Formation of Polyamide Nanoclusters at the Interfaces of Reverse Micelles Adsorbed and Their Application to Separation.

为了研究用固定的反胶束作为微反应器制备接枝聚酰胺刷表面的可行性，用十六烷基三甲基氯化铵(CTAC)反胶束吸附在二氧化硅表面，合成了尼龙6，6。尼龙改性硅胶的制备过程包括：(1)将含有1，6-己二胺和氢氧化钠的CTAC反胶束吸附到硅胶表面；(2)在反胶束界面上原位聚合1，6-己二胺和己二氯；(3)去除CTAC或反胶束等残留组分。利用反胶束技术考察了硅胶对1，6-己二胺的吸附行为。用1，1，1，3，3，3-六氟-2-丙醇从硅胶中回收尼龙后，用红外光谱对其进行鉴定，并用凝胶渗透色谱测定其相对分子质量和分子量分布。固定化尼龙的脱附行为表明，尼龙固定在二氧化硅上的主要作用可能是尼龙端胺基团与表面硅醇基团之间的氢键作用。用热重分析和透射电子显微镜对固定化过程进行了研究。在接触模式下，用原子力显微镜(AFM)对附着在玻璃板表面的尼龙单分子膜进行了表征。原子力显微镜照片显示尼龙单分子膜表面形成了接枝的聚合物刷子或纳米团簇，并以改性的硅胶粒子为固定相，对制备的硅胶表面进行了表征。该固定相稳定，并成功地用于以环己烷或其与二氧六环混合物为流动相分离邻位、间位和对位硝基苯甲醚。

For the purpose of studying the feasibility of preparing a surface modified with grafted polyamide brushes using a reverse micelle immobilized as a microreactor, nylon-6,6 was synthesized in cetyltrimethylammonium chloride (CTAC) reverse micelles adsorbed on silica surfaces. The nylon-modified silica gel preparation procedure involved: (1) adsorption of the CTAC reverse micelles containing 1,6-hexanediamine and sodium hydroxide onto silica gel surfaces, (2) in situ polymerization of 1,6-hexanediamine and adipoyl dichloride at the reversed micellar interfaces, and (3) the removal of residual components such as CTAC or reverse micelles. The adsorption behavior of 1,6-hexanediamine onto silica gels using the reverse micelles was also examined. After retrieving the produced nylon from the silica gel using 1,1,1,3,3,3-hexafluoro-2-propanol, infrared spectroscopy was used to identify it, and its molecular weight and molecular weight distribution were determined by gel permeation chromatography. The desorption behavior of the immobilized nylon implies that the principal interaction in the immobilization of nylon on silica may be hydrogen bonding between the terminal amine groups of nylon and the surface silanol groups. The immobilization was investigated by thermogravimetric analysis and transmission electron microscopy. Characterization of monolayers of nylon attached to glass plate surfaces was also carried out by atomic force microscopy (AFM) in contact mode. The AFM images of the nylon monolayers showed the formation of grafted polymer brushes or nanoclusters on the surfaces.Furthermore, the prepared surface of the silica gel was characterized by application in chromatographic analysis using the modified silica gel particles as a stationary phase. This stationary phase was stable and successfully employed for the separation of o-, m-, and p-nitroanisoles using cyclohexane or its mixture with dioxane as a mobile phase