Synthesis and Morphological Characterization of Sodium and Calcium Clay Nanostructured Poly(ε-Caprolactam) [Nylon 6] Hybrids

S. Vega-Díaz, F. Medellín-Rodríguez, S. Sánchez-Valdes, B. Handy, J. M. Mata-Padilla, O. Dávalos-Montoya
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Abstract

The synthesis and morphological characterization of Nylon 6 hybrids using the most common montmorillonite types, sodium and calcium, are reported. Two local nanoclays and a commercial, cation exchanged, reference were used in order to obtain the hybrid products. The local sodium and calcium nanoclays were first homoionized and then ion ex- changed with surfactants, being the main purpose to obtain similar reaction precursors as the commercial clay. Both local clay precursors and commercial clay showed similar crystallographic structure and layer-to-layer spacing after all phys- icochemical treatments. The best reaction conditions were first determined and then a simple infra-red based technique was implemented with the purpose to obtain the molecular weight of the hybrid products. It was determined that, sodium, calcium, and commercial nanoclays render relatively similar molecular weights of nanoclay hybrids using identical syn- thesis conditions. Thermal analyses indicated the formation of two and three melting endotherms in all cases depending on the isothermal crystallization temperature. X-ray diffraction patterns displayed crystal plane truncation which is usually observed in nanoclay hybrids. Plane truncation depended on the nanoclays nature, although the highest truncation was ob- served with commercial and sodium nanoclays. X-rays dispersion results allowed to infer the partial formation of non- hybrid polymer depending on the type of clay, sodium nanoclay showing the lesser proportion, and as a consequence the highest hybridization. Transmission electron microscopy results corroborated the relative degree of exfoliation and nano- clay dispersion of the hybrid products.
钠钙粘土纳米结构聚(ε-己内酰胺)[尼龙6]杂化物的合成及形态表征
本文报道了用最常见的蒙脱土类型钠和钙合成尼龙6杂化物及其形态表征。采用了两种本地纳米粘土和一种阳离子交换的商业参考材料,以获得杂交产物。首先对局部钠钙纳米粘土进行均离子化,然后与表面活性剂进行离子交换,以获得与商品粘土相似的反应前驱体。经过各种物理化学处理后,本地粘土前驱体与商品粘土的晶体结构和层间距相似。首先确定了最佳反应条件,然后采用简单的红外技术测定了杂化产物的分子量。结果表明,在相同的合成条件下,钠纳米粘土、钙纳米粘土和商用纳米粘土的分子质量相对相似。热分析表明,在所有情况下,根据等温结晶温度,形成两个和三个熔化吸热体。x射线衍射图显示了纳米粘土杂化体中常见的晶面截断现象。平面截断取决于纳米粘土的性质,但商用纳米粘土和钠纳米粘土的截面积最大。x射线色散结果可以根据粘土的类型推断非杂化聚合物的部分形成,钠纳米粘土显示的比例较小,因此杂化程度最高。透射电镜结果证实了杂交产物的相对剥落程度和纳米粘土的分散程度。
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