Effect of Organic Solvents on the Synthesis and Characterization of Carboxymethyl Cellulose from Sawdust

  • Joy Olayemi Biochemistry Department, Lagos State University, Ojo, Lagos, Nigeria
  • Samson Olayemi Analytical Research Division, Department of Production, Analytical Services, and Laboratory Management, Federal Institute of Industrial Research Oshodi, Lagos, Nigeria.
  • Olufemi Adeyemi Department of Chemical Sciences, Olabisi Onabanjo University, Ago-Iwoye, Ogun State, Nigeria.
  • Olayide Lawal Department of Industrial Chemistry, Federal University, Oye-Ekiti, Nigeria
  • Femi Adams Analytical Research Division, Department of Production, Analytical Services, and Laboratory Management, Federal Institute of Industrial Research Oshodi, Lagos, Nigeria.
  • Azeez Tijani Analytical Research Division, Department of Production, Analytical Services, and Laboratory Management, Federal Institute of Industrial Research Oshodi, Lagos, Nigeria.
Keywords: Sawdust, Cellulose, Carboxymethyl cellulose, Synthesis, Characterization


Sawdust generated as waste by-product from timber industries finds limited industrial applications and is mostly discarded or incinerated, causing environmental problems. This research work was carried out with a view of utilizing sawdust to synthesize Carboxymethyl cellulose (CMC). Cellulose was isolated from sawdust of commercially used hardwood (Mahogany- Khaya ivorensis) and softwood (Silk cotton- Eriodendron orientale) by alkali-acid and bleaching treatments. Using ethanol, butanol, isobutanol and isopropanol as solvent media, the isolated cellulose samples were converted to CMC through mercerization with sodium hydroxide (NaOH) and etherification with sodium monochloroacetic acid (SMCA). The products obtained were characterized using Degree of Substitution (DS), Fourier Transform Infrared (FTIR) Spectroscopy and Thermogravimetric Analysis (TGA). Studies revealed that optimum DS of 0.54 could be reached when isopropanol is used as solvent medium. The presence of carboxyl and methyl functional group at wavenumber 1580-1590 and 1380-1415 cm-1 respectively on the FTIR spectra confirmed the conversion of cellulose to CMC. TGA showed that the thermal stability of CMC is lower than that of the parent cellulose. The results obtained demonstrate a simple method for the conversion of sawdust to a high quality water-soluble cellulose derivative which has applications in the food, textile, cosmetics and pharmaceutical industries.


. P. Rachtanapun, (2009). Blended films of carboxymethyl cellulose (CMC) from papaya peel and corn starch. Kasetsart Journal (Natural Sciences), 43 (5), 259-266.

. K. Hattori, E. Abe, T. Yoshida, and J.A. Cuculo, (2004). New solvents for cellulose II ethylenediamine/thiocyanate salt system. Polymer Journal, 36 (2), 123-130.

. R.K. Singh, and A.K. Singh, (2012). Optimization of reaction conditions for preparing carboxymethyl cellulose from corn cobic agricultural waste. Waste Biomass Valor.

. X.H Yang, and W.L. Zhu, (2007). Viscosity properties of sodium carboxymethylcellulose solutions. Cellulose, 14, 409-417.

. T. Salmi, D. Valtakari, E. Paatero, B. Holmbom, and R. Sjoholm (1994). Kinetic study of the carboxymethylation of cellulose, journal of Industrial and Engineering Chemistry, 33, 1454-1459

. A. Alemdar, and M. Sain (2008). Isolation and characterization of nanofibers from agricultural residues- Wheat straw and soy hulls. Bioresources Technology, 9, 1664-1671

. O.S. Lawal, M.D. Lechner, W.M. Kulicke (2008). Single and multi-step carboxymethylation of water yam (Dioscorea alata) starch: Synthesis and characterization. International Journal of Biological Macromolecule,42 429-435.

. D. Pearson (1981). Chemical analysis of food. 7th Edition, J.A. Churchill, London Pp 100-105.

. I.M. Adekunle, T.A. Arowolo, I.T. Omoniyi, and O.T. Olubambi (2007). Risk assessment of aquatic lives exposed to cassava (Manihot esculanta crante) effluent using Nile tilapia (Oreochromic niloticus) and African mud catfish (Clarius gariepinus). Chemistry and Ecology, 23(5), 383 -392.

. B.K. Barai, R.S. Singhal, and P.R. Kulkarni, (1997). Optimization of a process for preparing carboxymethyl cellulose from water hyacinth (Eichornia crassipes). Carbohydrate Polymers, 32, 229–231.

. M.A. Belewu, (2006). A functional approach to dairy science and technology. African Journal of Biotechnology, 5(19), 1763 -1764.

. M.A. Bertuzzi, V.E.F. Castro, M. Armada, and J.C. Gottifredi, (2007). Water vapour permeability of edible starch based films. Journal of Food Engineering, 80,972-978.

. A. Bono, P.H, Ying, F.Y. Yan, C.L. Muei, R. Sarbatly, and D. Krishnaiah, (2009). Synthesis and characterization of carboxymethyl cellulose from palm kernel cake. Advances in Natural and Applied Sciences, 3 (1), 5-11.

. W. Burchard (2003). Solubility and Solution Structure of Cellulose Derivatives. Cellulose, 10, 213-225.

. W.R. Collings, R.D. Freeman, and R.C. Anthonisen, (1942). Method of making cellulose glycolic acid. US Patent 385698.

. Danilo Martins dos Santos, Andrea de Lacerda Bukzem, Diego Ascheri, Roberta Signini and Giberto Benedito de Aquino (2015). Microwave assisted carboxymethylation of cellulose extracted from brewers’ spent grain. Carbohydrate polymers, 131, 125-133

. D.F. Durso, (1981). Process for the preparation of cellulose ether derivatives. US Patent 4254258.

. K. Edelman, and T. Lindroos, (1990). Process for preparing sodium carboxy-methyl cellulose. US Patent 4941943.

. D. Fengel, and G. Wegner, (1989). Wood-Chemistry, ultrastructure, reactions. Walter de Gruyter, Berlin and New York, Pp 613.

. H.P. Fink, E. Walanta, and G. Mann (1995). In : J.F. Kenedy, G.O. Phillip, P.A. Williams and L. Piccilell eds, Cellulose and cellulose derivatives: physico-chemical aspects an industrial applications. Cambridge: Woodhead Publisher, pp.523-528

. P.S. Francis, (1961). Solution properties of water-soluble polymers. I. Control of aggregation of sodium carboxymethylcellulose (CMC) by choice of solvent and/or electrolyte. Journal of Applied Polymer Science, 5 (15), 261-270.

. T. Heinze, and T. Liebert T. (2001). Unconventional methods in cellulose fictionalization, Program of Polymeric Science. 26, 1689-1762.

. T. Heinze, and A. Koschella, (2005). Carboxymethyl ethers of cellulose and starch. Macromolecular Symposium, 223, 13–39.

. T. Heinze, T. Liebert, P. Klufers, and F. Meister, (1999). Carboxymethylation of cellulose in unconventional media. Cellulose, 6, 153–165.

. A. Holst, H. Lask, and M. Kostrzewa, (1978). Process for the production of water absorbing cellulose ethers. US Patent 4068068.

. A. Ikem, O. Osibanjo, M. K. C. Sridhar, and A. Sobande, (2002). Evaluation of ground water quality characteristics near two waste sites in Ibadan and Lagos, Nigeria. Water, Air, and Soil pollution, 140(1-4), 307 - 333.

. G.A Jeffrey, and W. Saenger, (1994). Hydrogen Bonding in Biological Structures. New York: Springer-Verlag, Berlin, Heidelberg, pp 925-944.

. J.F. Kadla, and R.D. Gilbert, (2000). Cellulose structure: a review. Cellulose Chemistry and Technology, 34, 197-216.

. J.D. Keller, (1986). In: M. Gliksman, ed. Sodium carboxymethylcellulose (CMC). Food hydrocolloids. Vol. 3. Boca Raton, Florida: CRC Press, pp. 45–104.

. J.J. Kester, and O.R. Fennema, (1986). Edible films and coatings: A review. Food Technology, 40 (12), 47-59.

. D. Klemm, B. Philipp, T. Heinze, U. Heinze, and W. Wagenknecht, (1998). Comprehensive Cellulose Chemistry: functionalization of cellulose. Vol. 2. Weinheim, Germany: Wiley-VCH, pp 107

. D. Klemm, B. Philipp, T. Heinze, U. Heinze, and W. Wagwnknecht, (2001). Comprehensive Cellulose Chemistry: Fundamentals and Analytical Methods. Vol. 1. Germany, pp. 1, 10, 14, 23, 58.

. F.J. Kolpak, and J. Blackwell, (1976). Determination of the structure of Cellulose II. Macromolecules, 9, 273- 278.

. H. Krassig, and J. Schurz, (1986). Cellulose. Ullmann's Encyclopedia of Industrial Chemistry. Weinheim, Germany: Wiley-VCH, pp 101

. H.A. Krassig, (1993). Cellulose: Structure, Accessibility and Reactivity. Vol.1. Switzerland: Gordon and Brech Science Publishers, pp. 307-313.

. M.R. Ladish, (1989). Biomass Handbook. In: Kitani, O. and Hall, C.W., eds. New York: Gordon and Breach Science Publisher, p. 435.

. H. Lennholm, and T. Iversen, (1995). Nordic Pulp. Paper Research Journal, 10, 104.

. A. Mandal, and D. Chakrabarty, (2011). Isolation of nanocellulose from sugarcane bagasse (SCB) and its characterization. Carbohydrate Polymers, 86, 1292-1299.

. G. Mann, J. Kunze, F. Loth, and H.P. Fink, (1998). Cellulose ethers with a blocklike distribution of the substituents by the structure-selective derivatization of cellulose. Polymer, 39, 3155–3165.

. A.J. Michell, and H.G. Higgins, (1965). Conformation and intramolecular hydrogen bonding in glucose and xylose derivatives. Tetrahedron, 21 (5), 1109-1120.

. A. C. O’Sullivan, (1997). Cellulose: The structure slowly unravels. Cellulose, 4, 173–207.

. A. O. Okhamafe, A.C. Igbobechi, and T.O. Obaseki, (1991) Cellulose extracted from groundnut preliminary physico chemical characterization. Pharmacy world Journal 8 (4) 120-123.

. A. Okoro, E.N. Ejike, and C. Anunso, (2007). Sorption model of modified cellulose as crude oil sorbent. Journal of Engineering and Applied Sciences, 2(2), 282 -285.

. N. Olaru, and L. Olaru, (2001). Influence of organic diluents on cellulose carboxymethylation. Journal of Macromolecular Chemistry and Physics, 202, 207-211.

. J.P. Reddy, and J.W. Rhim, (2014) Characterization of bionanocomposite films prepared with agar and paper-mulberry pulp nanocellulose. Carbohydrate polymers 110, 450-485.

. A.B. Savage, A.E. Young, and A.T. Maasberg, (1954). Ethers. In: E. Ott, H.M. Spurlin, and M.W. Grafflin, eds. Cellulose and Cellulose Derivatives Part II. New York: Interscience Publishers, Inc., pp. 882–954.

. H. Staudinger, (1932). Die hochmolekularen organischen Verbindungen - Kautschuk und Cellulose. Springer Verlag.

. V. Stigsson, G. Kloow, and U. Germgard, (2001). An historical overview of carboxymethyl cellulose (CMC) production on an industrial scale. Paper Asia 10, 17, 16-21.

. G.M. Thomas, E.M. Paquita, and J.P. Thomas, (2002). Cellulose ethers. Encyclopedia of polymer science and technology. New York: Wiley, pp 101.

. H.C. Trivedi, C.K. Patel, and R.D. Patel, (1981). Studies on carboxymethylcellulose: Potentiometric Titrations, 3. Macromoecular Chemistry and Physics, 182, 243-245.

. K. Varshney, and S. Naithani, (2011). Chemical functionalization of cellulose derived from nonconventional sources. Dehra, India: Forest Research Institution.

. D.L. Verraest, J.A. Peters, H.C. Kuzee, J.G. Batelaan, and V.H. Bekkum, (1995). Carboxymethylation of inulin. Carbohydrate Research, 271, 101–112.

. H. Yokoto, (1985). The mechanism of cellulose alkalization in the isopropyl alcohol-water-sodium hydroxide - cellulose system. Journal of Applied Polymer Science, 30, 263-277.

. T. Zimmerman, E. Pöhler, and P. Schwaller, (2005). Mechanical and morphological properties of cellulose fibril reinforced nanocomposites. Advanced Engineering Materials, 12, 1156.