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采用层层自组装的方法,以微米多孔硅胶小球为核,将硅胶纳米粒子多层包覆,制备了核壳型SiO2/SiO2硅胶小球。透射电子显微镜表明这种硅胶小球具有明显的核壳结构,氮气吸附实验证明该硅胶小球是典型的介孔材料,具有良好的介孔结构和窄的孔径分布。将其作为基质制备碳十八键合核壳型SiO2/SiO2色谱固定相,该固定相的碳含量与未组装硅球制备的碳十八键合固定相相比有显著提高。对其渗透性考察表明,渗透性较未组装硅胶小球制备的碳十八键合固定相有明显提高。利用8种芳香类化合物对该新型固定相进行色谱性能评价,结果表明,这种核壳型SiO2/SiO2固定相对芳香性化合物的分离选择性有明显改善,并有很好的峰对称性,是一类具有良好发展潜力的固定相。
The core-shell type SiO2 / SiO2 silica gel beads were prepared by multilayer self-assembly method. The micro-porous silica beads were used as the core, and the silica gel nano-particles were multilayered. Transmission electron microscopy showed that the silica gel beads have obvious core-shell structure. The nitrogen adsorption experiments show that the silica beads are typical mesoporous materials with good mesoporous structure and narrow pore size distribution. As a matrix, carbon-18-bonded core-shell SiO2 / SiO2 chromatographic stationary phase was prepared. The carbon content of the stationary phase was significantly higher than that of the carbon-18-bonded stationary phase prepared without silica sphere. The permeability of the test showed that permeability than the uncoated silica gel prepared carbon octadecane bonded phase was significantly improved. The chromatographic performance of the novel stationary phase was evaluated by eight kinds of aromatic compounds. The results showed that the selectivity of the core-shell SiO2 / SiO2 stationary phase to the aromatic compound was obviously improved and the peak symmetry was good. A class of stationary phases with good potential for development.