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H - Terminated Polyfluoroorganosiloxane 을 이용한 Liquid Silicone Rubber 의 제조와 그 특성
강두환(Doo Whan Kang),이권수(Kweon Soo Lee),여학규(Hak Gue Yeo),심정섭(Jung Sup Shim) 한국공업화학회 2002 공업화학 Vol.13 No.6
Octamethylcyclotetrasiloxane (D_4)과 1,3,5-trifluoropropylmethylcyclotrisiloxane (D_3^Me, CH2CH2CF3)을 1,1,3,3-tetramethyldisiloxane (MS)과 평형중합시켜 실리콘의 Si 원자에 dimethyl 및 trifluoropropyl기가 도입된 α, ω-hydrogen terminated poly (dimethyl-methyltrifluoropropyl)siloxane prepolymer (HPMFS)를 제조하였으며, 또한 D_4와 1,3,5-exaphenylcyclotrisiloxane (D_3^Ph2)을 MS와 평형중합시켜 Si 원자에 dimethyl 및 diphenyl기가 도입된 α, ω-hydrogen terminated poly (dimethyl-diphenyl)siloxane prepolymer (HPMPS)를 제조하였다. 제조한 HPMFS 및 HPMPS의 구조를 FT-IR 및 ^13C-NMR을 이용하여 확인하였다. 백금 촉매 하에서 양말단에 vinyl기가 도입된 polydimethylsiloxane (ViPDMS)에 HPMFS 및 HPMPS의 함량비를 5, 10 및 15phr로 달리하여 첨가한 다음 고속배합교반기를 이용하여 액상실리콘(liquid silicone rubber, LSR)을 제조하였다. 이때 HPMFS 및 HPMPS의 함량비를 달리하여 제조한 LSR의 경화반응 속도는 DSC를 이용하여 측정하였다. 이 때 각각 5, 10, 15 및 20 ℃/min.로 승온속도에 따른 발열 피이크로부터 얻은 activation energy를 사용하여 비교하였다. 또한 제조된 LSR의 가교밀도는 115 ℃에서 oscilation rheometer를 이용하여 측정하였다. α, ω-Hydrogen terminated poly(dimethyl-diphenyl) siloxane prepolymer (HPMPS) was prepared using the equilibrium polymerization of octamethylcyclotetrasiloxane (D_4), 1,3,5-trifluoropropylmethylcyclotrisiloxane (D_3^Me, CH2CH2CF3), and 1,1,3,3-tetramethyl disiloxane (MS). α, ω-Hydrogen terminated poly (dimethyl-methyltrifluoropropyl) siloxane prepolymer (HPMFS) was also prepared by the equilibrium polymerization of octamethylcyclotetrasiloxane (D_4), 1,3,5-hexaphenylcyclotrisiloxane (D_3^Ph2), and MS. The chemical structures of HPMFS and HPMPS were confirmed by FT-IR and ^13C-NMR. Liquid silicone rubber (LSR) was prepared from the reaction of vinyl polydimethylsiloxane (ViPDMS) and HPMFS or HPMPS with platinum catalyst at high stirring rate. The concentration of HPMFS and HPMPS were varied from 5 to 10 and to 15 phr based on ViPDMS. For each concentration of HPMFS and HPMPS, DSC measured the curing properties of LSR; heating rates were 5, 10, 15, and 20 ℃/min. The activation energy was calculated from the exothermic peak temperature, Cross-linking density of LSR was measured by oscillation rheometer at 115 ℃.