磁性介孔固相萃取剂的快速合成及其萃取性能研究

This project focuses on the facile synthesis of functionalized magnetic mesoporous silica or magnetic mesoporous carbon material and their extraction performance toward trace pollutants in environmental water samples. Functionalized mesoporous silica particles will be prepared through one-pot method in which the synthesis of magnetic particles, coating of mesoporous silica and modification are combined together in one vessel. On the basis of that, magnetic mesoporous carbon material can be obtained by adding proper carbon source (block copolymer or nonionic surfactant) followed by carbonization at high temperature and removing the hard template (silica) with alkali or hydrofluoric acid, rather than removing the surfactant as soft template directly. The extraction performance of the prepared magnetic mesoporous materials to the common organic pollutants in water samples will be investigated and an efficient and convenient method of extraction and determination of these pollutants in water samples will be established. The strategy studied in this project can greatly simplify the synthesis procedure of the extractants. Large scale of the extractants can be prepared facilely and the cost of synthesis and usage are saved. The extractants prepared in this project possess large surface area and high adsorption ability and can be easily isolated from water solution due to the superparamagnetic property. These endue the extractants with broad application prospects in the extraction and determination of trace pollutants from environmental water samples. Therefore, this project is an original research with important academic and application value.

项目旨在研究功能化磁性介孔硅胶或磁性介孔碳固相萃取吸附剂的快速合成方法，并研究其对环境样品中痕量有机污染物的萃取性能。采用"一锅法"将磁性纳米颗粒的制备、介孔硅胶包覆和功能化修饰在同一容器中一次完成，合成功能化的磁性介孔硅胶颗粒。在此基础上，如果添加合适的碳源（嵌段聚合物或非离子型表面活性剂），硅胶包覆后直接将其在高温下碳化，再利用碱溶（或酸溶）法将硅胶作为硬模板除去，即可得到磁性介孔碳材料。考察制备的磁性介孔材料对常见有机污染物的萃取性能，建立环境样品中痕量污染物的高效、快速萃取测定方法。本项目所研究的合成方法可大大简化萃取剂的合成步骤，快速、大批量合成磁性介孔萃取剂，降低制备和使用成本。合成的萃取剂具有极大的比表面积和强吸附能力，又具有超顺磁性，可方便地进行磁性固-液分离，使其在环境样品中污染物的萃取测定方面有广阔的应用前景。该项目是一项具有重要学术和应用价值的原创性研究。

由于具有独特的超顺磁性和优良的吸附性能，磁性纳米材料在环境样品中痕量目标物的吸附中有良好的应用前景，而如何在保证具有较强吸附能力的同时，简化材料的制备过程，降低合成成本，是这类吸附剂能够迅速普及推广的关键。针对这个问题，项目主要进行了三方面的研究。首先，利用“一锅法”，合成了对亚甲基蓝染料具有较强吸附性能的核壳式磁性介孔硅胶吸附剂，相比常规的“分步法”，大大简化了合成步骤；然后，以海藻酸钙聚合物为碳源，高温碳化后，合成了对溴百里香酚兰染料具有较强吸附能力的磁性多孔碳复合物，与常用的酚醛树脂聚合物相比，即节省了制备时间，又降低了合成条件要求；最后，通过将包覆于Fe3O4/SiO2磁性纳米颗粒表面的多酚-金属螯合聚合物碳化，并将中间的硅胶层去除，得到了铃铛型Fe3O4/空腔/C 磁性多孔碳吸附剂，提升了该吸附剂对有机染料的吸附性能。以此为基础，参与编写并出版了2部环境样品前处理方面的学术专著，还有一部正待出版。