Please use this identifier to cite or link to this item: http://hdl.handle.net/11455/59095
標題: 線性、高分歧狀與規則樹枝狀聚醯亞胺/聚醯胺之製備與性質探討
Preparation and Properties of Linear, Hyperbranced and Dendritic Polyimides/Polyamides
作者: 林慶炫
關鍵字: 材料科技
應用研究
摘要: A series of phosphorus-containing linear, hyperbranched and dendritic polyimides willbe prepared in this project. Novel diamines (2-4) will be prepared by the reaction of DOPO,aniline and 4-nitrobenzaldehyde, p-nitroacetophenone, 4-nitrobenzophenone, respectively.And, a series of polyimides will be prepared by diamines (2-4). Two A-B type monomers(9-10) will also be prepared, and polyimides (13-14) will be prepared. In the second year, aAB2 monomer (20) will be synthesized, and hyperbranched polyimides will be prepared.Three dendrons, [G-0]NO2, [G-1]NO2 and [G-2]NO2 will be prepared by the reaction of3-nitrophthalic anhydride, aniline and monomer (19). And three dendrimers [G-0]3C,[G-1]3C, [G-2]3C will be prepared by the nitro-displacement of compound (24) and[G-0]NO2, [G-1]NO2 and [G-2]NO2, respectively.The structure of synthesized monomer will be confirmed by FTIR, elemental analysis(EA), mass spectra (MS) and NMR spectra. Thermal properties of synthesized polyimideswill be studied using differential scanning calorimetry (DSC), dynamic mechanical analysis(DMA) and thermal gravimetric analysis (TGA). The structure-property relationship will bediscussed.
本計劃合成一系列磷系線性、分歧狀與樹枝規則狀聚醯亞胺與聚醯胺。在線性聚醯亞胺方面,先由DOPO、苯胺分別與4-nitrobenzaldehyde, p-nitroacetophenone,4-nitrobenzophenone 反應,形成雙胺單體(2-4),再和一系列雙酸酐反應成聚醯亞胺。另此,本計劃亦由DOPO,酚分別與4-aminoacetophenone 與4-aminobenzophenone 經三步驟合成A-B 型單體(9-10),將(9-10)在TPP/pyridine 或DBOP/ET3N 催化下聚合形成poly(amic acid)(11-12),最後熱閉環成聚醯亞胺(13-14)。在分歧狀聚醯亞胺方面,則是由DOPO、苯胺和benzophenonetetracarboxylic acid dimethyl ester 合成一AB2 單體(16)。接著在TPP/pyridine 或DBOP/Et3N 催化下進行單體(16)的縮合,形成hyperbranchedpoly(amic acid methyl ester)(17),之後再進行閉環形成hyperbranched polyimide (18)。在第二年計劃中,則將DOPO、苯胺與4,4’-dihydroxybenzophenone 反應合成具有兩個酚基及一個苯胺基的AB2單體(19),接著將AB2單體(19)和4-fluoroisophthalic anhydride反應形成具有OH 基與F 基的AB2 單體(20)。最後,將(20)以鹼催化下聚合成hyperbranched polyimide(21)。接著,利用苯胺和3-nitrophthalic anhydride 合成[G-0]NO2,再利用單體(19)的酚基和[G-0]NO2 的硝基進行親核性硝化取代(nitro-displacement),形成[G-1]NH2 接著,[G-1]NH2 的胺基和3-nitrophthalic anhydride 酸酐基進行縮合,形成[G-1]NO2 反應重複進行,形成dendrons [G-2]NO2。之後,再將dendrons 與含三個酚基的化學物(24),進行親核性硝化取代,形成規則樹枝狀聚醯亞胺。本計劃利用FTIR,元素分析(EA),質譜分析(MS),紅外線光譜儀(FT-IR)及核磁共振光譜(NMR)進行合成單體鑑定。以微差掃描熱分析(DSC)量測聚醯亞胺的玻璃轉移溫度(Tg);以動態機械性質分析儀量(DMA)測聚彈性模數及各級分子鏈弛轉移溫度。以熱重分析儀(TGA)量測其裂解溫度(Td),並探討聚醯亞胺結構與物性之關係。
URI: http://hdl.handle.net/11455/59095
其他識別: NSC97-2221-E005-031-MY2
文章連結: http://grbsearch.stpi.narl.org.tw/GRB/result.jsp?id=1749150&plan_no=NSC97-2221-E005-031-MY2&plan_year=98&projkey=PB9801-1341&target=plan&highStr=*&check=0&pnchDesc=%E7%B7%9A%E6%80%A7%E3%80%81%E9%AB%98%E5%88%86%E6%AD%A7%E7%8B%80%E8%88%87%E8%A6%8F%E5%89%87%E6%A8%B9%E6%9E%9D%E7%8B%80%E8%81%9A%E9%86%AF%E4%BA%9E%E8%83%BA%2F%E8%81%9A%E9%86%AF%E8%83%BA%E4%B9%8B%E8%A3%BD%E5%82%99%E8%88%87%E6%80%A7%E8%B3%AA%E6%8E%A2%E8%A8%8E
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