10.982~990(2060).fm

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1 Ï Ð Journal of the Korean Society of Clothing and Textiles Vol. 35, No. 8 (2011) p.982~990 e fùv p y x Á x w w, w w ƒ Characteristics of Kenaf Fibers Treated by Alkali Hye Ja YooÁHye-Ja Lee Dept. of Clothing & Textiles, Seowon University Dept. of Home Economics Education, Korea National University of Education ( ), ( ), y ( ) Abstract Kenaf fiber can be obtained by decortications of the kenaf plant stem. The properties of the kenaf fiber treated by alkali (NaOH) were investigated by spectrocolorimeter, SEM, X-ray diffractometer, FT-IR and TGA. The kenaf fibers treated by alkali became darker and their Munsell color values changed from Y (yellow) to YR (yellowred) according to an increased NaOH concentration. SEM observation of the kenaf fibers showed that their crimps were developed and their surfaces were cleaned by the removal of protruding ends and impurities after alkali treatments. In the x-ray diffraction analysis, the structures of the fibers were found in the form of cellulose I when treated with a 0-16% alkali concentration and cellulose II when treated with over 20%. It was also confirmed that the crystallinity was lowered according to an increased NaOH concentration. The change of fiber compositions was investigated in FT-IR analysis. Strong band of 1,738cm -1 and asymmetrical stretching strong bands of 1,630-1,600cm -1 in spectrum (which represent pectin) were not found in the samples because the pectin was removed by the alkali treatment. Weak bands of 1,728-1,730cm -1 and peaks of 1,245-1,259cm -1 (which represent hemicellulose) and peaks of 1,592cm -1, 1,504cm -1, 1,462cm -1 and 1,429cm -1 (which are related to lignin) were not found or reduced in the samples treated with a concentration over 20%. TGA indicated that the kenaf fiber had the better hydrophilic properties by alkali treatment. The higher Tmax in TGA and the higher thermal stability when treated by alkali with the higher concentration. The fibers treated with an alkali concentration over 30% did not show any changes in Tmax. Key words: Kenaf, Alkali, Crystallinity, FT-IR, TGA; fùv, e, y Ÿ, I.,, m,, s y š. ù w 20% š,, Corresponding author hjlee@knue.ac.kr w û. t xk s ƒ ƒ s l, s v v, ù, w ƒ š ƒ š (Lee et al., 2007; Park, 2008). w, w û w w s» ƒwš y š. w w ù w 982

2 e fùv p y 117 w» w y wš. e w y, g, fùv ƒ ƒ Ÿ š. ƒ erp,, ü, m, y y š. fùv ù ü w ü š yw w, k š» w w w f (Kevlar) y w (Franck, 2005). fùv w y w» w ƒ y w w š (Cho & Choi, 1996; Lim et al., 2007; Yoo & Lee, 2005). fùv» l ü g v, g ù p š v wý ƒ w» w ƒ y w» j. fùv rp, x,,,. w e w x, rp,, w» w q,, t, y e w y, yw j w e (Parikh et al., 2002; Song & Obendorf, 2006; Yoo et al., 2006). p w ƒœœ w e š w w. fùv» l ƒ»¾ yw œ ƒ Ÿ w š t e yùp j š»¾ w yùp fùv y j w e š, yùp fùv,, y. e fùv w ¼ ù», t xk w y r ù, yw y r w (Lee et al., 2004; Lee et al., 2003: Wang & Ramaswamy, 2003; Yoo et al., 2006) ùyùp w q ƒ 2~4% ù ù t t yww w» yùp p yƒ w m w. w» w s yùp fùv wš»» mw p, p, p y mw fù v w y w w y wš w. II. x 1. fùv v w 120 f ùv yw. fùv» v (bark) (core) w z v g w w. ³ w l 50~60cm v w. 2. e fùv v k e š 24 w z g w. fùv e yùp fù v p w» w yùp 2, 4, 6, 8, 10, 12, 16, 20, 30, 40% w y g 100 o C 60 fùv v ƒƒ wš w z w. ù w m e 24 w z w. 3.»» w fùv p d w yùp w Ÿ (JS-555, Technocolor System, Japan) d wš CIE L, a, b, E Munsell sƒw. x (FE-SEM, NOVA NanoSEM200, FEI Company, USA) w e fùv xk ,000 w. fùv w e y y sƒw» w X-ray Diffrac- 983

3 118 w wz 7PM/P tometer(dmax-2500, Rigaku, Japan) w š z (002 ) z ƒ(2θ 22.5 ) vj z ƒ(2θ 18.5 ) z w Segal w y w. ƒƒ 3mg w w z KBr 200mg yww 600kg/cm 2 pellet š, FT- IR Spectrometer(Thermo Mattson 60AR, USA) d w IR spectrum. e w fùv 8~10mg w z Thermogravimetric Analyzer(TGA Universal V4.2E, TA Instruments, USA) w ƒ w l 600 o C¾ 10 o C d w p y š w. III. š fùv v NaOH 0, 2, 4, 6, 8, 10, 12, 16, 20, 30, 40% w y g 100 o C 1 ƒƒ w z d,, IR rp, X-ray z, TGA w y mw e fùv p y w. 1. y <Table 1> w yùp w fùv t d w. yùp ƒ L (whiteness) û w š ƒw t w ùk û. a* b* +, e ƒ a* ƒ š b* redness ƒ yellowness Y(yellow) y YR(ywllowred) w w š NaOH 30% w y YR(yellowred) d. 2. SEM w xk SEM w e fùv xk ,000 w <Fig. 1> ùkþ. 250 w <Fig. 1> w e ƒ t w Áòw š ƒ ƒ v y ƒ w. 10,000 w <Fig. 2> e ƒ fùv ƒ v yƒ ú (Kwon et al., 1997) 4% ƒ ƒ w ù x j vƒ ù w. 20% w j vƒ wš ³ w y w. Kim et al.(2009) s v v Table 1. Color values of kenaf fiber bundles treated with alkali Temp. ( o Conc. of NaOH Color Values C) (v/v%) L* a* b* E Munsell Hue Reference (MgO White) Y Y Y Y Y Y Y Y YR YR 984

4 알칼리 처리에 따른 케나프 섬유의 특성 변화 연구 Fig. 1. SEM photographs of alkali treated kenaf fibers ( 250). Fig. 2. SEM photographs of alkali treated kenaf fibers ( 10,000)

5 120 w wz 7PM/P p wš 3% 5% yùp w fùv 30% yww w w z q y w 5% w fùv w w ƒ p w û š šw. Mwaikambo and Ansell(2002) hemp, sisal, jute, kapok 0.8~8% yùp w t xk y resin w ƒw š šw. š e w fùv t Áòw j vƒ w w š w š e fùv w p w w w q. 3. X z e w yùp 2~ 10% x I θ vjƒ. 30%, 40% θ vjƒ 22.5 vjƒ x ùkû, II y q (Aguilar-Vega & Cruz-Ramos, 1995). 20%, 30%ù 40% vj ƒ e ù 22.5 vj. yùp 2~16% y j 57~60% ù 20% Table 2. Crystallinity (%) of kenaf treated with various concentration of NaOH aqueous solutions Concentration of NaOH (%) Diffraction Intensity 18.5 o 22.5 o Crystallinity Index (%) untreated % % % % % % % % % % %, 30% 47.8%, 40% 42.8% y ƒ û 20% š w yƒ û y w., 20% w I ƒ š y y ù 20% w I ƒ y š y w. 30% w fùv II ë š y w 20% (Table 2). 4. IR spectrum w yùp w f ùv FT-IR rp <Fig. 1> ùkþ. OH p e 3,340~3,350cm 1 II I w, I 3,350cm 1 parallel polarized bandsƒ ùkù II 3,447cm -1 3,488cm -1 ü w w strong bandsƒ ùkù (Sao, 1987). 0~40%¾ w yùp w f ùv IR rp ü, w w OH streching bandsƒ II xk y y w., 20% y ùkù š, 20% e 3,450cm -1 shoulderƒ ùkù broad w, ü w y q. Singthong et al.(2005) š w 2,850cm 1 w band rp» w 2,850cm 1 bandƒ spectrum ùkûš e z ùkù. 1,250~1,500cm 1 5 peakƒ w ùkù X z ƒ I y w. wr, ù 16%¾ NaOH 1,030~1,025cm 1 úe š w vj ùkþ. 20% 995cm 1 w ƒ ùkùš š 895cm 1 vj ƒ úe cellulose II yƒ š (Kim & Yun, 1986). fùv 1,738cm 1 strong 986

6 e fùv p y 121 band 1,630~1,600cm 1 asymmetrical stretching strong band pectin w 1,738cm 1 band š yùp pectin ùkù. 1,630~ 1,600cm 1 band ùkùù 20% ùkù. Lee et al.(2003) fùv 2~4% yùp w q z rp 2~3% û š šw, š yùp. wr 1,728cm 1 ùkù weak band x e» e» w w, 1,245~1,259cm 1 vj x C-H bending» w yùp w vj p»ƒ x w. Mwaikambo and Ansell(2002) y FT-IR ew. 1,592cm 1, 1,504cm 1, 1,462cm 1, 1,429cm 1 q. ww w 1,592cm 1 1,510~1,500cm 1 x guaiacyl x w w. 16%¾ IR spectrum 1,592~1,600cm 1 1,504cm 1 guaiacylx ƒ ù 20% 30% spectrum š 40% guaiacylx ƒ. 1,232cm 1 syringylx xylan p»(c-o-c) (Kim, 1988; Wang & Ramaswamy, 2003). 30~40% š e spectrum vj ƒ» w ù û. Lee et al.(2006) š fùv e 0.7% ùp yw w w š w. e fùv ƒ w wš» w ù (Fig. 3). 5. TGA w p fùv w e ƒ p e y TGA mw r. TGA l 150 o C¾ w y ùkü, e w ƒ j ùkù (Zini et al., 2003). <Fig. 4> w e w fùv TGA w l 150 o C¾ y ùk ü. 150 o C w TGA ƒ NaOH 20% w 7.3~8.3% j ƒ ùkù ù 30% 9.3%, 40% 10.05% ùkù, e ƒ 20% w w 30% ƒw f ùv w e ƒ 20% w w 30% e y w. TGA wƒ ù Fig. 3. Infrared spectrum of kenaf fiber bundles treated with NaOH aqueous solutions. Fig. 4. Weight loss (%) from room temperature to 150 o C in TGA thermogram of kenaf fiber treated with alkali of various concentrations. 987

7 122 w wz 7PM/P Tmaxƒ 320 o C 70% k w w ƒ ùkù (Aguilar-Vega & Cruz-Ramos, 1995; Salamone, 1996; Zini et al., 2003). <Table 3> w e w fù v TGA w w Tmax y Tmax ùkü t. e w fùv Tmax 347 o C 64% ùkþ. 8% w e w fùv Tmax 372 ~375 o C ùkû w wƒ û Tmax 67~69% ùkû. w w ù Tmax 3~5% ƒ. 10~20% e w fùv Tmaxƒ 390~393 o C 10% w w 20 o Cù ƒ 77~79% 10% ƒ š ü û q. x ù w w š, w ƒ ù v y ƒ y ƒ ùkû. Kwon et al.(1997) šw NaOH w X-ray z, v š g w w x w Table 3. Tmax ( o C) and weight loss (%) at Tmax of kenaf fiber treated with alkali in TGA thermogram Concentration of NaOH (%) Tmax ( o C) Weight Loss (%) wƒ û» q. š 30% 40% yùp w Tmax yƒ ù ƒ ƒ ƒ 86% 91% ùkù ƒ j w. w w w w, fùv sww w w ü š w 30% š w q. IV. fùv q, y,, t w y š y ùp fùv e y w» w 2~40% s w,,,, p»» mw. 1. NaOH ƒ w š Y(yellow) ùkû yùp 30% YR (yellowred) y. 2. e w fùv t x w, t Áòw j vƒ w w p w š w w q % w I ƒ š y j y ù 20% w I ƒ y š y w. 30% w fùv II ë š y w 20%. 4. FT-IR rp fùv 1,738cm 1 strong band pectin w yùp pectin ùkù. 1,728~1,730cm 1 weak band 1,245~1,259cm 1 vj x» w p»ƒ x w. 1,592cm 1, 1,504cm 1, 1,462cm 1, 1,429cm 1 q. 20% e spectrum vj ƒ j 988

8 e fùv p y 123 û ƒ e w y w. 5. l 150 o C¾ TGA w y ùkü, e ƒ 20% w w 30% ƒw fùv w e ƒ 20% w w 30% e y w. 6. e w fùv Tmax 347 o C 8% w e w f ùv Tmax 372~375 o C, 10% e w fùv 390~393 o C ùk ù e ƒ ƒ ù 30% yƒ. e ƒ x ù Tmaxƒ wš ƒ š Tmax ƒ ƒ. References Aguilar-Vega, M., & Cruz-Ramos, C. A. (1995). Properties of henequen cellulosic fibers. Journal of Applied Plymer Science, 56, Cho, N. S., & Choi, T. H. (1996). Manufacturing of Korean traditional paperg (Hanji) from fast-growing new fiber plant kenafg (Hibiscus Cannabinus). Journal of Korea Tappi, 28(4), Franck, R. R. (2005). Bast and other plant fibres. Cambridge, England: Woodhead publishing Limited. Han, Y. S., Yoo, H. J., Lee, H. J., Rhie, J. S., Kim, J. H., Song, K. H., & Ahn, C. S. (2003). Research for kenaf fiber production in Korea. Journal of the Korean Society of Clothing and Textiles, 27(7), Kim, K. J., & Yun, B. S. (1986). Application of fourier transform infrared spectroscopy to qualitative and quantitative analysis of fiber blendsg (I). Journal of the Korean Society of Textile Engineers and Chemicals, 23(3), Kim, S. S., Lee, B. H., Kim, H. J., Oh, S. C., & Ahn, S. H. (2009). Mechanical properties of alkali treated kenaf fiber filled PP bio-composites. Mokchae Konghak, 37(3), Kim, Y. S. (1988). Application of infrared spectroscopical techniques for investigation archaeological woods. Mokchae Konghak, 16(4), 3 9. Kwon, H. Y., Park, Y. H., & Kong, Y. S. (1997). Effect of NaOH treatment on the structure and physical properties of flax fiber. Journal of the Korean Fiber Society, 34(2), Lee, H. J., Ahn, C. S., Kim, J. H., Yoo, H. J., Han, Y. S., & Song, K. H. (2004). Characteristics of kenaf/rayon fabrics. Journal of the Korean Society of Clothing and Textiles, 28(9/10), Lee, H. J., Han, Y. S., & Yoo, H. J. (2006). The change of kenaf fiber characteristics by the contents of noncellulosic material. Journal of the Korean Society of Clothing and Textiles, 30(11), Lee, H. J., Han, Y. S., Yoo, H. J., Kim, J. H., Song, K. H., & Ahn, C. S. (2003). Effect of chemical retting on the fiber seperation of kenaf bast. Journal of the Korean Society of Clothing and Textiles, 27(9/10), Lee, H. J., Yoo, H. J., & Han, Y. S. (2007). The properties of kenaf/polyester blended nonwovens. Journal of the Korean Society of Clothing and Textiles, 31(7), Lim, O., Lee, H. J., Yoo, H. J., & Han, Y. S. (2007). The production of kenaf hand-made paper. Journal of the Korean Society of Clothing and Textiles, 31(8), Mwaikambo, L. Y., & Ansell M. P. (2002). Chemical modification of hemp, sisal, jute and kapok fibers by alkalization. Journal of Applied polymer Science, 84(12), Parikh, D. V., Calamari, T. A,. Sawhney, A. P. S., Blanchard,G E. J., Screen, F. J., Warnock, M., Muller, D. H., & Stryjewski, D.G D. (2002). Improved chemical retting of kenaf fibers. Textiles Research Journal, 72(7), Park, S. M. (2008). Trend of technical textiles. Dyeing and Finishing, 8, Salamone, J. C. (Ed.). (1996). Polymeric materials encyclopedia Vol. 4G(F-G)U Boca Raton, FL: CRC Press. Sao, K. P., Mathew, M. D., & Ray, P. K. (1987). Infrared spectra of alkali treated degummed ramie. Textiles Research Journal, 57(7), Singthong, J., Ningsanond, S., Cui, S. W., & Goff, H. D. (2005). Extraction and physicochemical characterization of Krueo Ma Noy pectin. Food Hydrocolloids, 19(5), Song, K. H., & Obendorf, S. K. (2006). Chemical and biological retting of kenaf fibers. Textile Research Journal, 76(10), Wang, J., & Ramaswamy, G. N. (2003). One-step Processing and bleaching of mechanically separated kenaf fibers: Effects on physical and chemical properties. Textiles Research Journal, 73(4),

9 124 w wz 7PM/P Yoo, H. J., & Lee, H. J. (2005). Production and application of kenaf fiber. Fiber Technology and Industry, 9(2), Yoo, H. J., Lee, H. J., Kim, J. H., Ahn, C. S., Song, K. H., & Han, Y. S. (2006). The change of physical characteristics of kenaf fiber by the chemical processes. Journal of the Korean Society of Clothing and Textiles, 30(7), Zini, E., Scandola, M., & Gatenholm, P. (2003). Heterogeneous acylation of flax fibers reaction kinetics and surface properties. Biomacromolecules, 4,