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

为了研究利用固定化反胶团作为微反应器制备接枝聚酰胺刷的可行性，以十六烷基三甲基氯化铵（CTAC）为反胶团吸附于二氧化硅表面，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反胶团吸附到硅胶表面上，（2）在反胶团界面上原位聚合1，6-己二胺和己二酰氯，（3）除去残余组分如CTAC或反胶团。研究了反胶束体系对1，6-己二胺在硅胶上的吸附行为。在使用1，1，1，3，3，3-六氟-2-丙醇从硅胶中回收所生产的尼龙之后，使用红外光谱对其进行鉴定，并且通过凝胶渗透色谱法测定其分子量和分子量分布。固定化尼龙的脱附行为表明，尼龙在二氧化硅上的固定化的主要相互作用可能是尼龙的末端胺基与表面硅烷醇基团之间的氢键。通过热重分析和透射电镜对固定化进行了研究。附着在玻璃板表面的尼龙单层的表征也进行了原子力显微镜（AFM）的接触模式。AFM图像显示尼龙单分子膜表面形成了接枝聚合物刷或纳米团簇，并将改性后的硅胶颗粒作为固定相应用于色谱分析。该固定相稳定性好，可用于邻、间、对硝基苯甲醚的分离，并可用于环己烷或环己烷与二氧六环的混合物作为移动的流动相

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