PGMA-DVB聚合物微球的制备、改性及其在高效液相色谱中的应用

发布时间：2018-04-03 22:19

本文选题：种子乳液聚合　切入点：聚合物微球　出处：《青岛大学》2017年硕士论文

【摘要】：聚合物微球作为最常见的聚合物形貌之一,广泛应用在色谱分离、药物输送、光子晶体等多个领域。目前聚合物微球的制备方法复杂多样,种子乳液聚合由于易于控制,所制备的聚合物微球粒径均一,形貌多样,成为过去几十年间聚合物微球制备方法的研究热点之一。本研究通过种子乳液聚合制备出了粒径均一的聚合物微球,研究了不同类型的溶胀剂对聚合物微球形貌的影响,并将其用作色谱分离材料。本研究包括以下两方面内容:1.通过种子乳液聚合法成功制备平均粒径为4.6微米的多孔聚(甲基丙烯酸缩水甘油酯-二乙烯基)(PGMA-DVB)微球,利用重氮树脂(DR)进行改性。选取三种溶剂(甲苯、环己醇和十二烷醇)为致孔剂制备不同形态的多孔微球。发现由甲苯作为致孔剂所制备的聚合物微球比表面积大,孔结构良好,因此用于下一步改性。通过环氧基团的水解得到表面羟基化的聚合物微球,利用羟基与DR的氢键自组装,在紫外辐照下,成功将DR键合于PGMA-DVB微球上,并将所得多孔PGMA-DVB-DR微球作为高效液相色谱(HPLC)的固定相。该固定相可以用于混合模式分离机制,包括反相(RP)和亲水相互作用。研究发现该固定相可实现苯同系物的基线分离。另外,可以将副产物乙酸从乙烯基三氮唑反应产物中快速分离出来。并且由于仲氨基的存在,该微球有望成为有机酸分离的色谱填料。2.首次将表面活性剂Span 80作为溶胀剂引入到种子乳液聚合当中。利用Span 80的吸水性,调节其在聚合体系中的加入量,成功制备出了粒径均一且具有微孔、中空、大孔结构的PGMA-DVB聚合物微球并提出各类型微球形成的机理,为微孔、中空、大孔结构的聚合物微球制备提供了一种新方法。
[Abstract]:As one of the most common polymer morphologies, polymer microspheres are widely used in chromatographic separation, drug delivery, photonic crystal and other fields.At present, the preparation methods of polymer microspheres are complex and diverse. Because of the easy control of seed emulsion polymerization, the size of polymer microspheres is uniform and the morphology is diverse, which has become one of the research hotspots in the preparation of polymer microspheres in the past few decades.In this study, homogeneous polymer microspheres were prepared by seed emulsion polymerization. The effects of different swelling agents on the morphology of polymer microspheres were studied and used as chromatographic separation materials.This research includes the following two aspects: 1.The porous poly (glycidyl methacrylate divinylidene) PGMA-DVB microspheres with average diameter of 4.6 渭 m were prepared by seed emulsion polymerization and modified with diazo resin (DRN).Three solvents (toluene, cyclohexanol and dodecanol) were used to prepare porous microspheres with different morphology.It was found that the polymer microspheres prepared by toluene as pore-forming agent had large specific surface area and good pore structure, so they were used for further modification.The surface hydroxylated polymer microspheres were prepared by hydrolysis of epoxy group. The hydroxyl group and Dr were self-assembled by hydrogen bonding. Dr was successfully bonded to PGMA-DVB microspheres under ultraviolet irradiation.The porous PGMA-DVB-DR microspheres were used as the stationary phase of high performance liquid chromatography (HPLC).The stationary phase can be used for mixing mode separation mechanism, including reverse phase RP and hydrophilic interaction.It is found that the stationary phase can achieve the baseline separation of benzene homologues.In addition, the by-product acetic acid can be quickly separated from the product of vinyl triazole reaction.Due to the presence of secondary amino groups, the microspheres are expected to be used as chromatographic fillers for the separation of organic acids.The surfactant Span 80 was introduced into seed emulsion polymerization as swelling agent for the first time.The preparation of macroporous polymer microspheres provides a new method.
【学位授予单位】：青岛大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：TQ317;O652.63

【参考文献】