Elastomers and Composites

The Rubber Society of Korea (한국고무학회)
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Elucidation of the Vulcanization Structures of Filled cis-1,4-Polybutadiene Rubber by Solid State Carbon-13 NMR Spectroscopy

고체상태 NMR을 이용한 cis-1,4-polybutadiene 충진고무의 가황가교 구조 규명

  • Kim, Su-Dong (Dept. of Polymer Science and Engineering, Chungnam National University) ;
  • Park, Eun-Kyung (Small and Medium Business Administration) ;
  • Ryu, Ju-Whan (Dept. of Polymer Science and Engineering, Chungnam National University)
  • 김수동 (충남대학교 공과대학 바이오응용화학부) ;
  • 박은경 (중소기업청) ;
  • 류주환 (충남대학교 공과대학 바이오응용화학부)
  • Published : 2008.12.31
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Abstract

Using solid state $^{13}C$ NMR, polybutadiene rubber vulcanizates were qualitatively and quantitatively analyzed. In the filled conventional system of BR vulcanizate accelerated with TBBS, addition to the olefinic double bond and substitution in the $\alpha$ position to the double bond occurred simultaneously. Also the latter $\alpha$ substitution reaction was faster than the former addition reaction at initial reaction time. In addition, it was suggested that double bond-addition-polysulfide structures might be modified into 5-membered and 6-membered cyclic structures in overcure time. These chain modifications were correlated with the decrease in the chemical crosslink density in overcure time.

고체상태 $^{13}C$ NMR을 이용하여 폴리부타디엔 고무(BR) 가황체의 정성 및 정량분석을 행하였다. TBBS로 촉진된 기존의 충진 BR 가황체에서는 올레핀성 이중결합에의 부가반응과 이중결합 옆의 $\alpha$ 위치에서의 치환반응이 동시에 일어났다. 또한 반응 초기에는 이중결합 옆의 $\alpha$ 위치에서의 치환반응은 이중결합에의 부가반응보다 빠르게 진행되었다. 한편 과가류(overcure) 시간 동안 이중결합-부가 폴리설파이드 구조는 5각형 및 6각형 고리 구조로 변형되는 것으로 추정되었다. 이러한 사슬 변형은 과가류 시간에 발생하는 화학적 가교 밀도와 상관되었다.

Keywords

References

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