Institute of Polymer Science and Engineering, National Taiwan University, Taipei 10617, Taiwan.
J Colloid Interface Sci. 2010 Mar 1;343(1):209-16. doi: 10.1016/j.jcis.2009.11.018. Epub 2009 Nov 11.
Amine substitution of hexachlorocyclophosphazene (HCP) with poly(oxypropylene)diamines (POP) afforded HCP-POP adducts which were subsequently intercalated into a layered silicate clay. The relative thermal stabilities of the epoxies cured with the phosphazene-amines and the intercalated clays were studied. The organoclays, with the confined HCP-POP from 400 and 2000 g/mol M(w) amines, are nongelled products when using 1/6 M ratio of HCP/POP starting materials in tetrahydrofuran solvent. The intercalation of HCP-POP polyamine salts into sodium montmorillonite afforded the HCP-POP-embedded organoclays with an expanded interlayer silicate spacing (2.4-5.1 nm) from the original 1.2 nm spacing (X-ray diffraction). The effect of silicate clays was evaluated by blending the HCP-POP/clay hybrids into a two-component epoxy system (diglycidyl ether of 4,4'-isopropylidenediphenol (BPA) and a diamine) and fully cured to form solid materials. The distribution of the exfoliated silicate platelets in the matrix was analyzed by transmission electronic microscopy (TEM). Thermal gravimetric analysis (TGA) indicated an enhanced thermal stability for the HCP/clay epoxy nanocomposites, with a delayed weight-loss pattern (temperature of weight loss at 10% (T(10 wt.%)) from 360 to 385 degrees C and temperature of weight loss at 85% (T(85 wt.%)) from 598 to 696 degrees C), compared to the pristine epoxies. By comparing these epoxies with different amounts of phosphazene and/or silicates, the TGA revealed a synergistic effect for the presence of both phosphorous and silicate components. Furthermore, the epoxies had improved physical properties such as hardness (from 3H to 5H) and surface adhesion (observed by scanning electron microscope (SEM) on fracture surface).
六氯环磷腈（HCP）与聚（氧化丙烯）二胺（POP）的胺取代反应得到 HCP-POP 加合物，随后将其嵌入层状硅酸盐粘土中。研究了用磷腈-胺固化的环氧树脂和插层粘土的相对热稳定性。在四氢呋喃溶剂中，当 HCP/POP 起始原料的 1/6 M 摩尔比使用时，用 400 和 2000 g/mol M（w）胺的有机粘土是无凝胶产物。HCP-POP 聚胺盐嵌入钠蒙脱石中得到 HCP-POP 嵌入有机粘土，其层状硅酸盐间隔从原始的 1.2nm 间隔扩展到 2.4-5.1nm（X 射线衍射）。通过将 HCP-POP/粘土混合物混入双组分环氧树脂系统（双酚 A 的二缩水甘油醚（BPA）和二胺）中并完全固化形成固体材料来评估硅酸盐粘土的影响。通过透射电子显微镜（TEM）分析了剥离的硅酸盐片在基质中的分布。热重分析（TGA）表明 HCP/粘土环氧树脂纳米复合材料具有增强的热稳定性，失重模式延迟（失重 10%时的温度（T（10wt.%））从 360 至 385°C，失重 85%时的温度（T（85wt.%））从 598 至 696°C）与原始环氧树脂相比。通过比较这些含有不同量的磷腈和/或硅酸盐的环氧树脂，TGA 表明磷和硅酸盐成分的存在具有协同效应。此外，环氧树脂具有改善的物理性能，如硬度（从 3H 到 5H）和表面附着力（通过扫描电子显微镜（SEM）观察断裂表面）。
