CN104353431A - 一种β-环糊精修饰的磁性纳米粒子的制备方法 - Google Patents
一种β-环糊精修饰的磁性纳米粒子的制备方法 Download PDFInfo
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Abstract
本发明涉及一种β-环糊精修饰的磁性纳米粒子的制备方法,制备了一种核壳结构的复合纳米微球。首先采用水热法合成了磁性四氧化三铁纳米粒子,然后以稻壳水解的产物硅酸钠作为硅原,将纳米粒子包附一层SiO2,再将β-CD修饰在其表面,制备出具有一定吸附能力的磁性纳米微球,此种复合纳米微球不但具有磁性粒子的超顺磁性,而且还具有环糊精超分子的主客体包合作用,此种Fe3O4SiO2/β-CD的纳米微球以其优异的超顺磁性和超分子的包合作用会环境污染治理方面应用起到巨大的作用。
Description
技术领域
本发明涉及一种β-环糊精修饰的磁性纳米粒子的制备,具体涉及首先制备了一种核壳结构的复合纳米微球,再将β-CD修饰在其表面,获得具有一定吸附能力的磁性纳米微球的研究方法。
背景技术
过去的几十年,磁性纳米粒子已应用到很多不同领域,如传统的电学,光学,磁学等,在新领域的应用包括磁辅助生物分离与生物催化,有毒阴离子、阳离子和金属离子的吸附,如砷(V),铬(VI)和U(VI)。此外,磁性纳米粒子在磁性活体标记、细胞示踪、负载酶等生物医学领域展现出广阔的应用前景。磁性纳米粒子的应用成为目前最引人注目和最具活力的研究领域之一。众所周知,作为第二代超分子代表的环糊精(CDs)是不同数量的吡喃葡萄糖单元通过α-(1-4)糖苷键连接而成的环状低聚糖。由于环糊精中的葡萄糖单元均为椅式构象,形成了中间空洞且两端不封闭的锥筒形结构,其中,所有的伯羟基位于锥体的一侧,而所有仲羟基位于锥体的另一侧,所以环糊精的筒形结构也被称作截锥结构。因此,环糊精的外壁具有亲水性,而中心空腔是疏水、亲脂性的。由于这样的特点,环糊精可以有选择性的识别客体分子,与一些尺寸相宜的有机、无机客体分子相包合,形成超分子体系,因此在生物传感、医药材料、环境治理等领域得到广泛的应用,受到研究者们的亲睐。
当今许多工业生产面对的环境污染问题是去除污水中的染料。由于很多染料具有良好的溶解性,是常见的水污染物。其中一些偶氮类染料,一些微生物能够分解偶氮(N=N)基团,导致其形成芳香胺类产物,它们大部分是有毒的致癌物质,会影响水生生物的生存,造成严重环境问题。因此,去除工业废水中染料的方法是一个重大的挑战,现已应用的解决方法如吸附,混凝,生物降解,化学降解和光降解等。
发明内容
为实现本发明所提供的实验方案是:
(1)采用水热法合成了Fe3O4磁性纳米粒子
首先称取一定量的FeCl3·6H2O置于烧杯中,倒入一定量的乙二醇,室温溶解,搅拌向上述溶液加入一定量的无水乙酸钠,在高压反应釜反应,反应温度为220℃,时间为24h取出,将制备的黑色固体分别用无水乙醇、去离子水清洗,干燥即可得到Fe3O4纳米粒子;
(2)合成Fe3O4SiO2复合纳米粒子
称取一定比例的乙醇和去离子水于圆底烧瓶中,将步骤(1)一定量的清洗干净的Fe3O4纳米粒子经超声处理均匀散在混合溶液中,然后继续向混合体系中滴加一定量的硅酸钠溶液,通入CO2气体,在室温的条件下搅拌6-12h,停止搅拌后施加磁场使纳米粒子富集吸出,分别用去离子水和乙醇漂洗,真空干燥即可得到棕黑色的Fe3O4SiO2复合纳米粒子;
(3)环糊精修饰的磁性纳米粒子的合成
称取一定量的β-环糊精完全溶解在50mL的DMF里,让向此溶液加入一定量的氢化钠,在室温下搅拌得到白色透明溶液,然后将一定量的硅烷偶联剂加入到上述溶液中,置于抽真空的圆底烧瓶内,在氮气保护下搅拌2-8h,反应温度为90℃,反应结束后,将溶液冷却至室温,将一定量的步骤(2)中合成的Fe3O4SiO2加入到上述溶液,然后向混合溶液中滴加氨水(25%),然后在室温下将混合物剧烈搅拌反应结束后,通过磁铁将复合粒子吸出,分别用DMF、去离子水和乙醇漂洗,干燥即可得到棕黑色Fe3O4SiO2/β-CD磁性复合纳米粒子。
理解本发明,下面结合实施例对本发明做进一步地详细说明,但是本发明要求保护的范围并不局限于实施例表示的范围。
实施例1:
(1)采用水热法合成了Fe3O4磁性纳米粒子
首先称取1g的FeCl3·6H2O置于烧杯中,倒入50ml的乙二醇,室温溶解,搅拌向上述溶液加入3g的无水乙酸钠,在高压反应釜反应,反应温度为220℃,时间为24h取出,将制备的黑色固体分别用无水乙醇、去离子水清洗,干燥即可得到Fe3O4纳米粒子;
(2)合成Fe3O4SiO2复合纳米粒子
称取体积比例4∶1的乙醇和去离子水于圆底烧瓶中,将步骤(1)0.02g的清洗干净的Fe3O4纳米粒子经超声处理均匀散在混合溶液中,然后继续向混合体系中滴加10ml的硅酸钠溶液,通入CO2气体,在室温的条件下搅拌6-12h,停止搅拌后施加磁场使纳米粒子富集吸出,分别用去离子水和乙醇漂洗,真空干燥即可得到棕黑色的Fe3O4SiO2复合纳米粒子;
(3)环糊精修饰的磁性纳米粒子的合成
称取2g的β-环糊精完全溶解在50mL的DMF里,让向此溶液加入0.4g的氢化钠,在室温下搅拌得到白色透明溶液,然后将3ml的硅烷偶联剂加入到上述溶液中,置于抽真空的圆底烧瓶内,在氮气保护下搅拌6h,反应温度为90℃,反应结束后,将溶液冷却至室温。将0.8g的步骤(2)中合成的Fe3O4SiO2加入到上述溶液,然后向混合溶液中滴加氨水(25%),然后在室温下将混合物剧烈搅拌反应结束后,通过磁铁将复合粒子吸出,分别用DMF、去离子水和乙醇漂洗,干燥即可得到棕黑色Fe3O4SiO2/β-CD磁性复合纳米粒子。
Claims (1)
1.一种β-环糊精修饰的磁性纳米粒子的制备方法,具体步骤如下:
(1)采用水热法合成了Fe3O4磁性纳米粒子
首先称取一定量的FeCl3·6H2O置于烧杯中,倒入一定量的乙二醇,室温溶解,搅拌向上述溶液加入一定量的无水乙酸钠,在高压反应釜反应,反应温度为220℃,时间为24h取出,将制备的黑色固体分别用无水乙醇、去离子水清洗,干燥即可得到Fe3O4纳米粒子;
(2)合成Fe3O4SiO2复合纳米粒子
称取一定比例的乙醇和去离子水于圆底烧瓶中,将步骤(1)一定量的清洗干净的Fe3O4纳米粒子经超声处理均匀散在混合溶液中,然后继续向混合体系中滴加一定量的硅酸钠溶液,通入CO2气体,在室温的条件下搅拌6-12h,停止搅拌后施加磁场使纳米粒子富集吸出,分别用去离子水和乙醇漂洗,真空干燥即可得到棕黑色的Fe3O4SiO2复合纳米粒子;
(3)环糊精修饰的磁性纳米粒子的合成
称取一定量的β-环糊精完全溶解在50mL的DMF里,让向此溶液加入一定量的氢化钠,在室温下搅拌得到白色透明溶液,然后将一定量的硅烷偶联剂加入到上述溶液中,置于抽真空的圆底烧瓶内,在氮气保护下搅拌2-8h,反应温度为90℃,反应结束后,将溶液冷却至室温,将一定量的步骤(2)中合成的Fe3O4SiO2加入到上述溶液,然后向混合溶液中滴加氨水(25%),然后在室温下将混合物剧烈搅拌反应结束后,通过磁铁将复合粒子吸出,分别用DMF、去离子水和乙醇漂洗,干燥即可得到棕黑色Fe3O4SiO2/β-CD磁性复合纳米粒子。
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