CN102924977A - 一种磁性Fe3O4 纳米粒子表面改性的方法 - Google Patents
一种磁性Fe3O4 纳米粒子表面改性的方法 Download PDFInfo
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Abstract
本发明公开了一种磁性Fe3O4纳米粒子表面改性的方法,本方法采用各种烷基苯或氯甲基苯重氮盐通过重氮化反应改性磁性Fe3O4纳米粒子表面,使烷基苯与纳米磁性Fe3O4粒子间可产生共价键连接,而不是传统改性方法只能做到的改性试剂与Fe3O4粒子间仅产生物理吸附,本方法具有试剂与粒子间结合能力强,不易脱落的特点;本改性方法的另一特点是如选择带氯甲基官能基团的氯甲基苯基重氮盐除了可改性粒子表面性能,阻止粒子间团聚外,还具有多种后续反应功能,使这些连接在纳米磁性Fe3O4粒子表面的氯官能基团可作进一步的反应,如取代反应,聚合反应等,从而可赋予磁性Fe3O4纳米粒子更加广泛的应用价值。
Description
技术领域
本发明涉及一种磁性Fe3O4 纳米粒子表面改性的方法。
背景技术
纳米磁性粒子是一种新型的功能材料,在静态时无磁性吸引力,当外加磁场作用时,才表现出磁性,因此纳米磁性粒子有着广泛的理论和应用价值,其应用范围已涉及机械、工程、化工、医药等各个领域。纳米磁性粒子由于粒径小,易团聚,在使用前必须对其表面进行改性以避免磁性纳米粒子之间的相互凝聚及固定磁粒子。纳米磁性粒子表面改性的试剂种类较多,常用的有明胶、油酸、聚乙二醇(PEG)、聚乙烯醇(PVA)等。但这些试剂通常只是吸附在磁性粒子表面,充当表面活性剂的作用,而不能在磁性粒子表面作进一步的反应,即没有反应功能,再聚合功能等。
发明内容
本发明的目是提供一种磁性Fe3O4 纳米粒子表面改性的方法,本方法采用各种烷基苯或氯甲基苯重氮盐通过重氮化反应改性粒子表面,使烷基苯或氯甲基苯与纳米磁性Fe3O4粒子间可产生共价键连接,而不是传统改性方法只能做到的是改性试剂与Fe3O4粒子间仅产生物理吸附,因此本改性方法具有试剂与粒子间结合能力强,不易脱落的特点。本改性方法的另一特点是如选择带氯甲基官能基团的氯甲基苯基重氮盐除了可改性粒子表面性能,阻止粒子间团聚外,还具有多种后续反应功能,使这些连接在纳米磁性Fe3O4粒子表面的氯官能基团可作进一步的反应,如取代反应,聚合反应等,从而可赋予纳米磁性Fe3O4粒子更加广泛的应用价值。
本发明提供的一种磁性Fe3O4 纳米粒子表面改性的方法是:
在磁力搅拌下,按重量比1~1.3%的FeCl3,重量比0.5 ~0.7%的FeSO4, 重量比49~63%的去离子水,混合均匀,通氮,加入重量比30~36% 浓度 1M 的NaOH,加入后溶液变为深黑色,再加入重量比0.03~0.06%的重氮盐,反应温度室温,磁力搅拌1 小时,反应气氛N2,在此条件下得到表面改性的磁性Fe3O4纳米粒子 ,其粒径介于6~10nm。
所述重氮盐是烷基苯重氮盐或氯甲基苯重氮盐。
所述的烷基苯重氮盐是甲苯基重氮盐或乙苯基重氮盐。
所述反应完成后用无水乙醇洗涤,离心分离,干燥,得到表面改性的磁性Fe3O4纳米粒子。此粒子可在pH值为8的水溶液中稳定。
本发明的有益效果:
本发明提出的改性纳米磁性Fe3O4粒子的方法具有改性效果好,纳米粒子粒径小,可在pH值为8的水溶液中稳定,且改性试剂可与粒子间共价连接,改性表面结合强度高,如果选择带官能基团的重氮盐(如氯甲基苯基重氮盐)还可使粒子表面作进一步反应,具有更广泛的应用价值。本方法同时还具有反应简单,操作方便等特点。
具体实施方式
实施例1
在磁力搅拌下,在烧瓶中加入按重量比(下同)1%FeCl3,0.5%FeSO4, 去离子水63%,混合均匀,通氮,加入36%NaOH(1M),加入后溶液变为深黑色,再加入0.03%甲苯基重氮盐,磁力搅拌1小时,室温下反应。离心分离,用无水乙醇洗涤,离心分离,干燥,得到表面改性的磁性Fe3O4纳米粒子,此粒子在pH值为8的水溶液中稳定,粒径6~10nm。
实施例2
在磁力搅拌下,在烧瓶中加入重量比(下同)1.15% FeCl3,0.6%FeSO4, 去离子水56%,混合均匀 ,通氮,加入33%NaOH(1M),加入后溶液变为深黑色,再加入0.045%乙苯基重氮盐,磁力搅拌1小时。离心分离,用无水乙醇洗涤,离心分离,干燥,得到表面改性的磁性Fe3O4纳米粒子,此粒子在pH值为8的水溶液中稳定,粒径6~10nm。
实施例3
在磁力搅拌下,在烧瓶中加入重量比(下同)1.3%FeCl3,0.7%FeSO4, 去离子水49%,混合均匀,通氮,加入30%NaOH(1M),加入后溶液变为深黑色,再加入0.06%甲苯基重氮盐,磁力搅拌1小时。离心分离,用无水乙醇洗涤,离心分离,干燥,得到表面改性的磁性Fe3O4纳米粒子,此粒子在pH值为8的水溶液中稳定,粒径6~10nm。
实施例4
在磁力搅拌下,在烧瓶中加入重量比(下同)1%FeCl3,0.5%FeSO4, 去离子水63%,混合均匀,通氮,加入36%NaOH(1M),加入后溶液变为深黑色,再加入0.03%氯甲基苯重氮盐,磁力搅拌1小时,室温下反应。离心分离,用无水乙醇洗涤,离心分离,干燥,得到具有表面反应功能基的改性磁性Fe3O4纳米粒子,此粒子在pH值为8的水溶液中稳定,粒径6~10nm。
实施例5
在磁力搅拌下,在烧瓶中加入重量比(下同)1.15% FeCl3,0.6%FeSO4, 去离子水56%,混合均匀 ,通氮,加入33%NaOH(1M),加入后溶液变为深黑色,再加入0.045%氯甲基苯重氮盐,磁力搅拌1小时。离心分离,用无水乙醇洗涤,离心分离,干燥,得到具有表面反应功能基的改性磁性Fe3O4纳米粒子,此粒子在pH值为8的水溶液中稳定,粒径6~10nm。
实施例6
在磁力搅拌下,在烧瓶中加入重量比(下同)1.3%FeCl3,0.7%FeSO4, 去离子水49%,混合均匀,通氮,加入30%NaOH(1M),加入后溶液变为深黑色,再加入0.06%氯甲基苯重氮盐,磁力搅拌1小时。离心分离,用无水乙醇洗涤,离心分离,干燥,得到具有表面反应功能基的改性磁性Fe3O4纳米粒子,此粒子在pH值为8的水溶液中稳定,粒径6~10nm。
Claims (4)
1.一种磁性Fe3O4 纳米粒子表面改性的方法,其特征在于:在磁力搅拌下,按重量比1~1.3%的FeCl3,0.5~0.7%的FeSO4, 49~63%的去离子水,混合均匀,通氮,加入30~36% 1M 的NaOH,加入后溶液变为深黑色,再加入0.03~0.06%的重氮盐,反应温度室温,磁力搅拌1 小时,反应气氛N2,在此条件下得到表面改性的磁性Fe3O4纳米粒子 ,其粒径介于6~10nm。
2.如权利要求1所述的方法,其特征在于:所述重氮盐是烷基苯重氮盐或氯甲基苯重氮盐。
3.如权利要求2所述的方法,其特征在于:所述的烷基苯重氮盐是甲苯基重氮盐或乙苯基重氮盐。
4.如权利要求1所述的方法,其特征在于: 所述反应完成后用无水乙醇洗涤,离心分离,干燥,得到表面改性的磁性Fe3O4纳米粒子。
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US20120061608A1 (en) * | 2010-09-10 | 2012-03-15 | Hitachi Maxell, Ltd. | Functional particle with rough-surfaced polymer coating |
CN102648251A (zh) * | 2009-10-16 | 2012-08-22 | 惠普开发有限公司 | 双色可电寻址油墨 |
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US4554088A (en) * | 1983-05-12 | 1985-11-19 | Advanced Magnetics Inc. | Magnetic particles for use in separations |
US5160725A (en) * | 1987-03-24 | 1992-11-03 | Silica Gel Gesellschaft Mbh Adsorptions-Technik, Apparatebau | Magnetic liquid compositions |
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