Key Laboratory of Functional Molecule Design and Interface Process, School of Materials Science and Chemical Engineering, Anhui Jianzhu University, Hefei, 230601, China.
Anhui Provincial Key Laboratory of Environmental Pollution Control and Resource Reuse, School of Environment and Energy Engineering, Anhui Jianzhu University, Hefei, 230601, China.
Mikrochim Acta. 2020 May 14;187(6):328. doi: 10.1007/s00604-020-04268-w.
Based on a detailed study of the hydrolysis process of tetrabutyl orthotitanate (TBOT), TiO nanoclusters were modified inside the pores of SiO core-shell particles instead of the outside. The pore size distribution of SiO core-shell spheres modified with TiO (SiO@dSiO@TiO) was analyzed by Barrett-Joyner-Halenda (BJH) method and density functional theory (DFT) method, respectively. The results of the DFT calculations demonstrate that the TiO nanoclusters are always first formed in bulk solution and then enter the pores. By regulating the rate of hydrolysis of TBOT, almost all of the TiO nanoclusters are modified into the pores and the structure of the original SiO core-shell sphere is hardly affected. The morphology of the particles was characterized by scanning electron microscopy and transmission electron microscopy. The crystal phase of TiO was measured by XRD. SiO@dSiO@TiO spheres functionalized with C18 were packed into a stainless steel column. The chemical stability of SiO@dSiO@TiO spheres under alkaline was tested by flushing of a mobile phase at pH 13 for 7 days. The efficiency of the column after the alkali solution treatment still reaches 98,430 plates m, which is only about 1.6% lower than that before the alkali solution treatment. A series of basic and acidic analytes were also separated on the column. Graphical abstract TiO nanocrystals were coated into the pore of core-shell silica spheres. The prepared particles were packed into the column and separation performance up to 98,430 plates per meter was achieved.
通过对四丁基钛酸酯（TBOT）水解过程的详细研究，将 TiO 纳米簇修饰在 SiO 核壳粒子的孔内，而不是孔外。采用 Barrett-Joyner-Halenda（BJH）法和密度泛函理论（DFT）法分别分析了 TiO 修饰的 SiO 核壳球的孔径分布。DFT 计算结果表明，TiO 纳米簇总是先在本体溶液中形成，然后进入孔内。通过调节 TBOT 的水解速率，可以将几乎所有的 TiO 纳米簇都修饰到孔内，而原始 SiO 核壳球的结构几乎不受影响。通过扫描电子显微镜和透射电子显微镜对颗粒的形貌进行了表征。通过 XRD 测量了 TiO 的晶体相。用 C18 功能化的 SiO@dSiO@TiO 球填充到不锈钢柱中。通过在 pH 13 的流动相冲洗 7 天，测试了 SiO@dSiO@TiO 球在碱性条件下的化学稳定性。碱溶液处理后的柱效仍达到 98430 板 m，仅比碱溶液处理前低约 1.6%。还在该柱上分离了一系列碱性和酸性分析物。
