炔基修饰Fe_3O_4磁纳米粒子的合成及其“click”环加成反应  

Synthesis of alkyne-modified Fe_3O_4 magnetic nanoparticles and its “click” cycloaddition reaction

作　　者：刘静培[1,2] 李潇[2] 张岚[2] 周伟[2] 钟国清[1] 刘彦伯 王妮[2] 沈华[2] 张国欣[2] 

机构地区：[1]西南科技大学材料科学与工程学院,绵阳621010 [2]中国科学院上海应用物理研究所放射性药物研究中心,上海市201800 [3]上海市纳米科技与产业发展促进中心,上海市200237

出　　处：《四川大学学报（自然科学版）》2011年第5期1137-1142,共6页Journal of Sichuan University(Natural Science Edition)

基　　金：国家自然科学基金(10875163;10805069)

摘　　要：Fe_3O_4磁纳米粒子的炔基修饰包括:纳米磁性Fe_3O_4粒子的制备,硅胶包覆Fe_3O_4磁粒子,氨基修饰硅胶包覆的磁粒子,炔基修饰氨基修饰后的磁粒子.并采用苄基叠氮与所制备的炔基修饰磁Fe_3O_4纳米粒子进行click环加成反应.通过SEM、BET、XRD和VSM分别对Fe_3O_4和硅胶包覆Fe_3O_4的表面形貌、比表面积、晶型结构和磁性能进行表征;利用UV-Vis对磁性Fe_3O_4粒子表面的炔基进行半定量分析;采用FTIR对产物表面基团做定性分析.结果表明,Fe_3O_4磁纳米粒子平均粒径为180±20 nm,粒子呈球形且粒径分布范围窄,比表面积较大为114.954 m^2/g,其饱和磁化强度为70.347 emu/g;硅胶包覆后,球形表面相对较为光滑,饱和磁化强度有所降低.炔基修饰Fe_3O_4磁纳米粒子表面的1,2,3-三唑基团对应的红外吸收峰位于1560 cm^(-1),炔基量约为0.25×10^(-6)mol/mg.Fe3O4 Magnetic nanoparticles （MNPs） modified by alkyne were prepared by four successive reactions, which were MNPs preparation, silica-coating, surface modification with amino group and alkyne modification. Benzyl azide was selected and coupled with as-prepared alkyne modified MNPs via ＂click＂ reaction. The morphologies, specific surface area, crystal structures and magnetic strengths of MNPs and silica-cocoted modified MNPs were characterized by SEM, BET, XRD and VSM. Ultraviolet visible absorption spectrum could indirectly illustrate the semi-quantity for alkyne group on the MNPs＇ surface. Bonds on the surface of products synthesized by ＂click＂ reaction were determined by FTIR. The results showed that the MNPs prepared were well dispersed with size of 180-t-20 nm, specific surface area （BET） of 114. 954 m2/g and saturation magnetization （Ms） of 70. 347 emu/g, corre- spondingly, while the silica-MNPs showed larger smooth surfaces but lower Ms. The FTIR absorption band of 1,2,3-triazole on the surface of as-prepared spherical alkyne modified MNPs appeared around 1560 cm-1. The alkyne group （--C≡C） on the MNPs＇ surface was 0.25 × 10^-6 mol/rag -solid.

关 键 词：炔基修饰 磁性纳米粒子 CLICK反应 表面修饰 硅胶包覆 

分 类 号：O614[理学—无机化学]