Studies on the Modified Polyimide Resins Obtained from Rosin. 2. Synthesis and Properties of Polyamideimides via Tetracarboxylic Dianhydride Monomer Containing Preformed Bisamide
Kim JS, Choi HK
Rosin을 이용한 변성폴리이미드수지에 관한 연구. 2. 비스아미드 함유 사염기산이무수물 단량체를 경유하는 폴리아미드이미드의 합성과 물성
김점식, 최형기
Abstract
Tetracarboxylic dianhydride monomers containing preformed bisamide (bisamide) were synthesized from two diamines and rosin-maleic anhydride adduct (RMA) made from rosin and maleic anhydride. The polyamideimides have been obtained by the polycondensation reaction of the bisamide with various aromatic diamines catalyzed by triphenylphosphite in NMP solvent. The effect of copolymerization by means of varing two diamines in polymer unit on their characteristics was examined. The polymers were characterized by infrared, elemental analysis, x-ray diffractometry and inherent viscosity measurement. The viscosity of polymers ranges from 0.23 to 0.55d1/g ; higher viscosity was obtained from the homopolymers prepared by using only one kind of diamine such as 4,4''-diaminodiphenylether (ηinh of polymer, 0.55 dl/g) or 4,4''-diaminodiphenylmethane (ηinh of polymer, 0.53d1/g). The results of thermal analysis showed that the polymers had good thermal stability with the initial decomposition temperature ranging from 335 to 355℃. Isothermal ageing data also indicated that the polyamideimides were stable at 200℃ since no weight loss occurs even after 72hr heating in air.
Rosin과 말레산무수물로부터 RMA를 합썽하고 이를 두종류의 디아민과 반응시켜서 비스아미드 함유 사염기산이무수물단량체 (비스아미드)를 제조하였다. 비스아미드단량체와 몇가지 디아민을 NMP용제 내에서 triphenylphosphite를 촉매로 사용하여 축중합하였고. 디아민의 공중합효과를 검토하였다. 중합체는 IR. 원소분석, X-선회절분석 및 고유점성도의 측정으로 확인하였다. 중합체의 점성도는 0.23∼0.55dl/g의 범위였으며, 디아민이 각각 4, 4''-diaminodiphenylether 또는 4, 4''-diaminodiphenylmethane만으로 된 단일중합체의 점성도가 각각 0.55d1/g, 0.5361/g으로서 공중합체보다 높았다. 열분석결과 중합체의 초기분해온도는 335∼355℃의 범위로서 내열특성이 우수하였으며. 공기중에서의 등온내열성시험에서 200℃ (72hr)이하에서는 각 중합체의 중량감소가 거의 없었다.