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제118회 대한화학회 학술발표회, 총회 및 기기전시회 안내 In situ Monitoring of Thermal Crosslinking Reaction and Residual Vinyl Group of Re-adhesive Organosilicon by VT-NMR

2016년 8월 24일 20시 51분 23초
ANAL2.O-2 이곳을 클릭하시면 발표코드에 대한 설명을 보실 수 있습니다.
금 09시 : 03분
분석화학 - Oral Presentation of Young Analytical Chemists Ⅱ
저자 및
설혜원, 이태희1, 이태곤1, 김정권*, 김종혁1,*
충남대학교 화학과, Korea
1한국화학연구원 화학분석센터, Korea
The re-adhesive property of organosilicon is dependent on the residual vinyl group after the crosslinking reaction of hydrosilylation between vinyl group(Si-V, main chain) and hydrosilyl group(Si-H, crosslinker). When the vinyl group remains, we cannot expect good re-adhesive property because of adhesion over time. In this study, the end-point of crosslinking reactions was determined by variable temperature nuclear magnetic resonance(VT-NMR) spectroscopy. The relationship between adhesion and the residual vinyl group was confirmed by monitoring the crosslinking reaction. Our experiments were done with organosilicon mixture of main chain and crosslinker which has the end- or side-chain vinyl group and hydrosilyl group. Temperature was raised from 298 K to 373 K at a rate of 1.25 K/min and the spectra were recorded for a minute at each 5 K. The end-points of crosslinking reaction were determined by the loss of vinyl group signals and the appearance of crosslinking network(Si-CH2-CH2-Si) signal in distortionless enhanced by polarization transfer(DEPT) spectrum. In case of the most vinyl-terminated poly-dimethylsiloxane, vinyl group signal was disappeared below 373 K. When a vinyl group is positioned beside backbone(vinyl-methylsiloxane), however, it still remained until 373 K. Additionally, we also investigated samples from a supplier and compared the results with our initial work. The adhesive remnant indexes(ARI) were almost the same when the vinyl group signal disappeared, while it changed when the vinyl group signal remained.