7651. https://doi.org/10.1007/s10570-019-02672-x
Tedjani CF, Mya OB, Rebiai A (2020) Isolation and characterization of cellulose from date palm tree spathe sheath. Sustain Chem Pharm 17:100307. https://doi.org/10.1016/j.scp.2020.100307
Trache D, Hussin MH, Chuin CTH, Sabar S, Fazita MRN, Taiwo OFA, Hassan TM, Mohamad-Haafiz MK (2016) Microcrystalline cellulose: Isolation, characterization and bio-composites application – a review. Int J Biol Macromol 93:789–804. https://doi.org/10.1016/j.ijbiomac.2016.09.056
Trigui K, Loubens C, Magnin A, Putaux JL, Boufi S (2020) Cellulose nanofibrils prepared by twin-screw extrusion: effect of the fiber pretreatment on the fibrillation efficiency. Carbohydr Polym 240:116342. https://doi.org/10.1016/j.carbpol.2020.116342
Ventura-Cruz S, Tecante A (2019) Extraction and characterization of cellulose nanofibers from Rose stems (Rosa spp.). Carbohydr Polym 220:53–59. https://doi.org/10.1016/j.carbpol.2019.05.053
Ventura-Cruz S, Flores-Alamo N, Tecante A (2020) Preparation of microcrystalline cellulose from residual Rose stems (Rosa spp.) by successive delignification with alkaline hydrogen peroxide. Int J Biol Macromol 155:324–329. https://doi.org/10.1016/j.ijbiomac.2020.03.222
Wang ZC, Qin CQ, Zhang X, Wang Q, Li RX, Ren DF (2021) Effect of whey protein isolate/chitosan/microcrystalline cellulose/PET multilayer bottles on the shelf life of rosebud beverages. Food Chem 347:129006. https://doi.org/10.1016/j.foodchem.2021.129006
Xu F, Yu J, Tesso T, Dowell F, Wang D (2013) Qualitative and quantitative analysis of lignocellulosic biomass using infrared techniques: a mini-review. Appl Energy 104:801–809. https://doi.org/10.1016/j.apenergy.2012.12.019
Xu JK, Sun YC, Sun RC (2015) Synergistic effects of ionic liquid plus alkaline pretreatments on eucalyptus: lignin structure and cellulose hydrolysis. Process Biochem 50:955–965. https://doi.org/10.1016/j.procbio.2015.03.014
Yang L, Ru Y, Xu S, Liu T, Tan L (2021) Features correlated to improved enzymatic digestibility of corn stover subjected to alkaline hydrogen peroxide pretreatment. Bioresour Technol 325:124688. https://doi.org/10.1016/j.biortech.2021.124688
Yao W, Weng Y, Catchmark JM (2020) Improved cellulose X-ray diffraction analysis using Fourier series modeling. Cellulose 27:5563–5579. https://doi.org/10.1007/s10570-020-03177-8
Zhao T, Chen Z, Lin X, Ren Z, Li B, Zhang B (2018) Preparation and characterization of microcrystalline cellulose (MCC) from tea waste. Carbohydr Polym 184:164–170. https://doi.org/10.1016/j.carbpol.2017.12.024
Zhou Z, Liu D, Zhao Z (2021) Conversion of lignocellulose to biofuels and chemicals via sugar platform: an updated review on chemistry and mechanisms of acid hydrolysis of lignocellulose. Renew Sustain Energy Rev 146:111169. https://doi.org/10.1016/j.rser.2021.111169
Acknowledgments
J.C.G.H. wants to thank COMECYT for the financial support via the Cátedras COMECYT program (Grant No. CAT2021-0166). Authors also thank the Instituto Tecnológico de Toluca and Programa de Apoyo a la Investigación y el Posgrado de la Facultad de Química-UNAM (PAIP) (Grant 5000-9098) for technical help and additional financial support.
Funding
The authors have not disclosed any funding.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors have not disclosed any competing interests.
Additional information
Publisher's Note
Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.
Rights and permissions
Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.
About this article
Cite this article
Gómora-Hernández, J.C., Tecante, A., del Carmen Carreño-de-León, M. et al. Preparation of porous microcrystalline cellulose from mezcal industry agave bagasse by low reagent loading sequential chemical treatment. Cellulose 30, 2067–2084 (2023). https://doi.org/10.1007/s10570-022-05022-6
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s10570-022-05022-6