World Journal of Engineering OPTIMIZATION OF CELLULOSE FIBER ISOLATION FROM RICE STRAW AND ITS APPLICATION FOR THERMOPLASTIC COMPOSITE FORMATION Siritorn Narkchamnan1 and Chularat Krongtaew1* Department of Chemical Engineering, Faculty of Engineering, Mahidol University, Nakhon Pathom, 73170, Thailand. *E-mail: egchularat@mahidol.ac.th Isolation of natural fibers Rice straw (Oryza sativa) was cut into 2-mm pieces before pre-treatment. The cut rice straw was treated in three consecutive steps: 1) soaking in concentrated alkaline solution at NaOH concentration based on straw dry weight and then washed with 1-L distilled water, 2) hydrolysis by dilute HCl and then washed with 1-L distilled water, and 3) treatment in dilute alkaline solution containing 2%w/w NaOH. Finally, isolated fibers were homogenized to micro-nano scale. The central composite design (CCD) For the central composite design (CCD), variation of soaking time, solvent and NaOH concentrations was in a range of -1 and +1; soaking time (8 to 24h), solvent concentration (10 to 50%v/v) and NaOH concentration (15 to 25%w/w). Regression coefficients of the quadratic model of each response for isolated cellulose fibers from CCD are showed in Table.1. Processing of the biocomposite Starch thermoplastic composite was prepared by mixing of rice straw fibers, glycerol and cassava starch. Isolated cellulose rice straw fibers were added into a proportion of starch-to-glycerol of 50 : 6 %w/w. Composite was formed using compression molding technique at 210C for 6 min. The influence of cellulose fibers in composite was studied by varying the fiber content at 0%, 5%, 10% and 15%w/w. Analyses of fibers and biocomposite Thermogravimetric analysis (TGA) of the starch composite containing 0%, 5%, 10% and 15%w/w cellulose fibers was performed by thermogravimetric analyzer (Pyris Diamond TG/DTA, PerkinElmer) with a heating rate of 10°C/min in nitrogen atmosphere and temperature ranging between 30 and 500°C. Mechanical properties of the composite specimens were determined by using a universal testing machine (Instron 4467, USA) and 3-point bend fixture with a load cell of 0.5 kN. The flexural modulus and strength strain of the composite specimen were then calculated. Introduction Rice is the most export agricultural product of Thailand. Side products from rice processing can be utilized as precursors for alternative energy production, bioplastic formation, natural fertilizer manufacturing, etc [1]. At present, most of plastic industries depend greatly on petroleum sources which are non-degradable. They produce a large amount of plastic waste that has detrimental effect to environment concerning a global warming. Thus, utilization of environmentally friendly resources for biodegradable plastic application has become interesting topic throughout the world [2]. Rice straw, one of the most plentiful agro-residues in Thailand, composed mainly of holo-cellulose, alphacellulose and lignin. Alpha-cellulose in rice straw has crystalline structure that makes it suitable to use for increasing tensile strength and young modulus of plastic [3]. From the earlier work [7], the authors previously published a research work on cellulose isolation from rice straw and the crucial factors influencing alpha-cellulose yield and fiber morphology were reported. In the present work, experimental optimization study on cellulose isolation from rice straw at moderate condition at atmospheric pressure was conducted by using a central composite design (CCD). Isolated cellulose fiber was used for light weight starch thermoplastic formation. Experimental Materials Rice straw (Oryza sativa) was obtained from a local source (Nakhon Chaisee, Nakhon Pathom, Thailand). Chemicals for the experiments on chemical treatment of rice straw and the analyses were analytical grade and purchased from Sigma, Fluka and Ajax Finechem. Cassava starch, glycerol and magnesium stearate used for thermoplastic formation were from Erawan Co., Ltd., Ajax Finechem and Sigma. 1417 World Journal of Engineering Table 1 Regression coefficients of the quadratic models for holo-cellulose, alpha-cellulose, lignin contents and weight loss of isolated cellulose fibers from the CCD. Equation Z=a+bX1+cX2+dX3+eX12+fX22+gX32+hX1X2+iX1X3+jX2X3 Regression Holo-cellulose Alpha-cellulose Lignin Weight loss coefficients of the eq (3) eq (4) eq (5) eq (6) equation (eq) a -8.82 74.04 108.82 101.40 b 3.38 0.26 -3.38 -3.69 c 0.02 -0.02 -1.31 d 7.01 -7.01 e -0.03 0.04 0.03 0.05 f 0.03 0.01 -0.01 g -0.08 0.08 -0.07 h 0.02 0.03 -0.02 0.02 i -0.14 0.01 0.14 0.11 j 0.03 0.03 0.05 R2 0.95 0.51 0.95 0.55 2 R (adj) 0.85 0.24 0.85 0.11 P-value 0.0214 0.3316 0.1195 0.1903 design (CCD). Three factors influencing an increase of alpha-cellulose content and lignin removal including 1) soaking time, 2) solvent and 3) NaOH concentration were used for the experimental design. It was found that the optimum condition for the isolation of the natural fibers was at 24-h soaking time, 10%v/v solvent, and 25%w/w NaOH. From this condition, the alpha-cellulose content was 88.38%w/w and the weight loss was 58.43%. As shown in Fig.1, TGA analysis of starch/glycerol thermoplastic when adding 0%, 5%, 10% and 15% cellulose rice straw fibers demonstrated that an increase of cellulose rice straw fibers in the thermoplastic composite proportion (starch : glycerol of 50 : 6) decreased its degradation temperature. A significant increase of flexural strength and modulus was obtained after adding fibers into the starch thermoplastic composite as illutstrated in Table 2. References 120 100 Weight loss (%) 80 60 40 20 0 0 100 200 300 400 500 600 Temperature (°C) nofiber 10%fiber chemically treated 5%fiber 15%fiber Fig. 1 TGA thermograms of starch thermoplastic composite with different fiber contents (0 – 15%w/w) and chemically treated rice straw fibers. Table 2 Mechanical properties of the composites Strengtha Modulusa (kPa) (MPa) TPS-0% fibers 0.21±0.1 4.65±4.9 TPS-5% fibers 0.34±0.2 11.66±10.2 TPS-10% fibers 0.41±0.1 17.08±6.5 TPS-15% fibers 0.43±0.2 32.83±20.8 a All values are reported as mean ± s.d. (N≥3) TPS = thermoplastic starch Sample 1. William, J. O., Shey, J., Syed, H. I., Grgory, M., Glenn, M. E. and Jean, F. R. (2005). “Application of cellulose microfibrils in polymer nanocomposites”, Journal of Polymers and the Environment, 13, 301-306. 2. Wittaya, T. (2009). “Microcomposites of rice starch film reinforced with microcrystalline cellulose from palm pressed fiber”, International Food Research Journal, 16 493-500. 3. Sain, M. and Alemdar, A. (2008). “Biocomposites from wheat straw nanofibers: Morphology, thermal and mechanical properties”, Composites Science and Technology, 68, 557-565. Results and Discussion The optimization of cellulose isolation from rice straw was carried out by using the central composite 1418