Applied Chemistry for Engineering (공업화학)

The Korean Society of Industrial and Engineering Chemistry (한국공업화학회)
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Synthesis and Properties of Siloxane Containing Copolyimides

실록산이 함유된 폴리이미드의 합성과 물성

  • Moon, Yoon-Duk (Department of Industrial Chemistry, College of Engineering, Hanyang University) ;
  • Lee, Young Moo (Department of Industrial Chemistry, College of Engineering, Hanyang University)
  • 문윤덕 (한양대학교 공과대학 공업화학과) ;
  • 이영무 (한양대학교 공과대학 공업화학과)
  • Received : 1991.07.01
  • Published : 1991.12.30
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Abstract

Siloxane containing copolyimide (SPI) was synthesized from 3, 3', 4, 4'-benzophenonetetracarboxylic dianhydride(BTDA), 4, 4'-methylene dianiline(MDA), 4, 4'-oxydianiline(ODA) and amine-terminated polydimethyl-siloxane(PDMS). Homopolyamic acid(HPAA) in tetrahydrofuran(THF) was reacted with PDMS to obtain siloxane containing polyamic acid(SPAA) followed by the thermal curing to manufacture SPI. SPAA and HPAA exhibited inherent viscosity value of 0.35~0.48dl/g. Glass transition temperature of SPI ranged in $258^{\circ}C{\sim}264^{\circ}C$. SPI had a lower $T_g$ than that of HPI. ODA based HPI and SPI showed slightly higher $T_g$ values, thermal stability, and water content.

3, 3', 4, 4'-Benzophenonetetracarboxylic dianhydride(BTDA)와 방향족 디아인민 4, 4'-oxydianiline(ODA) 및 amine terminated polydimethyl siloxane(PDMS)을 이용하여 homopolyimide(HPI)와 siloxane 함유 polyimide(SPI)를 합성하였다. 제 1 단계 반응생성물인 homopolyamic acid(HPAA)는 극성용매인 N-methylpyrrolidone(NMP)을 이용하여 얻었다. 제 1 단계에서 얻은 HPAA와 tetrahydrofuran(THF)에 녹인 세 종류의 PDMS(분자량 $M_n=1700g/mol$, 4000g/mol, 7000g/mol)를 30wt%로 반응시켜 siloxane-copolyamic acid (SPAA)를 얻은 후 이를 thermal curing하여 SPI를 얻었다. SPI및 HPI의 precursor인 SPAA와 HPAA의 inherent viscosity는 0.35~0.48dl/g이었다. 함수율은 SPI는최저 0.998%, HPI는 최저 1.88%정도였다. BTDA/MDA/siloxane계의 유리전이온도는 $258^{\circ}C-267^{\circ}C$이었다. 열중량 분석 결과 BTDA/ODA/siloxane계의 경우가 BTDA/MDA/siloxane계보다 다소 높은 분해 온도를 갖는 것으로 나타났다.

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