화학공학소재연구정보센터
Polymer(Korea), Vol.44, No.5, 641-651, September, 2020
산화 그래핀-g-폴리(ε-카프로락톤)의 합성과 특성 분석
Synthesis and Characterization of Graphene Oxide-g-Poly(ε-caprolactone)
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초록
폴리염화비닐(PVC)의 인성 향상을 위한 나노필러로 사용하기 위해 산화 그래핀-g-폴리(ε-카프로락톤)(GO-g-PCL)을 합성하고 그 특성들을 분석하였다. 이를 위해 흑연으로부터 제조한 산화 그래핀(GO)에 염화티오닐을 반응시켜 염화아실 유도체화 GO를 얻었으며, 여기에 3가지 분자량(530, 1250, 2000 g/mol)의 폴리(ε-카프로락톤)(PCL)의 반응비를 변화시키면서 50 °C에서 grafting-to법으로 반응시켜 GO-g-PCL을 합성하였다. 합성한 GO-g-PCL은 TGA 분석으로부터 용매열 처리 GO와 비교하여 그래프트율을 구하였다. GO 단위무게당 일정한 몰비의 PCL을 반응시킬 때 PCL 디올의 분자량이 클수록 GO에 그래프트되는 PCL의 상대적인 분자 수는 적어지지만 얻을 수 있는 최대 그래프트율은 커졌다. 그래프트율이 5.3~5.5%로 비슷한 GO-g-PCL을 PVC에 0.3 wt%로 첨가한 PVC/GO-g-PCL 복합체 필름을 제조하고 이들의 인성 변화를 분석하였다. 복합체 필름은 순수 PVC에 비해 매우 큰 인성 증가를 나타내었으며, 그래프팅 시 사용한 PCL의 분자량이 작을수록 증가정도가 커졌다.
Graphene oxide-g-poly(ε-caprolactone) (GO-g-PCL) was synthesized and characterized in order to use it as a nanofiller for enhancing the toughness of poly(vinyl chloride) (PVC). Graphene oxide (GO) prepared from graphite was reacted with thionyl chloride to obtain acyl derivative of GO, and then GO-g-PCL was synthesized by grafting PCLs of three different molecular weights (530, 1250, 2000 g/mol) on it with various reactant ratios at 50 °C using a grafting-to method. Graft yield of the GO-g-PCL was obtained by TGA analysis comparing solvothermal treated GO. When the molar concentration of PCL per g GO was constant during the synthesis, increasing the MW of PCL reduced the number of PCL molecules grafted onto GO but increased the maximum graft yield. PVC/GO-g-PCL composite films were prepared by adding 0.3 wt% of GO-g-PCLs with a similar graft yield of 5.3-5.5% to PVC and their toughness changes were analysed. The composite films showed excellent increases in toughness compared to neat PVC, and the degree of increase was greater when the MW of PCL used for grafting was smaller.
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