화학공학소재연구정보센터
Applied Chemistry for Engineering, Vol.30, No.1, 81-87, February, 2019
에너지화 열가소성 탄성체에 사용될 수 있는 알콕시 계열과 알킬 아민 계열 GAP Copolymer의 합성 및 분석
Synthesis and Characterization of Alkoxy and Alkylamino GAP Copolymer for Energetic Thermoplastic Elastomer (ETPE)
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초록
에너지화 열가소성 탄성체 제조에 사용될 수 있는 새로운 계열의 glycidyl azide polymer (GAP)을 모색하기 위해 전구 체인 poly(epichlorohydrin) (PECH)에 친핵체인 아지드기와 알콕시 및 알킬 아민을 도입하여 4가지 GAP copolymer polyol을 합성하고 물성에 대하여 고찰하였다. 이 GAP copolymer 합성반응은 이종의 친핵체를 1단계 반응으로동시에 치환하여 미반응 sodium azide가 남지 않는 친환경적이며 효율적인 합성법으로 평가할 수 있다. 역개폐 짝풀림(inverse gated decoupling) 13C NMR 분석법과 Fourier transform infrared (FT-IR) 분석법으로 상대적 치환율을 정량적으로 분석하 였으며 반응 진행도를 모니터링 하였다. 합성된 GAP copolymer의 유리전이온도와 분자량은 differential scanning calorimetry (DSC)와 gel permeation chromatography (GPC)로 분석하였다. 합성된 poly(GA0.8-butoxide0.2), poly(GA0.7-n-butylamine0.3), poly(GA0.7-dipropylamine0.3), poly(GA0.7-morpholine0.3)의 유리전이온도는 -39 ℃에서 -26 ℃ 범위의 값을 나타내었다.
In this study, synthetic methods and physical properties for a new class of glycidyl azide polymer (GAP) were investigated for energetic thermoplastic elastomers (ETPE). Four kinds of GAP copolymer polyols were synthesized by introducing nucleophiles such as azide, alkoxide and alkyl amine into poly(epichlorohydrin) (PECH). The GAP copolymer synthetic reaction can be evaluated as an environmental benign and efficient synthetic method due to the simultaneous one-step reaction using two kinds of nucleophiles and the complete consumption of sodium azide. The relative stoichiometric substitution ratio analysis and the progress of reaction were checked and monitored by inverse gated decoupled 13C NMR and Fourier transform infrared (FT-IR) spectroscopy. The glass transition temperature and molecular weight were measured by differential scanning calorimetry (DSC) and gel permeation chromatography (GPC) analysis. The synthesized poly(GA0.8-butoxide0.2), poly(GA0.7-n-butylamine0.3), poly(GA0.7-dipropylamine0.3) and poly(GA0.7-morpholine0.3) had a glass transition temperature ranged from -39 to -26 ℃.
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