Elastomers and Composites

The Rubber Society of Korea (한국고무학회)
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Preparation and Characterization of Cellulose Nano-Whiskers Extracted from Microcrystalline Cellulose by Acid Hydrolysis

산 가수분해를 이용하여 microcrystalline cellulose로부터 추출 된 cellulose nano-whisker의 특성분석

  • Jeong, Hae-Deuk (Polymer Processing Research Lab, Department of Polymer Science and Engineering, Kumoh National Institute of Technology) ;
  • Yoon, Chang-Rok (Polymer Processing Research Lab, Department of Polymer Science and Engineering, Kumoh National Institute of Technology) ;
  • Lee, Jong-Hyeok (Polymer Processing Research Lab, Department of Polymer Science and Engineering, Kumoh National Institute of Technology) ;
  • Bang, Dae-Suk (Polymer Processing Research Lab, Department of Polymer Science and Engineering, Kumoh National Institute of Technology)
  • 정해득 (국립금오공과대학교 고분자공학과) ;
  • 윤창록 (국립금오공과대학교 고분자공학과) ;
  • 이종혁 (국립금오공과대학교 고분자공학과) ;
  • 방대석 (국립금오공과대학교 고분자공학과)
  • Received : 2010.02.17
  • Accepted : 2010.03.19
  • Published : 2010.03.30
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Abstract

Cellulose nanowhiskers (CNW) gamered increasing interest for their remarkable reinforcement of polymer composites. In this work, we were to produce cellulose whiskers from commercially available microcrystalline cellulose (MCC) by acid hydrolysis with sulfuric and hydrochloric acids. Electron microscopy found that each acid produced sililar cellulose crystals of diameters ranging from 20 to 30 nm and lengths ranging from 200 to 300 nm. Moreover, all samples showed remarkable flow birefringence through crossed polarization filters. Conductometric titration of CNW suspensions revealed that the sulfuric acid treated sample had a surface charge of between 140.00 mmol/kg and 197.78 mmol/kg due to sulfate groups, while that of the hydrochloric acid treated sample was undetectable. Thermogravimetric analysis showed that the thermal decomposition temperature and apparent activation energy (evaluated by Broido's method at different stages of thermal decomposition.) of H1-CNW - prepared by hydrolysis with hydrochloric acid - was higher than those of S1-CNW and S2-CNW - prepared by hydrolyzing MCC with sulfuric acid.

본 연구에서는 친환경적인 특징을 가지면서도 우수한 기계적 특성을 가지고 있어 고분자 복합재료의 보강제로 주목 받고 있는 Cellulose nanowhisker (CNW) 를 염산 혹은 황산을 사용한 산가수분해 방법을 이용하여 Microcrystalline cellulose (MCC) 로 부터 추출하였다. 염산 혹은 황산을 사용하여 추출된 CNW는 직경이 20 에서 30nm 정도였고, 길이가 200 에서 300 nm 로써, 형상학적 측면에서 유사한 특성을 가지는 것을 확인하였다. 또한 전해질 용액의 전기전도도를 이용한 적정 (conductometric titration) 결과 황산을 이용하여 제조되어진 CNW의 경우, 셀룰로오스 표면의 sulfate group 에 의해 나타나는 표면전하 값이 각각 140, 197.78 mmol/kg으로 나타났으며, 염산을 이용하여 제조되어진 CNW 의 경우 셀룰로오스 표면에 약한 전하 값을 가져 표면전하 값을 구할 수 없었다. 황산을 이용하여 추출된 CNW의 열중량 분석 결과 염산을 이용하여 추출된 CNW와 비교하여 열분해 온도가 급격히 감소하는 것을 확인할 수 있었으며, Broido's method를 이용하여 정의 되어진 열분해 거동에 대한 활성화 에너지 역시 상대적으로 낮음을 확인할 수 있었다.

Keywords

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