硅胶及磁性石墨烯表面改性及分离富集性能

发布时间：2018-04-23 03:31

本文选题：原子转移自由基聚合 + 混合模式色谱　；参考：《西北大学》2017年硕士论文

【摘要】：基质的表面修饰对拓宽其应用范围发挥着重要的作用。传统的修饰方法主要是将小分子键合在基体表面,此方法因键合位点有限,官能团接枝率低,吸附剂吸附性能较差。本文选择硅胶及磁性石墨烯两种基质,通过ATRP聚合或以POSS为核枝状聚合的方法,在基质表面进行功能化修饰,提高了功能团接枝率,制备了两种分离及吸附性能较好的分离材料。主要内容有:(1)通过ATRP方法将甲基丙烯酸缩水甘油酯(GMA)和甲基丙烯酸二甲氨乙酯(DMAEMA)键合在硅胶表面,制备出一种亲水/阴离子交换混合模式色谱固定相。通过改变聚合过程单体的使用比例,控制单体的接枝量,制备了三种固定相。通过流动相中水含量,盐浓度及pH值的变化验证固定相与溶质之间的亲水及离子交换相互作用。用不同种类溶质,特别是酸性和碱性化合物研究了三种固定相的色谱特性。结果表明,本文使用的合成方法,可以合成不同种类的色谱固定相,满足复杂样品调控选择性的分离要求。最后将色谱固定相成功应用于分离牛奶中的三聚氰胺。(2)以磁性石墨烯为基质,多面体齐聚倍半硅氧烷(polyhedral oligomeric silsesquioxanes,POSS)为配体,制备出一种吸附容量高的硼酸亲和吸附剂Fe3O4@GO@PDA@POSS@FPBA。采用红外光谱(FTIR),扫描电镜(SEM)及超导量子干涉磁测量仪(SQUID)对其表征。对萃取条件,包括吸附时间,pH值,洗脱溶剂进行了优化。其对邻苯二酚,异丙肾上腺素及沙丁胺醇的最大吸附量分别为353,514,139 μmol/g,对顺式二羟基化合物呈现出较好的吸附特性。
[Abstract]:The surface modification of matrix plays an important role in broadening its application range. The traditional modification method is to bond small molecules on the surface of the matrix. Because of the limited bonding sites, the grafting rate of functional groups is low, and the adsorption performance of adsorbent is poor. In this paper, silica gel and magnetic graphene were selected to modify the surface of the matrix by ATRP polymerization or dendritic polymerization with POSS as the core. The grafting rate of functional groups was improved. Two kinds of separation materials with good separation and adsorption properties were prepared. A hydrophilic / anion exchange chromatographic stationary phase was prepared by bonding glycidyl methacrylate (GMA) and dimethylaminoethyl methacrylate (DMAEMA) onto the silica gel surface by ATRP. Three kinds of stationary phases were prepared by changing the proportion of monomer used in the polymerization process and controlling the amount of monomer graft. The hydrophilic and ion exchange interactions between the stationary phase and the solute were verified by the changes of water content, salt concentration and pH value in the mobile phase. The chromatographic characteristics of three stationary phases were studied with different solutes, especially acidic and alkaline compounds. The results show that the synthetic method can synthesize different chromatographic stationary phases and meet the separation requirements of complex samples. Finally, the chromatographic stationary phase was successfully applied to the separation of melamine from milk.) using magnetic graphene as the matrix and polyhedral oligomeric silsesquioxanes-POSS) as the ligand, a boric acid affinity adsorbent Fe3O4, GOPDAPPOSSSFS FPBAwith high adsorption capacity, was prepared by using polyhedral oligomeric silsesquioxane and polyhedral oligosilane polysiloxane as ligand. It was characterized by FTIR, SEM (SEM) and squid (superconducting quantum interferometer). The extraction conditions, including adsorption time and pH value, and elution solvent were optimized. The maximum adsorption capacity of catechol, isoproterenol and salbutamol was 353514139 渭 mol / g, respectively.
【学位授予单位】：西北大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O652.6;TQ424

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