以陰離子聚合法合成等嵌段苯乙烯-異戊二烯SISIS共聚物及其氫化前後性質研究

Preparation of SISIS Rubber via Anionic Polymerization and Comparison of the Properties after Hydrogenation

鄒家榕(Jia-Rong Zou)

指導教授 ： 蔣見超

國立中正大學/工學院/化學工程學系/碩士(2015年)

摘要

本論文探討使用二級丁基鋰（sec-BuLi）為反應起始劑，並在非極性環己烷溶劑下進行活性陰離子聚合法合成苯乙烯系列嵌段共聚物，其中分子的硬質段為聚苯乙烯，軟質段為聚異戊二烯（苯乙烯-異戊二烯嵌段共聚物），並改變苯乙烯佔整體中的比例如30%、60%、90%來合成五嵌段的SISIS高分子，後透過全氫化反應使其苯環以及異戊二烯上的雙鍵全部氫化而得到CBC高分子，在使用儀器分析來比較他們的物、化性差異。
利用GPC的鑑定我們可以得知分子量及分子量分佈，並合成相量與絕對分子量的差異。透過1H-NMR的分析可以判斷我們合成的苯乙烯(Styrene)含量確實佔總分子量的約30%、60%、90%，並分析他們不同的加成比例如1,4加成、1,2加成。使用FTIR觀察分析氫化前後的特徵吸收峰變化，並利用TGA、DSC進行熱性質分析。之後利用AFM、SEM觀察氫化後高分子不同結構比例下的表面型態、微相分離變化，最後在使用DSR進行流變學量測。

關鍵字

流變學 ； 相分離 ； CBC ； 氫化 ； 異戊二烯 ； 苯乙烯 ； 陰離子聚合法

並列摘要

This research is to investigate that the sec-Butyl Lithium as an reactive initiator synthesize the block copolymer of the styrene series under the non-polar solvent cyclohexane through living anionic polymerization. In this research, the hard segment of the molecule is polystyrene and the soft segment is polyisoprene. The proportion of styrene was changed to 30 %, 60% and 90% to synthesize the pentablock SISIS. We also completed the reaction of hydrogenation in ITRI to produce the CBC polymer. The final part of this experiment is to figure out the differences between physical properties and chemical properties by using the instrumental analysis to make the comparison.
In order to complete the comparison, the analyses below have been done to produce the final result. According to GPC identification, the relative molecular weight and the distribution of the molecular weight can be acquired. In this research, the polymer with 60,000 molecular weight is produced. Styrene synthesized is verified as around 30%, 60% and 90% of the polymer’s total amount via 1H-NMR and we also use 1H-NMR to analyze the differ additions of polyisoprene as 1,4 addition, 1,2 addition and 3,4 addition. Another apparatus we used to observe the characteristic absorption peak which should appear in the polymer is FTIR. For the thermal properties, TGA and DSC are what we used to figure out the result. AFM and SEM is used to observe the microphase separation and surface morphology changes of hydrogenated polymer in different proportions. Finally, The measurement of rheological properties is completed by DSR.

並列關鍵字

rheology ； microphase separation ； CBC ； isoprene ； hydrogenation ； styrene ； anionic polymerization

參考文獻

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