Liu Xianbin, Li Laisheng, Du Yu, Guo Zhen, Ong Teng Teng, Chen Yuan, Ng Siu Choon, Yang Yanhui
School of Chemical and Biomedical Engineering, Nanyang Technological University, Singapore 637459, Singapore.
J Chromatogr A. 2009 Nov 6;1216(45):7767-73. doi: 10.1016/j.chroma.2009.09.013. Epub 2009 Sep 10.
A modified synthesis approach for spherical large pore-diameter SBA-15 mesoporous silica (SLP-SBA-15) with particle size range of 0.5-1microm was being reported. It was worth mentioning that in this improved methodology, the use of cetyltrimethylammonium bromide (CTAB) as co-template significantly reduced the self-assembly time from 24h to 45min. Moreover, under reflux condition, the reaction time could be further shortened by reducing the aging time from 48h to 6h. The resultant SLP-SBA-15 was thereafter successfully functionalized and packed into an ultra-high-performance liquid chromatography (UHPLC) column for the separation of aromatic compounds. A variety of characterizations demonstrated that the silica products exhibited a well-ordered 2d hexagonal mesostructure with well-formed spherical morphology. pore-diameter can be enlarged up to 8.2nm without affecting the structural order. The SLP-SBA-15 samples showed excellent thermal and hydrothermal stabilities. The octadecyltriethoxysilane functionalized SLP-SBA-15 (SLP-C18-SBA-15) was demonstrated to be an effective stationary phase in UHPLC application because the column exhibited significantly reduced column pressure (2800psi) at a flow rate of 0.4ml/min. Accordingly, it would afford greater flexibility for tuning of the flow rate to meet the fast separation requirement.
报道了一种用于合成粒径范围为0.5 - 1微米的球形大孔径SBA - 15介孔二氧化硅(SLP - SBA - 15)的改进方法。值得一提的是,在这种改进方法中,使用十六烷基三甲基溴化铵(CTAB)作为共模板可将自组装时间从24小时显著缩短至45分钟。此外,在回流条件下,通过将老化时间从48小时减少到6小时,反应时间可进一步缩短。随后,将所得的SLP - SBA - 15成功功能化并填充到超高效液相色谱(UHPLC)柱中用于分离芳香族化合物。各种表征表明,二氧化硅产物呈现出具有良好球形形态的有序二维六方介观结构。孔径可扩大至8.2纳米而不影响结构有序性。SLP - SBA - 15样品表现出优异的热稳定性和水热稳定性。十八烷基三乙氧基硅烷功能化的SLP - SBA - 15(SLP - C18 - SBA - 15)在UHPLC应用中被证明是一种有效的固定相,因为该柱在流速为0.4毫升/分钟时柱压显著降低(2800psi)。因此,它将为调节流速以满足快速分离要求提供更大的灵活性。