磁性中空/多孔纳米复合微球的制备、功能化及机理研究
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摘要
磁性中空/多孔纳米复合材料除了具有磁性材料的特殊性质(如超顺磁性)外,其中空或多孔的结构使其具有较大的比表面积、较小的密度、较大的内部空间且表面渗透性好等特点。因此,这类材料在生物医学、催化、污水处理等方面都有很好的应用前景。本论文的研究重点就是以探索磁性中空(多孔)纳米复合材料新颖而简便的合成方法为主,同时研究了其性能及其多功能化改进,并初步研究了该材料在催化和污水处理方面的初步应用。本论文的主要内容如下:
1.利用共沉淀法合成了表面同时含有亲油性的油酸和亲水性的羟基的两亲性磁性四氧化三铁纳米粒子(MPs)。通过控制反应条件可以对其表面的油酸含量进行调控,从而影响其表面性质。在这种两亲性磁性纳米粒子的存在下,利用正相细乳液体系,通过辐射引发苯乙烯界面聚合制备了具有超顺磁性的中空纳米复合微球。界面聚合是由位于油水界面的MPs表面的自由基引发的,而这些自由基是通过水中的·OH夺取MPs表面上羟基中的氢而产生的。研究发现两亲性磁性纳米粒子是形成磁性中空微球的关键,同时磁性纳米粒子表面的油酸含量也对中空球形成具有一定的影响。而制备过程的其它实验条件,如超声时间、MPs的用量、剂量率等则会影响磁性中空微球的大小和尺寸分布。该方法不需要核模板,可以在常温常压下进行;同时,γ射线可以起到消毒灭菌的作用,有利于产物在生物医学方面的应用。
2.以水滴作为形成中空球的软模板,在常温常压下通过辐射反相细乳液聚合制备超顺磁性中空纳米复合微球。水相中水辐解产生的自由基引发苯乙烯在油水界面聚合,从而形成磁性中空球。苯乙烯的用量是决定能否获得中空微球的关键,研究结果表明当苯乙烯用量较小时,可获得薄壁磁性中空球;提高苯乙烯用量,可增加磁性中空球的壁厚;但进一步增加苯乙烯用量,则得到实心的磁性聚合物纳米复合微球。另外,改变水相体积、乳化剂用量和剂量率都会对磁性中空球的尺寸和尺寸分布产生影响。通过这些实验结果进一步讨论了磁性纳米复合微球可能的形成机理。
3.由于在前面合成的磁性中空球的均一性和单分散性均不够好,这会严重影响其在后续生物医学方面的应用。因此,我们发展了一种在常温常压下通过辐射引发反相乳液聚合制备均一、近于单分散的、形貌可控的超顺磁性纳米复合微球的简单方法。12-丙烯酰氧基-9-十八烯酸(AOA,包含部分的钠盐Na-AOA)作为一种表面活性剂,同时可以和苯乙烯发生共聚,其独特的Y型结构能增加反相乳液的稳定性,使最终产物的均一性和单分散性获得提高。研究发现,通过改变加入苯乙烯的用量,可以得到具有不同壁厚和核尺寸的中空球和磁性实心球。
4.以两亲性的MPs为油溶性的乳化剂,十二烷基硫酸钠(SDS)为水溶性表面活性剂,通过水/油/水双重乳液制备了多空磁性纳米复合微球。该方法同样不需要硬模板来形成多孔结构,方法新颖,步骤简单。实验结果表明,初始加入的MPs的量会影响多空磁性纳米复合微球的孔尺寸;而在聚合过程中的实验条件,如搅拌和温度也是能否形成多空结构的重要因素。
5.结合γ射线可以方便制备无机纳米材料的优势,在磁性中空纳米复合微球基础上,制备了多功能的CdS/四氧化三铁/聚(苯乙烯-co-甲基丙烯酸甲酯)微球,它同时具有超顺磁性、荧光性和中空的性质。CdS通过磁性中空球表面的酯基螯合在其表面。紫外-可见吸收光谱和荧光发射光谱表明该多功能磁性复合微球具有量子限域效应。该方法提供了一种较简便温和的制备多功能磁性复合微球的新思路。
6.以多孔活性碳为载体,通过γ射线在常温常压下制备了负载超顺磁性γ-Fe_2O_3纳米粒子的多孔碳材料,磁性纳米粒子随机分散在多孔碳中。这种磁性碳材料具有大的比表面积(844 m~2/g)和大的孔容(0.86 cm~3/g),而且可以通过简单的改变铁盐的初始加入量来调控最终磁性碳材料的饱和磁化率。同时,我们也对磁性多孔碳材料应用于污水处理中有机污染物的清除方面进行了初步研究。结果表明其具有很高的除污能力,而且在污染物被吸收后,可以通过磁铁方便地将吸附污染物的磁性碳材料从中分离出来。另外,我们还研究了磁性多孔碳上负载具有催化活性的纳米银粒子,可应用在催化领域。这种负载银的磁性多孔碳材料在完成一次催化反应后,可以简单地通过磁铁进行回收再利用。实验结果表明其多次使用后仍保持有较高的催化活性。
Magnetic hollow(porous) materials not only process the unique characters of magnetic materials such as superparamagnetism but also their hollow or porous structure make them have large surface area,small density,large internal space and good surface permeability etc.Therefore,the materials have potential applications in bio-medicine,catalysis,sewage treatment etc.The research emphasis of this paper is on exploring the novel and facile synthesis methods of magnetic hollow(porous) materials,studying their properties and modifying them with multifunctional properties.Meanwhile,the applications of them in catalysis and the removal of pollutants in water are investigated also.The main contents of this paper comprise six parts as follows:
1.The amphiphilic magnetic nanoparticles(MPs) whose surface coexist hydrophobic oleic groups and hydrophilic hydroxyl groups are prepared through the co-precipitation method.The content of oleic acid at the surface of MPs which is able to impact the surface properties of MPs can be controlled by changing the reaction conditions.In the presence of the MPs,the superparamagnetic hollow nanocomposite microspheres are prepared in the miniemulsion system through radiation induced the interfacial polymerization of styrene.The polymerization is initiated by the free radicals on the surface of MPs located on the interface of water and oil.These radicals are produced by the attack of.OH etc.in the water against the active hydroxyl groups of MPs.The experimental results indicate that MPs are a key for the formation of magnetic hollow nanocomposite microspheres.Moreover,the content of oleic acid at the surface of MPs has effect on the formation of magnetic hollow spheres also.The experimental conditions such as the ultrasonication time,the added amount of MPs and the dose rate have effect on the size and the size distribution of magnetic hollow spheres.The approach to magnetic hollow nanocomposite microspheres is free to the core template and can be carried out at room temperature and under ambient pressure. Especially,the products synthesized byγ-ray are beneficial to their bio-applications because the contamination of chemical initiators is avoided and the final products are sterilized.
2.We report a facile route to prepare hollow superparamagnetic magnetite/polystyrene nanocomposite microspheres via irradiation induced inverse miniemulsion polymerization at room temperature and under ambient pressure.Water droplets act as a soft template for the formation of hollow structure.The free radicals produced from the radiolysis of water initiate the polymerization of styrene at the interface of oil and water,which lead to the formation of magnetic hollow spheres. The amount of styrene is a key to the formation of hollow spheres.Magnetic hollow spheres with different wall thickness are obtained through changing the amount of styrene in oil phase,and the more styrene can lead to the formation of solid magnetic nanocomposite microspheres.The volume of water phase,the amount of surfactant and the dose rate all have effect on the size and the size distribution of magnetic hollow spheres.According to the results,we further discuss the formation mechanism of magnetic nanocomposite microspheres.
3.Because the uniformity and monodispersity of magnetic hollow spheres in first two parts is not enough good,which is disadvantageous to downstream applications,we develop a facile approach to uniform and nearly monodisperse magnetic nanocomposite microspheres with controllable structure via irradiation induced inverse emulsion polymerization at room temperature and under ambient pressure.12-acryloxy-9-octadecenoic acid(AOA,containing part of sodium salts Na-AOA) as a surfactant can also copolymerize with the styrene.Moreover,its unique structure increases the stability of inverse emulsion,leading to the better uniformity and monodispersity of final products.It is interesting that just by changing the added amount of styrene,the magnetic hollow spheres with different wall thickness and various sizes of core,up to the magnetic solid spheres,can be obtained.
4.We offer a simply method to the preparation of multihollow magnetic nanocomposite microspheres via water-in-oil-in-water double emulsions.Amphiphilic magnetite nanoparticles act as an oil-soluble emulsifier and sodium dodecyl sulfate (SDS) acts as a water-soluble surfactant in the system.The method is novel,facile and template-free to the formation of porous structure.The results show that the added amount of MPs impacts the pore size of multihollow magnetic nanocomposite microspheres.In addition,the experimental conditions during the course of polymerization such as stirring and temperature are also two key factors to the formation of multihollow structure.
5.Combining the as-synthesized magnetic hollow nanocomposite microspheres and the superiority of the facile preparation of inorganic nanomaterials viaγ-ray,we prepare multifunctional CdS/magnetite/poly(styrene-co-methyl methacrylate) microspheres,which possess superparamagnetic,fluorescent and hollow properties.CdS nanoparticles are chelated on the surface of magnetic hollow spheres through the carbonyl groups located at the surface of them.The Uv-vis and photoluminescence spectrum show that the multifunctional nanocomposite spheres have the quantum-confined effect.In this section,we offer a facile and mild method to the synthesis of multifunctional magnetic nanocomposite microspheres.
6.Using porous activated carbons as carriers,we prepare superparamagnetic porous carbons materials,in which superparamagneticγ-Fe_2O_3 nanoparticles are randomly dispersed in the porous carbons.The magnetic porous carbon materials have large surface area(844 m~2/g) and large pore volume(0.86 cm~3/g).Meanwhile, the saturation magnetism can be tunable by changing the initial amount of iron salt. We also study the application of magnetic porous carbon materials in the removal of organic pollutants in water.After the pollutants are absorbed by magnetic carbon materials,they can be separated from the water easily by the magnet.The experimental results display the magnetic porous materials have high capacity of removing the pollutants.On the other hand,Ag nanoparticles which possess catalysis are loaded in magnetic porous carbon materials,which can apply in the catalytic area and be recycled by the magnet.The experimental results show that they still have better catalytic activity after being used many times.
1.利用共沉淀法合成了表面同时含有亲油性的油酸和亲水性的羟基的两亲性磁性四氧化三铁纳米粒子(MPs)。通过控制反应条件可以对其表面的油酸含量进行调控,从而影响其表面性质。在这种两亲性磁性纳米粒子的存在下,利用正相细乳液体系,通过辐射引发苯乙烯界面聚合制备了具有超顺磁性的中空纳米复合微球。界面聚合是由位于油水界面的MPs表面的自由基引发的,而这些自由基是通过水中的·OH夺取MPs表面上羟基中的氢而产生的。研究发现两亲性磁性纳米粒子是形成磁性中空微球的关键,同时磁性纳米粒子表面的油酸含量也对中空球形成具有一定的影响。而制备过程的其它实验条件,如超声时间、MPs的用量、剂量率等则会影响磁性中空微球的大小和尺寸分布。该方法不需要核模板,可以在常温常压下进行;同时,γ射线可以起到消毒灭菌的作用,有利于产物在生物医学方面的应用。
2.以水滴作为形成中空球的软模板,在常温常压下通过辐射反相细乳液聚合制备超顺磁性中空纳米复合微球。水相中水辐解产生的自由基引发苯乙烯在油水界面聚合,从而形成磁性中空球。苯乙烯的用量是决定能否获得中空微球的关键,研究结果表明当苯乙烯用量较小时,可获得薄壁磁性中空球;提高苯乙烯用量,可增加磁性中空球的壁厚;但进一步增加苯乙烯用量,则得到实心的磁性聚合物纳米复合微球。另外,改变水相体积、乳化剂用量和剂量率都会对磁性中空球的尺寸和尺寸分布产生影响。通过这些实验结果进一步讨论了磁性纳米复合微球可能的形成机理。
3.由于在前面合成的磁性中空球的均一性和单分散性均不够好,这会严重影响其在后续生物医学方面的应用。因此,我们发展了一种在常温常压下通过辐射引发反相乳液聚合制备均一、近于单分散的、形貌可控的超顺磁性纳米复合微球的简单方法。12-丙烯酰氧基-9-十八烯酸(AOA,包含部分的钠盐Na-AOA)作为一种表面活性剂,同时可以和苯乙烯发生共聚,其独特的Y型结构能增加反相乳液的稳定性,使最终产物的均一性和单分散性获得提高。研究发现,通过改变加入苯乙烯的用量,可以得到具有不同壁厚和核尺寸的中空球和磁性实心球。
4.以两亲性的MPs为油溶性的乳化剂,十二烷基硫酸钠(SDS)为水溶性表面活性剂,通过水/油/水双重乳液制备了多空磁性纳米复合微球。该方法同样不需要硬模板来形成多孔结构,方法新颖,步骤简单。实验结果表明,初始加入的MPs的量会影响多空磁性纳米复合微球的孔尺寸;而在聚合过程中的实验条件,如搅拌和温度也是能否形成多空结构的重要因素。
5.结合γ射线可以方便制备无机纳米材料的优势,在磁性中空纳米复合微球基础上,制备了多功能的CdS/四氧化三铁/聚(苯乙烯-co-甲基丙烯酸甲酯)微球,它同时具有超顺磁性、荧光性和中空的性质。CdS通过磁性中空球表面的酯基螯合在其表面。紫外-可见吸收光谱和荧光发射光谱表明该多功能磁性复合微球具有量子限域效应。该方法提供了一种较简便温和的制备多功能磁性复合微球的新思路。
6.以多孔活性碳为载体,通过γ射线在常温常压下制备了负载超顺磁性γ-Fe_2O_3纳米粒子的多孔碳材料,磁性纳米粒子随机分散在多孔碳中。这种磁性碳材料具有大的比表面积(844 m~2/g)和大的孔容(0.86 cm~3/g),而且可以通过简单的改变铁盐的初始加入量来调控最终磁性碳材料的饱和磁化率。同时,我们也对磁性多孔碳材料应用于污水处理中有机污染物的清除方面进行了初步研究。结果表明其具有很高的除污能力,而且在污染物被吸收后,可以通过磁铁方便地将吸附污染物的磁性碳材料从中分离出来。另外,我们还研究了磁性多孔碳上负载具有催化活性的纳米银粒子,可应用在催化领域。这种负载银的磁性多孔碳材料在完成一次催化反应后,可以简单地通过磁铁进行回收再利用。实验结果表明其多次使用后仍保持有较高的催化活性。
Magnetic hollow(porous) materials not only process the unique characters of magnetic materials such as superparamagnetism but also their hollow or porous structure make them have large surface area,small density,large internal space and good surface permeability etc.Therefore,the materials have potential applications in bio-medicine,catalysis,sewage treatment etc.The research emphasis of this paper is on exploring the novel and facile synthesis methods of magnetic hollow(porous) materials,studying their properties and modifying them with multifunctional properties.Meanwhile,the applications of them in catalysis and the removal of pollutants in water are investigated also.The main contents of this paper comprise six parts as follows:
1.The amphiphilic magnetic nanoparticles(MPs) whose surface coexist hydrophobic oleic groups and hydrophilic hydroxyl groups are prepared through the co-precipitation method.The content of oleic acid at the surface of MPs which is able to impact the surface properties of MPs can be controlled by changing the reaction conditions.In the presence of the MPs,the superparamagnetic hollow nanocomposite microspheres are prepared in the miniemulsion system through radiation induced the interfacial polymerization of styrene.The polymerization is initiated by the free radicals on the surface of MPs located on the interface of water and oil.These radicals are produced by the attack of.OH etc.in the water against the active hydroxyl groups of MPs.The experimental results indicate that MPs are a key for the formation of magnetic hollow nanocomposite microspheres.Moreover,the content of oleic acid at the surface of MPs has effect on the formation of magnetic hollow spheres also.The experimental conditions such as the ultrasonication time,the added amount of MPs and the dose rate have effect on the size and the size distribution of magnetic hollow spheres.The approach to magnetic hollow nanocomposite microspheres is free to the core template and can be carried out at room temperature and under ambient pressure. Especially,the products synthesized byγ-ray are beneficial to their bio-applications because the contamination of chemical initiators is avoided and the final products are sterilized.
2.We report a facile route to prepare hollow superparamagnetic magnetite/polystyrene nanocomposite microspheres via irradiation induced inverse miniemulsion polymerization at room temperature and under ambient pressure.Water droplets act as a soft template for the formation of hollow structure.The free radicals produced from the radiolysis of water initiate the polymerization of styrene at the interface of oil and water,which lead to the formation of magnetic hollow spheres. The amount of styrene is a key to the formation of hollow spheres.Magnetic hollow spheres with different wall thickness are obtained through changing the amount of styrene in oil phase,and the more styrene can lead to the formation of solid magnetic nanocomposite microspheres.The volume of water phase,the amount of surfactant and the dose rate all have effect on the size and the size distribution of magnetic hollow spheres.According to the results,we further discuss the formation mechanism of magnetic nanocomposite microspheres.
3.Because the uniformity and monodispersity of magnetic hollow spheres in first two parts is not enough good,which is disadvantageous to downstream applications,we develop a facile approach to uniform and nearly monodisperse magnetic nanocomposite microspheres with controllable structure via irradiation induced inverse emulsion polymerization at room temperature and under ambient pressure.12-acryloxy-9-octadecenoic acid(AOA,containing part of sodium salts Na-AOA) as a surfactant can also copolymerize with the styrene.Moreover,its unique structure increases the stability of inverse emulsion,leading to the better uniformity and monodispersity of final products.It is interesting that just by changing the added amount of styrene,the magnetic hollow spheres with different wall thickness and various sizes of core,up to the magnetic solid spheres,can be obtained.
4.We offer a simply method to the preparation of multihollow magnetic nanocomposite microspheres via water-in-oil-in-water double emulsions.Amphiphilic magnetite nanoparticles act as an oil-soluble emulsifier and sodium dodecyl sulfate (SDS) acts as a water-soluble surfactant in the system.The method is novel,facile and template-free to the formation of porous structure.The results show that the added amount of MPs impacts the pore size of multihollow magnetic nanocomposite microspheres.In addition,the experimental conditions during the course of polymerization such as stirring and temperature are also two key factors to the formation of multihollow structure.
5.Combining the as-synthesized magnetic hollow nanocomposite microspheres and the superiority of the facile preparation of inorganic nanomaterials viaγ-ray,we prepare multifunctional CdS/magnetite/poly(styrene-co-methyl methacrylate) microspheres,which possess superparamagnetic,fluorescent and hollow properties.CdS nanoparticles are chelated on the surface of magnetic hollow spheres through the carbonyl groups located at the surface of them.The Uv-vis and photoluminescence spectrum show that the multifunctional nanocomposite spheres have the quantum-confined effect.In this section,we offer a facile and mild method to the synthesis of multifunctional magnetic nanocomposite microspheres.
6.Using porous activated carbons as carriers,we prepare superparamagnetic porous carbons materials,in which superparamagneticγ-Fe_2O_3 nanoparticles are randomly dispersed in the porous carbons.The magnetic porous carbon materials have large surface area(844 m~2/g) and large pore volume(0.86 cm~3/g).Meanwhile, the saturation magnetism can be tunable by changing the initial amount of iron salt. We also study the application of magnetic porous carbon materials in the removal of organic pollutants in water.After the pollutants are absorbed by magnetic carbon materials,they can be separated from the water easily by the magnet.The experimental results display the magnetic porous materials have high capacity of removing the pollutants.On the other hand,Ag nanoparticles which possess catalysis are loaded in magnetic porous carbon materials,which can apply in the catalytic area and be recycled by the magnet.The experimental results show that they still have better catalytic activity after being used many times.
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