일산화탄소, 에틸렌, 프로필렌의 삼원 공중합; 팔라듐 촉매에 대한 불균일 첨가제의 효과
초록/요약
일산화탄소와 올레핀의 공중합을 통해 합성된 폴리케톤은 우수한 물성을 가진다. 특히, 내화학성과 내마모성이 뛰어나 자동차 내·외장재와 같은 각종 산업자재로의 응용을 기대할 수 있다. 하지만 공정상의 문제점으로 인해, 대량생산 및 상품화에 어려움을 겪고 있다. 일산화탄소와 에틸렌의 교대 공중합을 통해 만들어진 폴리케톤은 Tm 이 높아 가공 시에 상당히 높은 온도가 요구된다. 또한, 팔라듐 촉매와 함께 과량의 불균일 첨가제를 사용하는 기존의 합성법을 통해 얻어진 고분자는 품질이 낮다. 따라서, 본 연구에서는 이러한 문제점을 해결할 수 있는 새로운 합성법을 제안하고자 한다. 팔라듐 매의 활성을 유지하면서 폴리케톤의 품질을 높이기 위해 극소량의 불균일 산촉매를 사용하였고, Tm 을 낮추기 위하여 프로필렌을 추가적으로 사용하여 삼원 공중합을 수행하였다. 이 때 사용된 불균일 산촉매의 크기를 조절하여, 크기에 따라 촉매 활성 및 고분자 특성이 어떻게 변하는지를 연구하였다.
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Abstract ····························································································································· Ⅰ
Contents ···························································································································· Ⅱ
List of Schemes ··············································································································· Ⅳ
List of Figures··················································································································· Ⅴ
List of Tables ···················································································································· Ⅵ
1. Introduction ············································································································ 1
1) Background ······································································································ 1
2) Motive ················································································································ 4
2. Result and Discussion ························································································ 6
1) 사전연구 ··········································································································· 6
2) Pd에 배위한 리간드의 구조에 따른 효과 ········································ 8
3) 불균일 첨가제의 종류에 따른 활성 ·················································· 10
4) 불균일 산촉매의 크기 조절과 활성의 관계 연구 ······················ 12
5) 고분자 반응의 최적화 ············································································· 13
(1) Pressure study ······························································································ 13
(2) Equivalent study ·························································································· 15
(3) Terpolymerization ······················································································· 16
6) 메커니즘 ········································································································· 21
3. Conclusion ············································································································ 23
4. Experimental section ························································································ 24
1) Synthesis of Palladium catalyst ····························································· 24
(1) Pd(dmppp)(OAc)2 ······················································································· 24
(2) Pd(dppp)(OAc)2 ··························································································· 29
(3) Characterization ························································································· ·30
2) Catalytic Terpolymerization Reaction ················································· 33
(1) General Procedure ····················································································· 33
(2) Characterizaiton ·························································································· 34
5. Reference ··············································································································· 38
Abstract······························································································································ 43
