聚苯乙烯多孔微球的制备、改性及在混合模式液相色谱中的应用
发布时间：2018-10-12 10:14
【摘要】：与普通聚合物微球相比,聚合物多孔微球在多孔结构、高交联度和机械性能稳定等方面具有优势。多孔的结构导致其比表面积大,渗透压相比之下要小很多,而高交联度可以使其具有稳定的机械性能,所以其在色谱等方面有很广泛的应用。色谱柱作为液相色谱的关键部件,其性能很大程度上取决于色谱柱填料的性能,而对于多孔微球进行改性,从而提高其色谱分离性能受到越来越多科研工作者的关注。本论文基于两步溶胀法合成聚合物多孔微球在单分散性等方面的优势,为实现多孔微球的精准可控合成,分别对影响聚合物多孔微球的因素进行了考察,并将其进行改性,考察了其在色谱方面的性能。具体工作如下:1.采用两步种子溶胀聚合法,成功合成了单分散性良好的聚苯乙烯多孔微球,微球粒径为5μm。为实现多孔微球的准确可控性合成对多孔聚合物微球表面形态的影响因素包括致孔剂比例、溶胀温度和交联剂种类进行了考察。当致孔剂邻苯二甲酸二丁酯(DBP)与甲苯的比例为1:3时得到的聚苯乙烯多孔微球比表面积最大,溶胀温度为25℃时表面最粗糙,使用乙二醇二甲基丙烯酸酯(EDMA)做交联剂时得到的多孔微球的结构比较疏松。对各类微球的比表面积进行了比较,得到的结果为比表面积最大的是P(S-DVB)-4,其值为562 m~2/g。2.对聚合物多孔微球进行了重氮树脂改性,并以改性后的微球为色谱柱填料进行了几种色谱分离实验。利用光交联的反应原理,用水溶性的感光高分子重氮树脂实现了对聚合物微球的功能化改性。首先将微球磺酸化,然后将重氮树脂和磺酸基进行接枝,最后用紫外灯对其进行照射,将静电相互作用转化为共价相互作用。提高了固定相的极性,不仅保留并增强了对于非极性物质的性能,还实现了对极性物质的分离性能。本论文进行的多孔聚苯乙烯多孔微球的合成考察了各种因素对聚合物多孔微球表面形态的影响,对实现孔径分布和比表面积的可控具有一定的意义。多孔微球随后的改性综合了物理吸附和化学键合方法的诸多优点,通过光照交联即可实现对聚合物微球简单快捷的功能化改性,是一种高效,稳定,绿色环保的改性方法。对非极性物质和极性物质都实现了良好的分离性能。
[Abstract]:Compared with conventional polymer microspheres, polymer porous microspheres have advantages in porous structure, high crosslinking degree and stable mechanical properties. The porous structure leads to large specific surface area, much smaller osmotic pressure, and high crosslinking degree can make it have stable mechanical properties, so it is widely used in chromatography and other fields. As a key component of liquid chromatography, the performance of chromatographic column depends largely on the performance of column fillers, and the porous microspheres are modified to improve their chromatographic separation performance. In this paper, based on the advantages of two-step swelling synthesis of polymer porous microspheres in monodispersity, in order to achieve the precise and controllable synthesis of porous microspheres, the factors affecting polymer porous microspheres were investigated and modified. Its performance in chromatography was investigated. The specific work is as follows: 1. The porous polystyrene microspheres with good monodispersity were successfully synthesized by two-step seed swelling polymerization. The size of the microspheres was 5 渭 m. In order to realize the accurate controllable synthesis of porous microspheres, the factors affecting the surface morphology of porous polymer microspheres, including the proportion of pore-forming agents, swelling temperature and kinds of crosslinking agents, were investigated. When the ratio of dibutyl phthalate (DBP) and toluene is 1:3, the porous polystyrene microspheres have the largest specific surface area and the roughest surface when the swelling temperature is 25 鈩，
本文编号：2265742
[Abstract]:Compared with conventional polymer microspheres, polymer porous microspheres have advantages in porous structure, high crosslinking degree and stable mechanical properties. The porous structure leads to large specific surface area, much smaller osmotic pressure, and high crosslinking degree can make it have stable mechanical properties, so it is widely used in chromatography and other fields. As a key component of liquid chromatography, the performance of chromatographic column depends largely on the performance of column fillers, and the porous microspheres are modified to improve their chromatographic separation performance. In this paper, based on the advantages of two-step swelling synthesis of polymer porous microspheres in monodispersity, in order to achieve the precise and controllable synthesis of porous microspheres, the factors affecting polymer porous microspheres were investigated and modified. Its performance in chromatography was investigated. The specific work is as follows: 1. The porous polystyrene microspheres with good monodispersity were successfully synthesized by two-step seed swelling polymerization. The size of the microspheres was 5 渭 m. In order to realize the accurate controllable synthesis of porous microspheres, the factors affecting the surface morphology of porous polymer microspheres, including the proportion of pore-forming agents, swelling temperature and kinds of crosslinking agents, were investigated. When the ratio of dibutyl phthalate (DBP) and toluene is 1:3, the porous polystyrene microspheres have the largest specific surface area and the roughest surface when the swelling temperature is 25 鈩，
本文编号：2265742
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