Journal of the Korean Industrial and Engineering Chemistry, Vol.13, No.6, 594-599, October, 2002
H-Terminated Polyfluoroorganosiloxane을 이용한 Liquid Silicone Rubber의 제조와 그 특성
Preparation and Characteristics of Liquid Silicone Rubber Using H-terminated Polyfluoroorganosiloxane
E-mail:
초록
Octamethylcyclotetrasiloxane (D4)과 1,3,5-trifluoropropylmethylcyclotrisiloxane (D3 (Me, CH2CH2CF3))을 1,1,3,3,-tetramethyldisiloxane (MS)과 평형중합시켜 실리콘의 Si원자에 dimethyl 및 trifluoropropyl기가 도입된 α,ω-hydrogen terminated poly (dimethyl-methyltrifluoropropyl)siloxane prepolymer (HPMFS)를 제조하였으며, 또한 D4와 1,3,5-hexaphenylcyclotrisiloxane (D3(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 15 phr로 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. 이때 각각 5, 10,15 및 20 ℃/min.로 승온속도에 따른 발열 피이크로부터 얻은 activation energy를 사용하여 비교하였다. 또한 제조된 LSR의 가교밀도는 115 ℃에서 oscillation rheometer를 이용하여 측정하였다.
α,ω-Hydrogen terminated poly(dimethyl-methyltrifluoropropyl) siloxane prepolymer (HPMFS) was prepared using the equilibrium polymerization of octamethylcyclotetrasiloxane (D4), 1,3,5-trifluoropropylmethylcyclotrisiloxane (D3 (Me, CH2CH2CF3)), and 1,1,3,3,-tetramethyl disiloxane(MS). α,ω-Hydrogen terminated poly (dimethyl-diphenyl) siloxane prepolymer (HPMPS) was also prepared by the equilibrium polymerization of octamethylcyclotetrasiloxane (D4), 1,3,5-hexaphenylcyclotrisiloxane (D3 (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 ℃.
Keywords:α,ω-hydrogen terminated poly(dimethyl-methyltrifluoropropyl) siloxane (HPMFS);α,ω-hydrogen terminated poly(dimethyl-diphenyl)siloxane (HPMPS);liquid silicone rubber;crosslinking density
- Zhu M, Chung DDL, Composites, 22(3), 219 (1991)
- Nielsen LE, Ind. Eng. Chem. Fundam., 13(1), 17 (1974)
- Korea Patent, 072659 (1998)
- Taniguchi H, Key Eng. Mat., 159, 39 (1999)
- Lee HH, Lee HJ, Kim JH, J. Korean Ind. Eng. Chem., 7(4), 633 (1996)
- Momper B, Wagner T, Maschke U, Bullaufl M, Polym. Commun., 31, 186 (1990)
- Kang DW, Kim YM, J. Ind. Eng. Chem., 5(4), 280 (1999)
- Japan Patent, 平8-325457
- Sau KP, Khastgir D, Chaki TK, Angew. Makromol. Chem., 258, 11 (1998)
- McGrath JE, Riffle JS, Yilgor L, Banthia AK, ACS Symp. Ser., 2(211) (1983)
- Park SG, Ko SW, J. Korean Fiber Soc., 32(5), 494 (1995)
- U.S. Patent, 3,337,497
- Gilbert AR, Kantor SW, J. Polym. Sci., XL, 35 (1959)
- Jang J, Yi J, Polym. J., 27(4), 404 (1995)