Polymer(Korea), Vol.20, No.2, 182-190, March, 1996
주사슬에 실페닐렌-실록산기를 갖는 새로운 방향족 폴리아미드의 합성과 물성
Synthesis and Characterizations of New Aromatic Polyimides Containing Silphenylene-Siloxane Moieties in the Main Chain
초록
주사슬에 실리콘을 함유하는 새로운 방향족 폴리아미드 (PIM, PIP시리즈)를 실페닐렌-실록산기를 갖는 단량체인 1,3-bis(m-aminophenyl)-1,1,3,3-tetramethyldisiloxane(DMDA) 또는 1,3-bis(p-isocyanatophenyl)-1,1,3,3-tetramethyldisiloxane (DMIS)과 스피로아세탈 및 다양한 방향족 단량체와의 축합중합에 의하여 합성하였다. 이들 중합체들의 구조는 FT-IR, 1H-NMR, 원소분석 그리고 WAXD로 확인하였으며 열적성질 및 열안정성은 DSC와 TGA로 측정하였다. PIM 및 PP시리즈의 중합체들은 용액점성도가 0.25-0.41 dL/g의 범위였으며, DMF, DMAc, DMSO, NMP같은 유기용매에 쉽게 용해되는 성질을 보여주었으며 제조된 중합체의 Tg와 Tm은 각각 100-170℃ 및 245-315℃였다. 또 TGA에 의해 확인된 중합체의 IDT와 T10은 질소 분위기하에서 각각 290-400℃ 및 312-415℃였다. 이들 두 시리즈는 X-선 분석 결과 모두 반결정형의 구조를 갖는 것으로 판명되었다.
New aromatic polyimides (PIM and PIP series) having silicone moieties in the main chain were prepared by the polycondensation reaction of meta- and para-oriented silphenylene/siloxane containing monomers with spiroacetal and other aromatic monomers. The monomers employed were 1,3-bis(m-aminophenyl)-1,1,3,3-tetramethyldisiloxane(DMDA) and 1,3-bis-(p-isocyanatophenyl)-1,1,3,3-tetra-methyldisiloxane (DMIS). The structures and thermal properties of these polymers were determined by FT-IR, 1H-NMR, elemental analysis, WAXD, DSC, and TGA. PIM and PIP series of polymers had inherent viscosities in he range of 0.25-0.41 dL/g. They were readily soluble in various organic polar solvents such DMF, DMAc, and NMP. The Tg and Tm of these Polymers were detected over the temperature range of 100-170℃ and 245-315℃, respectively, according to their DSC traces. The thermal stabilitles of these polymers were also evaluated by TGA, which showed that their IDT and T10 were in the range of 290-400℃ and 312-415℃, respectively, under the nitrogen atmosphere. WAXD patterns of PIM and PIP series showed that their structures were semi crystalline.
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