【摘要】：與普通聚合物微球相比,聚合物多孔微球在多孔結(jié)構(gòu)、高交聯(lián)度和機(jī)械性能穩(wěn)定等方面具有優(yōu)勢。多孔的結(jié)構(gòu)導(dǎo)致其比表面積大,滲透壓相比之下要小很多,而高交聯(lián)度可以使其具有穩(wěn)定的機(jī)械性能,所以其在色譜等方面有很廣泛的應(yīng)用。色譜柱作為液相色譜的關(guān)鍵部件,其性能很大程度上取決于色譜柱填料的性能,而對于多孔微球進(jìn)行改性,從而提高其色譜分離性能受到越來越多科研工作者的關(guān)注。本論文基于兩步溶脹法合成聚合物多孔微球在單分散性等方面的優(yōu)勢,為實(shí)現(xiàn)多孔微球的精準(zhǔn)可控合成,分別對影響聚合物多孔微球的因素進(jìn)行了考察,并將其進(jìn)行改性,考察了其在色譜方面的性能。具體工作如下:1.采用兩步種子溶脹聚合法,成功合成了單分散性良好的聚苯乙烯多孔微球,微球粒徑為5μm。為實(shí)現(xiàn)多孔微球的準(zhǔn)確可控性合成對多孔聚合物微球表面形態(tài)的影響因素包括致孔劑比例、溶脹溫度和交聯(lián)劑種類進(jìn)行了考察。當(dāng)致孔劑鄰苯二甲酸二丁酯(DBP)與甲苯的比例為1:3時得到的聚苯乙烯多孔微球比表面積最大,溶脹溫度為25℃時表面最粗糙,使用乙二醇二甲基丙烯酸酯(EDMA)做交聯(lián)劑時得到的多孔微球的結(jié)構(gòu)比較疏松。對各類微球的比表面積進(jìn)行了比較,得到的結(jié)果為比表面積最大的是P(S-DVB)-4,其值為562 m~2/g。2.對聚合物多孔微球進(jìn)行了重氮樹脂改性,并以改性后的微球?yàn)樯V柱填料進(jìn)行了幾種色譜分離實(shí)驗(yàn)。利用光交聯(lián)的反應(yīng)原理,用水溶性的感光高分子重氮樹脂實(shí)現(xiàn)了對聚合物微球的功能化改性。首先將微球磺酸化,然后將重氮樹脂和磺酸基進(jìn)行接枝,最后用紫外燈對其進(jìn)行照射,將靜電相互作用轉(zhuǎn)化為共價(jià)相互作用。提高了固定相的極性,不僅保留并增強(qiáng)了對于非極性物質(zhì)的性能,還實(shí)現(xiàn)了對極性物質(zhì)的分離性能。本論文進(jìn)行的多孔聚苯乙烯多孔微球的合成考察了各種因素對聚合物多孔微球表面形態(tài)的影響,對實(shí)現(xiàn)孔徑分布和比表面積的可控具有一定的意義。多孔微球隨后的改性綜合了物理吸附和化學(xué)鍵合方法的諸多優(yōu)點(diǎn),通過光照交聯(lián)即可實(shí)現(xiàn)對聚合物微球簡單快捷的功能化改性,是一種高效,穩(wěn)定,綠色環(huán)保的改性方法。對非極性物質(zhì)和極性物質(zhì)都實(shí)現(xiàn)了良好的分離性能。
[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，

本文編號：2265742