聚甲基丙烯酸甲酯（PMMA）由於具有高的光穿透性、高硬度與高耐候性等許多優點，所以被廣泛的應用在日常生活中。不幸的，PMMA本身是屬於高可燃性塑膠，使得它在許多領域應用上受到限制。因此，為了提高PMMA的耐燃性與熱穩定性，增加它的商業價值與應用範圍，本研究主要目的就是分別添加反應型的水滑石與磷系難燃劑而合成出具高耐熱性的難燃型PMMA。
本研究第一部份即是利用改良式二階段本體聚合法製備出不同LDH-U含量的剝離型LDH-U/PMMA奈米複合材料，LDH-U則是利用共沈澱的方式製備，主要是當做反應型無機難燃劑使用。本研究使用X-ray繞射儀與穿透式電子顯微鏡來分析LDH-U在PMMA中的分散行為。具有5 wt% LDH-U添加量的LDH-U/PMMA奈米複合材料（PMMAL5），在結束預聚合反應後，水滑石層板就已被剝離且均勻的分散在預聚合物中。微差掃瞄熱卡計與熱重分析儀的實驗結果說明了這些奈米複合材料均比PMMA具有更高的玻璃轉移溫度（Tg）與5％重量損失溫度（T5%）。當添加5 wt %的LDH-U時，奈米複合材料的Tg與T5%分別比純PMMA高出22 oC與89 oC，而這些奈米複合材料的抗拉強度與楊氏模數同樣高於純的PMMA，且隨著LDH-U的添加量增加而增加。在難燃性質部分，經由極限耗氧指數（LOI）與UL-94測試結果表示，雖然添加5 wt%的 LDH-U可以提高LOI，但仍然無法有效的抑制燃燒。
本研究第二部分即是利用苯基二氯磷酸酯先與2-烴乙基-甲基丙烯酸酯進行酯化反應，然後經由水解步驟而合成出2-甲基丙醯乙基苯基磷酸酯（MEPP）；MEPP主要是當做反應型磷系難燃劑使用，之後使用二階段本體聚合法製備出不同MEPP含量的MEPP/MMA共聚合物。藉由Fineman-Ross、Kelen-Tüdos與Joshi-Joshi三種不同方法來探討MEPP/MMA聚合系統的單體反應比。分析結果顯示出MEPP與MMA主要是進行隨機共聚合反應，且高分子鏈上的自由基比較傾向與MEPP單體反應。MEPP的加入，在輕微降低PMMA的Tg下，可大幅提昇PMMA的熱穩定性，而LOI與UL-94測試結果證實，當MEPP的添加量為20 wt%時，MEPP/MMA共聚合物可以有效的抑制燃燒而具有難燃的特性。
凝聚相產物的分析結果說明MEPP/MMA共聚合物的裂解可大致被區分成下列六個部分：（1）不穩定P-O-C aromatic與aliphatic結構的斷裂、（2）MMA的脫除、（3）MEPP單元上酯基的分解與碳酸酐結構的生成、（4）碳酸酐結構的分解、（5）甲基結構的斷裂以及（6）P-O-P與P-O-Φ複合結構的生成。綜合氣相產物的分析結果， MEPP/MMA共聚合物裂解所產生的氣相產物隨著溫度升高，依序為MMA、phenol、alcohol/phosphate、aldehyde、CO/CO2。最後，根據凝聚相產物與氣相產物的分析結果，本文提出了MEPP/MMA共聚合物可能的熱裂解機構。

Poly(methyl methacrylate) (PMMA) is widely used in various industries because of its high optical transmission, hardness, and weatherability. Unfortunately, PMMA is a high flammability plastic, which has limited its use in many applications. The fire resistance and thermal stability of PMMA need to be urgently improved to increase its commercial value and range of industrial applications. Therefore, the main aim of this investigation is to synthesize flame-retardant PMMA with high thermal-resistance by incorporating reactive layered double hydroxides (LDHs) and phosphorus-containing flame retardant, respectively.
In the first part of this study, the exfoliated LDH-U/PMMA nano- composites containing various contents of LDH-U were prepared in a modified two-stage process by bulk polymerization. The 10-undecenoate intercalated LDH (LDH-U) for use as a reactive inorganic flame retardant was prepared via the co-precipitation method. Moreover, the dispersed behavior of the LDH-U in the PMMA matrix was identified by X-ray diffraction and transmission electron microscopy. For the LDH-U/PMMA nanocomposite containing 5 wt% LDH-U (PMMAL5), the LDH layers were exfoliated and homogeneously dispersed in the pre-polymer matrix following the pre-polymerization. All these nanocomposites significantly demonstrate enhanced glass transition temperature (Tg) and decomposition temperatures at 5% weight loss (T5%) compared to the pristine PMMA, as identified by differential scanning calorimetry and thermogravimetric analysis. For example, the Tg and T5% of PMMAL5 increased by 22 oC and 89 oC, respectively. In addition, the ultimate tensile strength and Young’s modulus of these nanocomposites was also enhanced by incorporating the LDH-U into the PMMA matrix and increasing it with the amount of LDH-U. The fire-retardant properties of these nanocomposites were also studied by limiting oxygen index (LOI) and UL-94 tests, indicating that PMMAL5 cannot effectively inhibit burning, despite having higher LOI value than that of the pristine PMMA.
In second section of this study, 2-methacryloxyethyl phenyl phosphate (MEPP), as a phosphorus-containing flame retardant, was synthesized via the esterification of phenyl dichlorophosphate with 2-hydroxyethyl methacrylate, followed by hydrolysis. The MEPP/MMA copolymers containing various contents of MEPP were prepared by two-stage bulk polymerization. Moreover, the monomer reactivity ratios of MEPP/MMA system were calculated by three methods of Finemann-Ross, Kelen-Tüdös and Joshi-Joshi, indicating that MEPP undergoes random copolymerization with MMA, and MEPP enters preferentially into the polymer chain. The thermal stability of MEPP/MMA copolymers was considerably enhanced with only a slight reduction in Tg. LOI and UL-94 tests provide considerable evidence that a MEPP/MMA copolymer with only 20 wt% MEPP (PMMA20) can effectively inhibit burning and exhibit flame retardance.
According to the analytical results of the condensed-phase products, the thermal degradation of MEPP/MMA copolymer can be roughly separated into six portions: (1) the scissions of the least stable P-O-C aromatic and aliphatic structures, (2) the elimination of MMA, (3) the ester group decomposition accompanying the formation of carbonic anhydride structure, (4) the decomposition of carbonic anhydride structure, (5) the scissions of methyl group and (6) the formation of P-O-P and P-O-Φ complex structures. The volatilized products for the thermal degradation of MEPP/MMA copolymer were characterized by TGA/FT-IR technique, indicating that the volatilized products were MMA, phenol, alcohol/phosphate, aldehyde and CO/CO2, depending on the temperature of onset formation. Finally, possible mechanisms for the thermal degradation of MEPP/MMA copolymer were also proposed in accordance with the analytic results of condensed-phase and volatilized products.

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