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Tetramethyldisiloxane -1,4- bis ( dimethylhydroxysilyl ) benzene 공중합체의 합성 및 특성
Syntheses and Properties of Copolymers of Tetramethyldisiloxane and 1,4- Bis ( dimethylhydroxysilyl ) benzene
김선일 , 윤영재 , 나재운 ( Sun Il Kim , Young Jae Yun , Jae Woon Na )
공업화학 7권 3호 490-495(6pages)
UCI I410-ECN-0102-2009-570-007331818

Organocyclosiloxane oligomer[(R₂SiO)_n, n= 2, 3, 4, 5]와 dimethyldichlorosilane을pyridine N-oxide 촉매 존재하에서 개환 반응시켜 linear chlorine terminated siloxane(yields;71.2∼86.5%)를 얻었다. 0℃에서 linear chlorine terminated siloxane과 dimethylamine을 반응시켜 amine terminated siloxane oligomer(yields;76.2∼85.3% )를 얻은 후 이 화합물들과 1,4-bis(dimethylhydroxysilyl)benzene을 반응시켜 공중합체들(yields;58.0∼71.0% )을 합성하였다. 이들 공중합체의 구조는 FT-IR 및 ¹H-NMR로 확인하였으며, DSC 및 TGA thermogram을 통하여 이들 중합체들의 열적특성을 사하였다. TGA thermogram으로부터 polymer I (n=2)의 초기분해온도는 476℃로 가장 낮았고, Polymer IV(n=5)가 485℃로 가장 높았다. n의 수가 증가할수록 열안정성은 다소 우수한 것으로 관찰되었고, DSC thermogram에서 중합체들의 유리전이온도는 polymr IV (n=5)가 -76℃로 가장 낮았으며, n의 수가 감소할수록 높게 나타났음을 알 수 있었다.

Low molecular weight linear chlorine terminated siloxanes (yields;71.2∼86.5% ) were prepared by reactions of cyclotri-, cyclotetra- and cyclopentasiloxane with dimethyldichlorosilane in the presence of pyridine N-oxide catalyst. The amine terminated siloxane oligomers were obtained in good yields(76.2∼85.3%) by he reaction of linear chlorine terminated siloxanes with dimethylamine at 0℃. In this investigation, we have studied on the syntheses and properties of copolymers (yields;58.0∼71.0%) obtained from the reaction of amine terminated siloxane oligomers with 1,4-bis(dimethylhydroxysilyl) benzene. The structures and properties of the copolymers were examined by FT-IR, ¹H-NMR, TGA and DSC. Initial degradation temperatures(T_D^i) of the polymer I and IV were confirmed as 476 and 485℃, respectively. The thermal stabilities of the polymers were found to be increased with increasing n of (R₂SiO)_n²The glass transition temperatures(Tg) of the polymers were increased with decreasing n of (R₂,SiO)_n, and the lowest Tg revealed -76℃ when n=5.

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