Polymer(Korea), Vol.27, No.1, 17-25, January, 2003
원자 이동 라디칼 중합을 이용한 Polystyrene-b-Poly(acrylic acid) 블록 이오노머의 합성 및 분석
Synthesis and Characterization of Polystyrene-b-Poly(acrylic acid) Block Ionomer via Atom Transfer Radical Polymerization
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초록
원자 이동 라디칼 중합(ATRP)을 이용하여 CuBr/N,N,N',N'',N''-pentamethyldiethylene triamine 촉매 시스템하에서 용액중합으로 polystyrene 거대 개시제와 polystyrene-b-t-poly(butyl acrylate) (PS-b-P(tBA)) 블록 공중합체를 합성한 후, 가수분해를 통해 polystyrene-b-poly(acrylic acid) 양친매성 블록 공중합체를 얻었다. 또한, 이를 중화하여 블록 이오노머를 제조하였다. 합성된 PS-b-P(tBA) 블록 공중합체는 분자량이 5000-10000 정도로 조절되었고, 분자량 분포도 1.2 이하로 비교적 좁게 나타났다. 공중합체는 1H-NMR, FT-IR로 분석하였으며, DSC로 열적 성질을 측정한 결과, styrene의 비율이 더 많기 때문에 100 ℃ 근처에서 Tg가 나타났으며, TEM을 통해 이온 그룹의 상분리를 확인하였다.
Using atom transfer radical polymerization (ATRP), polystyrene macroinitiators and polystyrene-b-poly(t-butyl acrylate) (PS-b-P(tBA)) block copolymers were synthesized by CuBr/PMDETA catalyst system in solution. After hydrolysis, polystyrene-b-poly(acrylic acid), amphiphilic block copolymers, were formed. Subsequent neutralization of polyacid block led to the block ionomers. The molecular weight of the synthesized PS-b-P(tBA) block copolymers was easily-controlled to 5000-10000 and their distributions were less than 1.2. The chemical structures of the synthesized block copolymers were characterized by 1H-NMR and FT-IR. In the DSC thermograms, Tg appeared in the vicinity of 100 ℃ because of higher styrene content. In addition, the phase separation of the block ionomers was observed by TEM.
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