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

为研究以反胶束固定为微反应器制备接枝聚酰胺电刷表面改性的可行性，以十六烷基三甲基氯化铵（CTAC）反胶束吸附于二氧化硅表面合成尼龙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)在反胶束界面处原位聚合1,6-己二胺和二氯己二酰；(3)去除CTAC或反胶束等残留成分。考察了反胶束对1,6-己二胺在硅胶上的吸附行为。用1,1,1,3,3,3-六氟-2-丙醇从硅胶中回收所得尼龙，用红外光谱对其进行鉴定，并用凝胶渗透色谱法测定其分子量和分子量分布。固定化尼龙的解吸行为表明，尼龙在二氧化硅上固定化的主要相互作用可能是尼龙末端胺基与表面硅醇基之间的氢键作用。用热重分析和透射电镜研究了固定化效果。在接触模式下，利用原子力显微镜（AFM）对附着在玻璃板表面的尼龙单层进行了表征。尼龙单层的AFM图像显示在表面形成接枝聚合物刷或纳米团簇。此外，将改性后的硅胶颗粒作为固定相，对制备的硅胶表面进行了表征，并应用于色谱分析。该固定相稳定，以环己烷或其与二恶烷的混合物为流动相，成功地分离了邻硝基、间硝基和对硝基苯胺

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