球形介孔二氧化硅微球的制备及其在高效液相色谱中的应用

发布时间：2018-06-22 18:35

  本文选题：单分散 + 二氧化硅微球　； 参考：《华东理工大学》2017年硕士论文

【摘要】：随着高效液相色谱(HPLC)在化工、医药、环境等领域的广泛应用,人们对HPLC提出了更高的要求,色谱填料作为HPLC的核心,是色谱研究中最为关键的部分。单分散介孔硅胶微球依然是应用最为广泛的高效液相色谱基质材料。为了提高色谱柱的分离效率,选择性和稳定性,小颗粒硅胶和杂化硅胶等新型材料成为液相色谱填料新的发展方向。本论文研究了新型的亚2 μm小颗粒介孔二氧化硅微球和有机-无机杂化介孔硅胶微球的合成方法及其在高效液相色谱中的应用。在溶胶-凝胶法的基础上,采用非离子表面活性剂十二胺为模板剂,十二胺聚氧乙烯醚为扩孔剂,制备了亚2 μm单分散介孔二氧化硅微球,用十八烷基二甲基氯硅烷键合后作为反相色谱固定相,应用于超高效液相色谱(UPLC)。详细考察了溶胶-凝胶过程中,醇水比例和反应温度对硅胶微球形貌的影响,老化温度和时间等因素对孔径的影响。其中,通过控制甲醇和水的比例在2.4:1到4:1的范围内,可以得到粒径为0.4～2 μm单分散二氧化硅微球;通过调节老化温度和时间,可在4.4～11.6 nm范围内调节孔径的大小,对制备的反相C18柱进行了动力学和反相保留行为的评价。参照单分散介孔二氧化硅微球合成的实验条件,以乙烯基三甲氧基硅烷和正硅酸乙酯为混合硅源,通过共缩聚法制备了乙烯基有机-无机杂化介孔硅胶微球,研究了硅源比例TEOS/VTMS对杂化硅胶形貌和孔径的影响。在水热后处理的过程中,以AC1210为扩孔剂的基础上,并加入一定浓度的氟化铵来进一步扩大孔径。最终采用TEOS/VTMS为5:1的硅源比例合成乙烯基杂化材料,将制备的2.3 μm杂化硅胶微球在100℃下老化12小时,得到了比表面积351 m2/g,孔径7.2 nm的乙烯基有机-无机杂化介孔硅胶微球。通过巯基-烯点击化学反应在硅胶表面引入半胱氨酸,制备了亲水色谱固定相,并对色谱柱在亲水模式下对极性化合的保留行为进行了研究。
[Abstract]:With the wide application of high performance liquid chromatography (HPLC) in the fields of chemical industry, medicine, environment and so on, people put forward higher requirements for HPLC. As the core of HPLC, chromatographic packing is the most important part of chromatographic research. Monodisperse mesoporous silica gel microspheres are still the most widely used matrix materials for high performance liquid chromatography (HPLC). In order to improve the separation efficiency, selectivity and stability of chromatographic column, new materials, such as small particle silica gel and hybrid silica gel, have become the new development direction of liquid chromatographic packing. In this paper, a new type of mesoporous silica microspheres with sub2 渭 m particles and organic-inorganic hybrid mesoporous silica microspheres were synthesized and their applications in high performance liquid chromatography (HPLC) were studied. Based on the sol-gel method, the monodisperse mesoporous silica microspheres of 2 渭 m were prepared by using dodecylamine as template and dodecylamine polyoxyethylene ether as pore expander. Octadecyl dimethyl chlorosilane was used as a stationary phase in reversed phase chromatography and applied to ultra-high performance liquid chromatography (UPLC). The effects of alcohol-water ratio and reaction temperature on the morphology of silica gel microspheres, aging temperature and time on the pore size were investigated in detail. By controlling the ratio of methanol to water in the range of 2.4: 1 to 4:1, the monodisperse silica microspheres with a particle size of 0.4 渭 m can be obtained, and the pore size can be adjusted in the range of 4.4 渭 m 11.6 nm by adjusting the aging temperature and time. The kinetics and retention behavior of the prepared reversed C 18 column were evaluated. According to the experimental conditions for the synthesis of monodisperse mesoporous silica microspheres, vinyl trimethoxysilane and ethyl orthosilicate were used as the mixed silica source to prepare vinyl organic-inorganic hybrid mesoporous silica microspheres by co-condensation. The effect of silicon source ratio TEOS / VTMS on the morphology and pore size of hybrid silica gel was studied. In the process of hydrothermal treatment, the pore size was further expanded by adding a certain concentration of ammonium fluoride on the basis of AC1210 as the pore expander. Finally, the vinyl hybrid material was synthesized by using the ratio of TEOS / VTMS at 5:1. The prepared 2.3 渭 m hybrid silica gel microspheres were aged at 100 鈩，

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