Synthesis and Characterization of New Polyamides Containing 1,3-Bis(p-carboxyphenyl)-1,1,3,3-tetramethyldisiloxane
Lee SM, Kim KS, Park KT
1,3-Bis(p-carboxyphenyl)-1,1,3,3,-tetramethyldisiloxane을 함유하는 새로운 폴리아미드의 합성과 성질
이수민, 김기수, 박경택
Abstract
New aromatic polyamides having silicon moieties in the main chain were prepared by polycondensation reaction of silphenylene/siloxane-containing monomer with spiroacetal and other aromatic monomers. The silphenylene/siloxane-containing monomer type employed was 1,3-bis(p-chlorocarbonylphenyl)-1,1,3,3-tetramethyldisiloxane (DMCL). The structures of these polymers were determined by FT-IR, 1H-NMR and elemental analyses. Their thermal properties were characterized by DSC and TGA. The polymers had inherent viscosities in the range of 0.21∼0.69dL/g. These polymers were readily soluble in various polar solvents such as DMF, DMAc, DMSO and NMP. The melting transition (Tm), initial decomposition (IDT) and 10% weight loss temperatures (T10) of these polymers were detected over the temperature range of 196∼282℃, 352∼415℃ and 394∼464℃, respectively. The structures of PAS series as determined by WAXD indicated that they were found to be semicrystalline.
주사슬에 실리콘을 함유하는 새로운 방향족 폴리아미드를 실페닐렌/실록산기 함유 단량체와 스피로아세탈을 비롯한 다양한 방향족 단량체와의 축합중합으로 합성하였다. 이때 사용된 실페닐렌/실록산 함유 단량체 는 1,3-bis(p-chlorocarbonylphenyl)-1,1,3,3-tetramethyldisiloxane (DMCI)였다. 합성된 이들 중합체의 구조는 FT-IR, 1H-NMR 그리고 원소분석으로 하였으며 열적 성질은 DSC와 TG.A로 측정하였다. 합성된 중합체들의 용액점성도는 0.21∼0.69 dL/g였으며 DMF, DMAc, DMSO 그리고 NMP와 같은 극성 용매에 용해되는 성질을 가졌다. 중합체의 녹음 전이온:.(Tm), 초기분해온도(IDT) 그리고 10% 질량손실온도(T10)는 각각 196∼282℃, 352∼415℃ 그리고 394∼464℃였다. 고광각 X-ray 회절(WAXD) 실험 결과 PAS 시리즈 중합체는 반결정형의 구조를 소유하는 것으로 판명되었다.