Effect of Heat Treatment and Particle Size on the Crystalline Properties of Wood Cellulose

입자크기 및 열처리가 목재 셀룰로오스의 결정 특성에 미치는 영향

Abstract

This study was carried out to investigate the effect of heat-treatment and particle size on the crystalline properties of the wood cellulose. The color of wood flours was changed from light yellow in control sample to dark yellow or deep brown by heat treatment at $100^{\circ}C$ to $200^{\circ}C$. Relative crystallinity of the heat treated wood cellulose decreased with decreasing particle size from wood chips to 200 mesh, and there was little change in the crystal width. As the temperature was increased, relative crystallinity of the wood increased and crystal width was not changed. As a result of the FT-IR analysis, it was confirmed that the peaks were gradually decreased at -OH elongation as the heat-treated temperature was increased. The lignin C-H bending of $1425cm^{-1}$ and the hemicellulose C-H bending of $1370cm^{-1}$ did not change with the increase of the heat treatment temperature. In addition, it was revealed that C-C stretching of carbohydrate near $1031cm^{-1}$ decreased with increasing heat treatment temperature. Consequently, it is suggested that particle size and heat treatment affected the crystalline properties of wood cellulose.

본 연구에서는 목분입자 크기 및 열처리가 목재 셀룰로오스의 결정 특성에 미치는 영향을 검토하기 위하여 형태학적 특성, 셀룰로오스 결정특성, 화학성분분석을 실시하였다. 목분의 색은 열처리 온도가 $100^{\circ}C$에서 $200^{\circ}C$로 높아짐에 따라, 진한 황색에서 진한 갈색을 보였다. 열처리 목재셀룰로오스의 상대결정화도는 목재?에서 200 mesh로 목재의 입자 크기가 작아질수록 낮은 값을 보였으며, 결정폭의 변화는 거의 없었다. 온도가 $100^{\circ}C$에서 $200^{\circ}C$로 증가함에 따라 목재의 상대결정화도가 증가하였고, 결정 폭의 변화는 뚜렷하지 않았다. FT-IR분석 결과, 열처리 온도가 높아짐에 따라 -OH 신축에서 피크가 점차 감소한 것을 확인하였다. $1425cm^{-1}$의 리그닌 C-H 굽힘과, $1370cm^{-1}$의 헤미셀룰로오스 C-H 굽힘은 열처리 온도의 증가에 따른 차이를 보기 어려웠다. $1235cm^{-1}$의 OH-phenolic 신축의 특성 피크와 $1031cm^{-1}$ 부근의 탄수화물의 C-C 신축이 열처리 온도가 높아질수록 감소한 것을 확인할 수 있었다. 결론적으로 목재의 입자크기 및 열처리는 목재 셀룰로오스의 결정특성 변화에 영향을 주는 것이 확인되었다.

Fig. 1. Hammer mill¹ and continuous grinder² usedto prepare the wood. Sources: ¹(Hammer Mill Vertica DFZK [GM], BühlerGmbH Germany); ²(KOREAMEDI CO., LTD. Korea).

Fig. 2. Appearance of wood flours treated at different temperatures.

Fig. 3. Micrographs of heat-treated wood flours at different temperatures.

Fig. 4. X-ray diffraction patterns of heat-treated wood samples of different sizes.

Fig. 5. Fourier-transform infrared spectroscopy (FTIR) spectra of 100-mesh heat-treated wood flours at different temperatures.

Table 1. Weight loss of wood flours under different conditions

Table 2. Effect of heat treatment on the crystalline properties of wood samples of different sizes

Table 3. Assignment of the infrared bands to functional groups in wood

Table 4. Assignment of the infrared bands to functional groups in wood (Bodirlau and Teaca., 2009; Dai and Fan, 2011; Wang et al., 2012).