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標題: 含磷難燃性環氧樹脂高分子之研究
Syntheses and Thermal Properties of Phosphorus Containing Epoxy Polymers
作者: 王俊仁
Wang, Jun-Ren
關鍵字: phosphorylated curing agent;含磷硬化劑;epoxy polymer;activation energy;LOI;環氧樹脂;活化能;極限氧指數值
出版社: 材料工程學研究所
本研究主要合成兩系列具胺基之含磷化合物,藉由胺滴定、FTIR、EA及NMR (H1及P31)來鑑定含磷硬化劑結構;並進行與環氧樹脂硬化反應,形成具難燃性之材料。由DSC動態掃描可得知硬化週期,並藉此定出各組硬化劑與環氧樹脂單體BE188之適當硬化條件,此外更藉由不同升溫掃描速率求出各含磷硬化劑與BE188之硬化反應活化能,得知芳香族硬化劑之硬化反應活化能大於脂肪族硬化劑。經硬化後所得之含磷環氧樹脂高分子具有較低之起始熱裂解溫度,此乃因為引入了熱穩定性較差之含磷化合物所致,同時,經由磷化物裂解所形成之焦炭層,可提昇其焦炭殘餘率及LOI值,證實其難燃特性。在TGA升溫過程中,空氣下的環氧樹脂高分子因為高溫時的氧化作用,使其裂解過程較氮氣下為複雜;而在裂解動力學的測定上,則是藉由TGA動態掃描(Ozawa模式)的方式所求得,其中具有苯環結構者,因具有較好的高溫熱穩定性,因此裂解活化能較高。本實驗合成之新型含磷硬化劑藉由硬化過程導入環氧樹脂中,大幅提昇環氧樹脂高分子難燃特性化。

Two series of novel phosphoric amide containing amine curing agents (P%=3~15) were developed in this study. These curing agents were characterized by FTIR, amine titration, elemental analysis and NMR. The curing reactions of these phosphorylated curing agents were studied by differential scanning calormeter (DSC) using dynamic methods. Activation energies of the epoxy monomer BE188 cured with aliphatic or aromatic curing agents were also determined, and the value calculated from aromatic curing agents were larger than those of aliphatic curing agents. These phosphorylated epoxy polymers possessed lower degradation temperatures and higher char yields as compared to the pristine epoxy polymers. The first stage of degradation, which results from the decomposition of phosphorus containing functional groups, exhibited lower activation energy than the other stages. Larger limited oxygen index (LOI) values as well as higher char yields of these polymeric epoxy resins confirmed the effectiveness of phosphorylated epoxy polymers as flame retardants. From TGA data, different degradation stages were found in nitrogen and air, respectively. The kinetic of thermal degradation of phosphorylated epoxy polymers based on BE188 and the above-mentioned curing agents were also studied by Ozawa method. It was found that the epoxy polymer containing aromatic components exhibited larger degradation activation energies. Based on the above, facile introduction of the phosphorus containing functional groups into commercial curing agents has been achieved in this study. As a result of that, the phosphorylated epoxy polymers exhibit enhanced flame retardation properties.
Appears in Collections:材料科學與工程學系

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