磷基改質環氧樹脂之結構、耐燃性及熱裂解動力學研究

Study on the Structure, Fire-retardant Properties and Thermal Pyrolysis Kinetics of Epoxy Resin Modified Phosphorus Groups

李宗翰(Tsung-Han Lee)

指導教授 ： 鄭俊麟 ； 華沐怡

中原大學/工學院/化學工程研究所/碩士(2006年)

https://doi.org/10.6840/cycu200600713

摘要

本論文研究含磷環氧樹脂在製造印刷電路板的過程中所產生的揮發性物質予以收集並分析其組成。利用 FTIR、LC-MS 檢測物質之組成，利用 TGA 來得到含磷環氧樹脂之熱重損失。
由 FTIR 與 LC-MS 結果可看出，DOPO 在經過 130 ℃ 加熱冷凝系統收集揮發物後之組成仍是 DOPO 結構，比較其 TGA 圖後發現在 130 ℃ 前的重量損失只是水分與 DOPO 的蒸發。含磷環氧樹脂經過 185 ℃ 加熱冷凝系統收集揮發物經由 FTIR 與 LC-MS 檢測之後發現，揮發物以 DMF 與丙酮為主，另有少量的 2MI 與環氧基反應之末端側鏈的斷裂，因此其 TGA 圖在 185 ℃ 前的重量損失主要為溶劑的逸散。
論文研究的第二個部分利用 PPy 與 PPy/clay 複合物添加於環氧樹脂中，利用 PPy 中的 Amine group 與環氧樹脂中的環氧基進行開環硬化反應使結構更加的緻密，藉此希望可提高材料的熱穩定性與耐燃性。從 IR 圖中發現 Amine group 與環氧基有進行開環反應，接著比較 DSC以及熱裂解反應動力學數據後發現添加 2.5 wt% 添加物於環氧樹脂中具有較高的玻璃轉移溫度以及熱裂解反應活化能，LOI 的研究中可以發現添加物會使材料的耐燃性提升。

關鍵字

環氧樹脂 ； 聚吡咯 ； 動力學

並列摘要

The aim of this research was to study the volatility substance produced during the manufacturing process of Printed Circuit Board (PCB) using phosphorus-containing epoxy resin as the materials. The chemical structure and composition of the volatility substance was analyzed by Fourier transform infrared (FTIR) spectroscopy and Liquid Chromatography-Mass (LC-MS), respectively. The weight loss of epoxy resin was studied by Thermogravimetric (TGA).

For IR and LC-MS spectra, no composition change was found for volatility substance of 9,10-dihydro-9-oxa-10-Phosphaphenanthrene- 10-oxide (DOPO) before and after heating at 130 ℃. In comparison with the result of TGA, the weight loss after heating at 130 ℃ was due to the evaporation of water and DOPO. However, the volatility substances were mainly of DMF and acetone after heating at 185 ℃.as measured by FTIR and LC-MS, which caused the weight loss shown by TGA.

Influences of additives such as Polypyrrole (PPy) and PPy/clay on the thermal stability of epoxy resin were also studied. The ring open reaction between Amine group and epoxy group was confirmed as measured by IR. The highest of Tg and ΔH were obtained when the additive content was 2.5 wt% as analyzed by DSC. The anti-combustion capability of the composites was also increased with the addition of PPy as shown by the limit oxygen index (LOI) test.

並列關鍵字

epoxy ； polypyrrole ； clay ； kinetic

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