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研究生:葉文亮
研究生(外文):Wen-Liang Yeh
論文名稱:以苯乙烯-馬來酸酐共聚合物接枝聚乙二醇之合成及其應用
論文名稱(外文):Synthesis and Application of Styrene-Maleic Anhydride Copolymer Grafted by Poly (ethylene Glycol)
指導教授:陳志勇陳志勇引用關係王振乾王振乾引用關係
指導教授(外文):Chuh-Yung ChenCheng-Chien Wang
學位類別:碩士
校院名稱:國立成功大學
系所名稱:化學工程學系碩博士班
學門:工程學門
學類:化學工程學類
論文種類:學術論文
論文出版年:2002
畢業學年度:90
語文別:中文
論文頁數:84
中文關鍵詞:馬來酸酐聚乙二醇接枝共聚合物交流阻抗
外文關鍵詞:polyethylene glycolsolid-state polyelectrolytemaleic anhydridecomb-like
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本文以苯乙烯-馬來酸酐共聚合物(Styrene Maleic anhydride copolymer,簡稱SMA)與PEG(Polyethylene glycol),利用酸酐與醇的酯化反應合成出具醚基側鏈之接枝共聚合物,簡稱SMA-g-PEG。文中探討反應物比例、PEG的分子量、添加之鋰鹽濃度等因素對此接枝共聚合物的物性以及導電行為的影響。經由紅外線光譜(FT-IR)以及核磁共振光譜(7Li NMR)分析聚合物內鋰離子的分佈情形,結果顯示鋰離子被PEG的醚基所溶合。由DSC的結果得到鋰鹽濃度的增加,因PEG上之醚基鏈段與鋰離子形成類似物理性架橋的結構,所以其玻璃轉移溫度(Tg)會隨著鋰鹽濃度的增加而提高。TGA的結果也顯示,添加鋰鹽會提昇共聚合物之熱裂解溫度。最後,本文以交流阻抗技術(AC Impedance)來量測不同組成及不同鋰鹽濃度對接枝共聚合物於導電度的影響。結果得知各組成之共聚合物的導電度隨鋰鹽濃度的上升有先上升後下降的現象。此乃因為鋰鹽濃度的增加,增加了可供離子導電的鋰離子數量,同時亦增加了聚合物中物理性架橋的程度,使鋰離子的運動性(mobility)下降,造成導電度隨著鋰鹽濃度的增加有一極大值存在。再者,由變溫導電度的量測,發現此共聚合物符合VTF方程式,表示此聚合物之導電方式乃是利用高分子醚基側鏈的鏈運動帶動鋰離子而導電。
The preparation of SMA (styrene-maleic anhydride copolymer) and PEG (polyethylene glycol) comb-like copolymer as a solid-state polyelectrolyte was employed by esterification with anhydride and alcohol. The state of lithium ion is copolymer was characterized by Fourier-transform infrared (FT-IR) and 7Li solid-state NMR. In addition, the effect of lithium on the physical properties of copolymers was also measured by differential scanning calorimeter (DSC) and thermal gravity analysis (TGA). From the FT-IR and 7Li solid-state NMR spectra, the interactions of lithium ions and the ether oxygen of the PEG segments is observed. The Tg and Td of copolymer with salts doped was obviously increased from the DSC and TGA result. These results indicated the interactions of lithium ion with PEG segment form transient cross-links inside the copolymers.The conductivity corresponding to the various PEG recipes and dopping LiClO4 concentration in graft copolymer were investigated. All of the conductivity of copolymer was located in the range of 10-5 to 10-7 Scm-1 from the AC Impedance measurement, and existed maximum value that related to the composition of copolymer and dopping lithium ion concentration. The mechanism of conductivity for this copolymer was following the Vogel-Tamman-Fulcher (VTF) theory.
中文摘要……………………………………………………………………I
英文摘要……………………………………………………………………II
誌謝…………………………………………………………………………III
總目錄………………………………………………………………IV
表目錄………………………………………………………………VI
圖目錄……………………………………………………………VII
符號一覽表…………………………………………………………………IX
第一章 緒論………………………………………………………………1
第二章 文獻回顧
2-1 前言…………………………………………………………………5
2-2 高分子離子導體的組成和結構……………………………………5
2-2.1 高分子基材的種類……………………………………………5
2-2.2 金屬離子源的種類………………………………………………8
2-2.3 高分子金屬錯合物的形成和結構…………………………10
2-3 錯合物的離子導電原理…………………………………………13
2-3.1晶體空位擴散模型………………………………………………16
2-3.2自由體積模型……………………………………………………16
2-4 高分子離子導電體的電化學行為……………………………18
2-4.1 離子遷移率…………………………………………………18
2-4.2 電化學穩定性………………………………………………20
2-5 研究動機……………………………………………………………21
第三章 實驗部分
3-1 試藥………………………………………………………………25
3-2 儀器……………………………………………………………25
3-3 實驗方法及步驟………………………………………………26
3-3.1 反應物之前處理…………………………………………26
3-3.2 SMA-g-PEG接枝共聚合物之合成…………………………27
3-3.3 紅外線光譜分析(IR)……………………………………………28
3-3.4 熱裂解分析(TGA)………………………………………………28
3-3.5 微差熱掃描分析(DSC)…………………………………………28
3-3.6 元素分析(EA) …………………………………………………28
3-3.7 核磁共振光譜分析(NMR)……………………………………28
3-3.8 交流阻抗分析(AC Impedance)…………………………………28
第四章 結果與討論
4-1 SMA-g-PEG共聚合物之結構鑑定………………………………30
4-1.1 紅外線光分析(IR)……………………………………………30
4-1.2元素分析(EA)………………………………………………32
4-1.3 核磁共振光譜分析(13C CP/MAS NMR)………………………32
4-2 添加LiClO4對SMA-g-PEG物性上的影響………………………33
4-2.1紅外線光分析(IR)……………………………………………33
4-2.2核磁共振光譜分析(7Li NMR)…………………………………34
4-2.3微差熱掃描分析(DSC)…………………………………………35
4-2.4熱裂解分析(TGA)………………………………………………36
4.3 交流阻抗分析(AC Impedance)……………………………………36
第五章 結論…………………………………………………………40
參考文獻……………………………………………………………41
自述………………………………………………………………………84
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