Extraction and characterization of cellulose microfibers from Retama raetam stems

Khenblouche, Abdelkader; Bechki, Djamel; Gouamid, Messaoud; Charradi, Khaled; Segni, Ladjel; Hadjadj, Mohamed; Boughali, Slimane

doi:10.1590/0104-1428.05218

Abdelkader Khenblouche ^* * khenblouche89@gmail.com

Laboratory of New and Renewable Energy in Arid Zones – LENREZA, University of Ouargla, Ouargla, Algeria

https://orcid.org/0000-0001-8034-8215

Djamel Bechki

Laboratory of New and Renewable Energy in Arid Zones – LENREZA, University of Ouargla, Ouargla, Algeria

Messaoud Gouamid

Department of Chemistry, Faculty of Mathematics & Material Sciences, University of Ouargla, Ouargla, Algeria

Khaled Charradi

Laboratory of Nanomaterials and Systems for Renewable Energies – LaNSER, Research and Technology Center of Energy, Techno-park Borj-Cedria, Hammam-Lif, Tunis, Tunisia

Ladjel Segni

Laboratory of Process Engineering, Faculty of Applied Sciences, University of Ouargla, Ouargla, Algeria

Mohamed Hadjadj

Laboratory of Valorization and Promotion of Saharian Resources – VPRS, University of Ouargla, Ouargla, Algeria

Slimane Boughali

Laboratory of New and Renewable Energy in Arid Zones – LENREZA, University of Ouargla, Ouargla, Algeria

* khenblouche89@gmail.com

Source	Crystallinity index (CrI)	Reference
Coconut palm leaf sheath	47.7%	Uma Maheswari et al.^[²²22 Uma Maheswari, C., Obi Reddy, K., Muzenda, E., Guduri, B. R., & Varada Rajulu, A. (2012). Extraction and characterization of cellulose microfibrils from agricultural residue – Cocos nucifera L. Biomass and Bioenergy, 46, 555-563. http://dx.doi.org/10.1016/j.biombioe.2012.06.039. http://dx.doi.org/10.1016/j.biombioe.20... ^]
Sugarcane bagasse	50%	Jonjankiat et al.^[²³23 Jonjankiat, S., Wittaya, T., & Sridach, W. (2011). Improvement of poly (vinyl alcohol) adhesives with cellulose microfibre from sugarcane bagasse. Iranian Polymer Journal , 20(4), 305-317. ^]
Agave fibers	64.4%	Reddy et al.^[²⁴24 Reddy, K. O., Zhang, J., Zhang, J., & Rajulu, A. V. (2014). Preparation and properties of self-reinforced cellulose composite films from Agave microfibrils using an ionic liquid. Carbohydrate Polymers, 114, 537-545. http://dx.doi.org/10.1016/j.carbpol.2014.08.054. PMid:25263924. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Mengkuang leaves	69.5%	Sheltami et al.^[³3 Sheltami, R. M., Abdullah, I., Ahmad, I., Dufresne, A., & Kargarzadeh, H. (2012). Extraction of cellulose nanocrystals from mengkuang leaves (Pandanus tectorius ). Carbohydrate Polymers, 88(2), 772-779. http://dx.doi.org/10.1016/j.carbpol.2012.01.062. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Soy hulls	69.6%	Alemdar and Sain^[²⁵25 Alemdar, A., & Sain, M. (2008). Isolation and characterization of nanofibers from agricultural residues–Wheat straw and soy hulls. Bioresource Technology , 99(6), 1664-1671. http://dx.doi.org/10.1016/j.biortech.2007.04.029. PMid:17566731. http://dx.doi.org/10.1016/j.biortech.20... ^]
Commercial microcrystalline cellulose	73.91%	Kale et al.^[²⁰20 Kale, R. D., Bansal, P. S., & Gorade, V. G. (2018). Extraction of microcrystalline cellulose from cotton sliver and its comparison with commercial microcrystalline cellulose. Journal of Polymers and the Environment, 26(1), 355-364. http://dx.doi.org/10.1007/s10924-017-0936-2. http://dx.doi.org/10.1007/s10924-017-09... ^]
Sisal fibers	75% ±1	Morán et al.^[²⁶26 Morán, J. I., Alvarez, V. A., Cyras, V. P., & Vázquez, A. (2008). Extraction of cellulose and preparation of nanocellulose from sisal fibers. Cellulose , 15(1), 149-159. http://dx.doi.org/10.1007/s10570-007-9145-9. http://dx.doi.org/10.1007/s10570-007-91... ^]
Wheat straw	77.8%	Alemdar and Sain^[²⁵25 Alemdar, A., & Sain, M. (2008). Isolation and characterization of nanofibers from agricultural residues–Wheat straw and soy hulls. Bioresource Technology , 99(6), 1664-1671. http://dx.doi.org/10.1016/j.biortech.2007.04.029. PMid:17566731. http://dx.doi.org/10.1016/j.biortech.20... ^]
Retama Reatam	77.8%	This work
Hibiscus sabdariffa	78.95%	Sonia and Priya Dasan^[²⁷27 Sonia, A., & Priya Dasan, K. (2013). Chemical, morphology and thermal evaluation of cellulose microfibers obtained from Hibiscus sabdariffa. Carbohydrate Polymers, 92(1), 668-674. http://dx.doi.org/10.1016/j.carbpol.2012.09.015. PMid:23218352. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Palmyra palm Fruits	81.9%	Reddy et al.^[²⁸28 Reddy, K. O., Maheswari, C. U., Dhlamini, M. S., & Kommula, V. P. (2016). Exploration on the characteristics of cellulose microfibers from Palmyra palm fruits. International Journal of Polymer Analysis and Characterization, 21(4), 286-295. http://dx.doi.org/10.1080/1023666X.2016.1147799. http://dx.doi.org/10.1080/1023666X.2016... ^]

Spectra	Wavenumber (cm^-1)	Assignment	Ref.
(a), (b), (c)	876-897	C–O–C stretching at the b-(1→4)-glycosidic linkages	Oh et al.^[³²32 Oh, S. Y., Yoo, D. I., Shin, Y., Kim, H. C., Kim, H. Y., Chung, Y. S., Park, W. H., & Youk, J. H. (2005). Crystalline structure analysis of cellulose treated with sodium hydroxide and carbon dioxide by means of X-ray diffraction and FTIR spectroscopy. Carbohydrate Research, 340(15), 2376-2391. http://dx.doi.org/10.1016/j.carres.2005.08.007. PMid:16153620. http://dx.doi.org/10.1016/j.carres.2005... ^]
(a), (b), (c)	1029-1031	C–O–C pyranose ring skeletal vibration	Sun et al.^[³³33 Sun, J. X., Sun, X. F., Zhao, H., & Sun, R. C. (2004). Isolation and characterization of cellulose from sugarcane bagasse. Polymer Degradation & Stability , 84(2), 331-339. http://dx.doi.org/10.1016/j.polymdegradstab.2004.02.008. http://dx.doi.org/10.1016/j.polymdegrad... ^]
(b), (c)	1051-1054	C–O–C pyranose ring skeletal vibration	Sun et al.^[³³33 Sun, J. X., Sun, X. F., Zhao, H., & Sun, R. C. (2004). Isolation and characterization of cellulose from sugarcane bagasse. Polymer Degradation & Stability , 84(2), 331-339. http://dx.doi.org/10.1016/j.polymdegradstab.2004.02.008. http://dx.doi.org/10.1016/j.polymdegrad... ^]
(a), (b), (c)	1144-1159	C–O–C stretching at the b-(1→4)-glycosidic linkages	Oh et al.^[³²32 Oh, S. Y., Yoo, D. I., Shin, Y., Kim, H. C., Kim, H. Y., Chung, Y. S., Park, W. H., & Youk, J. H. (2005). Crystalline structure analysis of cellulose treated with sodium hydroxide and carbon dioxide by means of X-ray diffraction and FTIR spectroscopy. Carbohydrate Research, 340(15), 2376-2391. http://dx.doi.org/10.1016/j.carres.2005.08.007. PMid:16153620. http://dx.doi.org/10.1016/j.carres.2005... ^]
(a), (b)	1224-1236	–COO vibration of acetyl groups / C–O stretching of the aryl group	Reddy et al.^[²⁸28 Reddy, K. O., Maheswari, C. U., Dhlamini, M. S., & Kommula, V. P. (2016). Exploration on the characteristics of cellulose microfibers from Palmyra palm fruits. International Journal of Polymer Analysis and Characterization, 21(4), 286-295. http://dx.doi.org/10.1080/1023666X.2016.1147799. http://dx.doi.org/10.1080/1023666X.2016... ^]
(a), (b), (c)	1316-1327	C–C and C–O skeletal vibrations	Gao et al.^[³⁴34 Gao, X., Chen, K.-L., Zhang, H., Peng, L.-C., & Liu, Q.-X. (2014). Isolation and characterization of cellulose obtained from bagasse pith by oxygen-containing agents. BioResources , 9(3), 4094-4107. http://dx.doi.org/10.15376/biores.9.3.4094-4107. http://dx.doi.org/10.15376/biores.9.3.4... ^]
(a), (b), (c)	1370-1374	O–H bending	Gao et al.^[³⁴34 Gao, X., Chen, K.-L., Zhang, H., Peng, L.-C., & Liu, Q.-X. (2014). Isolation and characterization of cellulose obtained from bagasse pith by oxygen-containing agents. BioResources , 9(3), 4094-4107. http://dx.doi.org/10.15376/biores.9.3.4094-4107. http://dx.doi.org/10.15376/biores.9.3.4... ^]
(a), (b), (c)	1417-1429	CH2 bending	Gao et al.^[³⁴34 Gao, X., Chen, K.-L., Zhang, H., Peng, L.-C., & Liu, Q.-X. (2014). Isolation and characterization of cellulose obtained from bagasse pith by oxygen-containing agents. BioResources , 9(3), 4094-4107. http://dx.doi.org/10.15376/biores.9.3.4094-4107. http://dx.doi.org/10.15376/biores.9.3.4... ^]
(a), (b), (c)	1644-1646	OH bending of the absorbed water	Alemdar and Sain^[²⁵25 Alemdar, A., & Sain, M. (2008). Isolation and characterization of nanofibers from agricultural residues–Wheat straw and soy hulls. Bioresource Technology , 99(6), 1664-1671. http://dx.doi.org/10.1016/j.biortech.2007.04.029. PMid:17566731. http://dx.doi.org/10.1016/j.biortech.20... ^]
(a)	1734	C=O stretching	Sain and Panthapulakkal^[³⁵35 Sain, M., & Panthapulakkal, S. (2006). Bioprocess preparation of wheat straw fibers and their characterization. Industrial Crops and Products, 23(1), 1-8. http://dx.doi.org/10.1016/j.indcrop.2005.01.006. http://dx.doi.org/10.1016/j.indcrop.200... ^]
(a), (b), (c)	2896-2922	C–H stretching	Kondo and Sawatari^[³⁶36 Kondo, T., & Sawatari, C. (1996). A Fourier transform infra-red spectroscopic analysis of the character of hydrogen bonds in amorphous cellulose. Polymer, 37(3), 393-399. http://dx.doi.org/10.1016/0032-3861(96)82908-9. http://dx.doi.org/10.1016/0032-3861(96)... ^]
(a), (b), (c)	3323-3332	H-bonded OH groups stretching	Kondo and Sawatari^[³⁶36 Kondo, T., & Sawatari, C. (1996). A Fourier transform infra-red spectroscopic analysis of the character of hydrogen bonds in amorphous cellulose. Polymer, 37(3), 393-399. http://dx.doi.org/10.1016/0032-3861(96)82908-9. http://dx.doi.org/10.1016/0032-3861(96)... ^]

Source	Extraction method	diameter (μm)	Ref.
Sisal fibers	Alkali, peroxide and HNO₃/HAc treatments	12.8-31	Morán et al.^[²⁶26 Morán, J. I., Alvarez, V. A., Cyras, V. P., & Vázquez, A. (2008). Extraction of cellulose and preparation of nanocellulose from sisal fibers. Cellulose , 15(1), 149-159. http://dx.doi.org/10.1007/s10570-007-9145-9. http://dx.doi.org/10.1007/s10570-007-91... ^]
Coconut palm leaf sheath	Chlorination, alkali and HNO₃/HAc treatments	10-15	Uma Maheswari et al.^[²²22 Uma Maheswari, C., Obi Reddy, K., Muzenda, E., Guduri, B. R., & Varada Rajulu, A. (2012). Extraction and characterization of cellulose microfibrils from agricultural residue – Cocos nucifera L. Biomass and Bioenergy, 46, 555-563. http://dx.doi.org/10.1016/j.biombioe.2012.06.039. http://dx.doi.org/10.1016/j.biombioe.20... ^]
Soy hull	Alkali treatment and HCl Acid hydrolysis	10-15	Alemdar and Sain^[²⁵25 Alemdar, A., & Sain, M. (2008). Isolation and characterization of nanofibers from agricultural residues–Wheat straw and soy hulls. Bioresource Technology , 99(6), 1664-1671. http://dx.doi.org/10.1016/j.biortech.2007.04.029. PMid:17566731. http://dx.doi.org/10.1016/j.biortech.20... ^]
Wheat straw	Alkali treatment and HCl Acid hydrolysis	10-15	Alemdar and Sain^[²⁵25 Alemdar, A., & Sain, M. (2008). Isolation and characterization of nanofibers from agricultural residues–Wheat straw and soy hulls. Bioresource Technology , 99(6), 1664-1671. http://dx.doi.org/10.1016/j.biortech.2007.04.029. PMid:17566731. http://dx.doi.org/10.1016/j.biortech.20... ^]
Agave fibers	Chlorination, alkali and HNO₃/HAc treatments	8-14	Reddy et al.^[²⁴24 Reddy, K. O., Zhang, J., Zhang, J., & Rajulu, A. V. (2014). Preparation and properties of self-reinforced cellulose composite films from Agave microfibrils using an ionic liquid. Carbohydrate Polymers, 114, 537-545. http://dx.doi.org/10.1016/j.carbpol.2014.08.054. PMid:25263924. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Hibiscus sabdariffa	Steam explosion and oxalic acid hydrolysis	10.04	Sonia and Priya Dasan^[²⁷27 Sonia, A., & Priya Dasan, K. (2013). Chemical, morphology and thermal evaluation of cellulose microfibers obtained from Hibiscus sabdariffa. Carbohydrate Polymers, 92(1), 668-674. http://dx.doi.org/10.1016/j.carbpol.2012.09.015. PMid:23218352. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Sisal fibers	Chlorination and alkali treatments	7-11.2	Morán et al.^[²⁶26 Morán, J. I., Alvarez, V. A., Cyras, V. P., & Vázquez, A. (2008). Extraction of cellulose and preparation of nanocellulose from sisal fibers. Cellulose , 15(1), 149-159. http://dx.doi.org/10.1007/s10570-007-9145-9. http://dx.doi.org/10.1007/s10570-007-91... ^]
Cotton	Sulfuric acid hydrolysis	5-10	Chatterjee et al.^[⁴⁴44 Chatterjee, A., Kiran Kumar, G., Dharma Sagar, B., Sravanti, K., Ramakrishna, K., & Rajesh, C. (2018). Pure and copper doped cellulose microfibers-a case study. Materials Research Express, 5(10), 105302. http://dx.doi.org/10.1088/2053-1591/aad9d4. http://dx.doi.org/10.1088/2053-1591/aad... ^]
Sugarcane bagasse	Nitric acid hydrolysis	5-10	Jonjankiat et al.^[²³23 Jonjankiat, S., Wittaya, T., & Sridach, W. (2011). Improvement of poly (vinyl alcohol) adhesives with cellulose microfibre from sugarcane bagasse. Iranian Polymer Journal , 20(4), 305-317. ^]
Palmyra palm fruit	Chlorination, alkali and HNO₃/HAc treatments	4-11	Reddy et al.^[²⁸28 Reddy, K. O., Maheswari, C. U., Dhlamini, M. S., & Kommula, V. P. (2016). Exploration on the characteristics of cellulose microfibers from Palmyra palm fruits. International Journal of Polymer Analysis and Characterization, 21(4), 286-295. http://dx.doi.org/10.1080/1023666X.2016.1147799. http://dx.doi.org/10.1080/1023666X.2016... ^]
Napier grass fibers	Chlorination, alkali and HNO₃/HAc treatments	8.3	Reddy et al.^[²⁹29 Reddy, K. O., Maheswari, C. U., Dhlamini, M. S., Mothudi, B. M., Kommula, V. P., Zhang, J., Zhang, J., & Rajulu, A. V. (2018). Extraction and characterization of cellulose single fibers from native african napier grass. Carbohydrate Polymers, 188, 85-91. http://dx.doi.org/10.1016/j.carbpol.2018.01.110. PMid:29525176. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Retama Raetam Stems	Alkali and alkaline peroxide treatments	6-7	This work
Jatropha Curcus L seed shell	Chlorination, alkali and HNO₃/HAc treatments	0.23-1.04	Puttaswamy et al.^[⁴⁵45 Puttaswamy, M., Srinikethan, G., & Shetty, K. V. (2017). Biocomposite composed of PVA reinforced with cellulose microfibers isolated from biofuel industrial dissipate: Jatropha Curcus L. seed shell. Journal of Environmental Chemical Engineering , 5(2), 1990-1997. http://dx.doi.org/10.1016/j.jece.2017.04.004. http://dx.doi.org/10.1016/j.jece.2017.0... ^]

Samples	T_max (◦C)	Char (%)	Reference
Date seeds cellulose microfibers	300	11	Nabili et al.^[⁴⁸48 Nabili, A., Fattoum, A., Brochier-Salon, M.-C., Bras, J., & Elaloui, E. (2017). Synthesis of cellulose triacetate-I from microfibrillated date seeds cellulose (Phoenix dactylifera L.). Iranian Polymer Journal , 26(2), 137-147. http://dx.doi.org/10.1007/s13726-017-0505-5. http://dx.doi.org/10.1007/s13726-017-05... ^]
Bamboo cellulose microfibers	328	13	Chen et al.^[⁴⁹49 Chen, W., Yu, H., Liu, Y., Hai, Y., Zhang, M., & Chen, P. (2011). Isolation and characterization of cellulose nanofibers from four plant cellulose fibers using a chemical-ultrasonic process. Cellulose, 18(2), 433-442. http://dx.doi.org/10.1007/s10570-011-9497-z. http://dx.doi.org/10.1007/s10570-011-94... ^]
Rice hulls microcrystalline cellulose	283	23	Adel et al.^[⁵⁰50 Adel, A. M., Abd El-Wahab, Z. H., Ibrahim, A. A., & Al-Shemy, M. T. (2011). Characterization of microcrystalline cellulose prepared from lignocellulosic materials. Part II: physicochemical properties. Carbohydrate Polymers, 83(2), 676-687. http://dx.doi.org/10.1016/j.carbpol.2010.08.039. http://dx.doi.org/10.1016/j.carbpol.201... ^]
bean hulls microcrystalline cellulose	281	25	Adel et al.^[⁵⁰50 Adel, A. M., Abd El-Wahab, Z. H., Ibrahim, A. A., & Al-Shemy, M. T. (2011). Characterization of microcrystalline cellulose prepared from lignocellulosic materials. Part II: physicochemical properties. Carbohydrate Polymers, 83(2), 676-687. http://dx.doi.org/10.1016/j.carbpol.2010.08.039. http://dx.doi.org/10.1016/j.carbpol.201... ^]
Onion skin cellulose microfibers	333	26	Reddy and Rhim^[⁵¹51 Reddy, J. P., & Rhim, J.-W. (2018). Extraction and characterization of cellulose microfibers from agricultural wastes of onion and garlic. Journal of Natural Fibers , 15(4), 465-473. http://dx.doi.org/10.1080/15440478.2014.945227. http://dx.doi.org/10.1080/15440478.2014... ^]
Retama Raetam cellulose microfibers	311	42	This work
Cotton silver microcrystalline cellulose	340	57	Das et al.^[⁵²52 Das, K., Ray, D., Bandyopadhyay, N. R., & Sengupta, S. (2010). Study of the properties of microcrystalline cellulose particles from different renewable resources by XRD, FTIR, nanoindentation, TGA and SEM. Journal of Polymers and the Environment , 18(3), 355-363. http://dx.doi.org/10.1007/s10924-010-0167-2. http://dx.doi.org/10.1007/s10924-010-01... ^]
Jute microcrystalline cellulose	280	61	Das et al.^[⁵²52 Das, K., Ray, D., Bandyopadhyay, N. R., & Sengupta, S. (2010). Study of the properties of microcrystalline cellulose particles from different renewable resources by XRD, FTIR, nanoindentation, TGA and SEM. Journal of Polymers and the Environment , 18(3), 355-363. http://dx.doi.org/10.1007/s10924-010-0167-2. http://dx.doi.org/10.1007/s10924-010-01... ^]

[1] * khenblouche89@gmail.com

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Extraction and characterization of cellulose microfibers from Retama raetam stems

Abstract