核—壳型磁性复合纳米材料的制备及其抑菌与催化性研究
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摘要
生产技术水平的提高,带来生活水平的提高,随之也为人类带来更多的负面效应。人类对环境的污染越来越严重,最终使得细菌的种类增加,生长繁殖速度加快,细菌对抗生素的抵抗能力提高。这就使抗菌能力较强的新型抗菌剂的出现变得非常必要。纳米抗菌剂效率最高,但其回收与管理不便。因此本文以磁性颗粒作为载体,对其进行修饰,在磁性核表面负载上抗菌剂,制备出磁性复合抗菌剂。这样不但保证了抗菌剂是做纳米级的抗菌效率高,同时回收和管理也变得非常容易。并通过X-射线衍射仪(XRD), X-射线光电子能谱仪(XPS),扫描电子显微镜(SEM),透射电子显微镜(TEM),傅里转换红外光谱仪(FTIR),X-射线能量散射仪(EDX)和超导量子干涉磁测量系统(SQUID)等手段对所得样品的结构,形貌,磁性进行表征。最后研究复合抗菌剂在不同条件下的抗菌作用。本论文的主要工作从以下三个方面展开
1.结合溶剂热法,水热法和化学还原法制备了Fe3O4@C@Ag(?)Fe3O4@Ag磁性复合纳米颗粒。Fe3O4@C@Ag复合颗粒的平均尺寸在250nm左右,具有较强的磁性,且其表面沉积了一层致密的纳米银颗粒,平均尺寸约为15nm。相反,Fe304@Ag复合颗粒,表面沉积的纳米银颗粒疏松且尺寸分部较大。抑菌试验结论为：在体系纳米银浓度相同的条件下,Fe3O4@C@Ag复合颗粒的抑菌性比Fe304@Ag强。复合颗粒的抗菌性与纳米银的浓度及尺寸有关,当纳米银浓度为5μg/mL时,Fe3O4@C@Ag抑菌性最强。这种载银磁性复合颗粒可回收残余的纳米银,还可使纳米银的局部浓度增大提高其抗菌效率。同时因纳米银具有光学性和催化性,所以Fe3O4@C@Ag复合颗粒将会在许多领域有广泛应用。
2.通过溶剂热法合成磁性γ-Fe2O3载体。研究发现反应温度和碱源的浓度对产物相组成有影响,160℃可以得到纯γ-Fe2O3。通过调节前躯体FeCl3的浓度依次为20,40和60 mmol/mL时,可控制产物的颗粒尺寸依次为205,280和403nm。磁性测试结果表明得到的γ-Fe203为铁磁性,其饱和磁化强度为77.3 emu/g。从而使得以γ-Fe203为载体制备的复合颗粒可操作性更强。
3.通过结合溶剂热法,Stober法和溶胶-凝胶水热法制备磁性复合纳米颗粒γ-Fe2O3@SiO2@TiO2-Ag光降解实验结论为：亚甲基橙浓度为30μg/mL时,加入TiO2-Ag浓度为1 mg/mL的复合催化剂,在250W紫外灯下光降解1 h,亚甲基橙可被完全降解。因磁性核的存在使得此复合催化剂可高效回收重复使用,经18次循环使用,其催化活性几乎还保持稳定。由于银的存在,γ-Fe2O3@SiO2@TiO2-Ag不但在黑暗条件下有较强的抗菌性,在紫外光照射条件下几乎可以抑制所有细菌的生长。既具有光催化降解有机污染物的能力又具有抑制细菌生长的能力使得γ-Fe2O3@SiO2@TiO2-Ag复合颗粒将会在水处理方面有广阔的应用前景。
The level of production technology improving, along with the improvement of living standards, accompanied with more negative effects appear. Human pollution to the environment more and more serious, ultimately making the type of bacteria increase, accelerates the growth and reproduction of bacteria, resistance to antibiotics increase. This makes the emergence of new antimicrobial with strong antibacterial ability has become very necessary. The efficiency of nano-antibacterial agent is higher, but its recovery and management is inconvenience. In this paper, with magnetic particles as a carrier, modified its surface and loaded antibacterial agents on its surface. Lastly, magnetic composite antibacterial agent was prepared. This will not only ensure the high efficient and also the convenience of recovery and management the antibacterial agent. The structure, morphology and magnetic properties of the samples were characterized by means of X-ray diffraction (XRD),X-ray photoelectron spectroscopy (XPS),scanning electron microscopy (SEM). transmission electron microscopy (TEM). fourier transform infrared spectroscopy (FTIR),X-ray energy dispersive analyzer (EDX),magnetic measurement system (SQUID). We research the antibacterial property of the compound antibacterial agent under different conditions.The main work of this paper was developed from the following three aspects.
1.Synthesis of Fe3O4@C@Ag and Fe3O4@Ag composites by solvothermal method, hydrothermal and chemical reduction. The size of the obtained Fe3O4@C@Ag composites is 250 nm, with strong ferromagnetic and a layer of compacted Ag nanoparticles deposited on its surface, the mean size of the Ag nanoparticle is 15 nm. Contrarily,the Ag nanoparticles on the surface of Fe3O4@Ag are loose and the size distribution is large. The antibacterial testing shows that:The antibacterial property of the compsosites is related to the concentration and size of Ag nanoparticles. When the concentration of Ag nanoparticle is 5μg/mL. the antibacterial properties of Fe3O4@C@Ag composites is the strongest. The magnetic composites can recycle the residual Ag nanoparticles and make the concentration of Ag nanoparticles is higher in special locality. The Fe3O4@C@Ag nanocomposites will have more potential uses in many fields for the catalytic and optical properties of the Ag nanopaerticles.
2. The magnetic particlesγ-Fe2O3 was synthesized by solvothermal method. We found that the reaction temperature and concentration of alkali resource have effect to the phase structure of the production. At 160℃. we obtained the pureγ-Fe2O3,By adjusting the concentration of the FeCl2 at 20,40 and 60 mmol/L. the particles size of theγ-Fe2O3 is 205, 280 and 403 nm respectively. The result of magnetism testing shown that the saturation magnetization of theγ-Fe2O3 was 77.3 emu/g,The strong magnetic makes the composites withγ-Fe2O3 as a carrier with stronger operability.
3. Theγ-Fe2O3@SiO2@TiO2-Ag magnetic nanocomposites were synthesized by combining solvothermal,Stober method and sol-gel hydrothermal method. When the concentration of the methyl orange is 30μg/mL. the concentration of composites catalysts contained TiO2-Ag is 1 mg/mL,under the UV light (250 W) irradiation, after 1 h. almost all the methyl orange was decomposed. For the presence of the magnetic core, the composites catalyst can be efficient recovery and reused, after 18 cycles, the catalysis ability keep stable. For the presence of Ag nanoparticles. the composites has antibacterial ability under dark condition, also it can restrain the growth of all the bacteria under UV irradiation. Both the ability of photocatalytic degradation of organic pollutants and inhibit the growth bacterial, make the composites has broad application in the water treatment area.
1.结合溶剂热法,水热法和化学还原法制备了Fe3O4@C@Ag(?)Fe3O4@Ag磁性复合纳米颗粒。Fe3O4@C@Ag复合颗粒的平均尺寸在250nm左右,具有较强的磁性,且其表面沉积了一层致密的纳米银颗粒,平均尺寸约为15nm。相反,Fe304@Ag复合颗粒,表面沉积的纳米银颗粒疏松且尺寸分部较大。抑菌试验结论为：在体系纳米银浓度相同的条件下,Fe3O4@C@Ag复合颗粒的抑菌性比Fe304@Ag强。复合颗粒的抗菌性与纳米银的浓度及尺寸有关,当纳米银浓度为5μg/mL时,Fe3O4@C@Ag抑菌性最强。这种载银磁性复合颗粒可回收残余的纳米银,还可使纳米银的局部浓度增大提高其抗菌效率。同时因纳米银具有光学性和催化性,所以Fe3O4@C@Ag复合颗粒将会在许多领域有广泛应用。
2.通过溶剂热法合成磁性γ-Fe2O3载体。研究发现反应温度和碱源的浓度对产物相组成有影响,160℃可以得到纯γ-Fe2O3。通过调节前躯体FeCl3的浓度依次为20,40和60 mmol/mL时,可控制产物的颗粒尺寸依次为205,280和403nm。磁性测试结果表明得到的γ-Fe203为铁磁性,其饱和磁化强度为77.3 emu/g。从而使得以γ-Fe203为载体制备的复合颗粒可操作性更强。
3.通过结合溶剂热法,Stober法和溶胶-凝胶水热法制备磁性复合纳米颗粒γ-Fe2O3@SiO2@TiO2-Ag光降解实验结论为：亚甲基橙浓度为30μg/mL时,加入TiO2-Ag浓度为1 mg/mL的复合催化剂,在250W紫外灯下光降解1 h,亚甲基橙可被完全降解。因磁性核的存在使得此复合催化剂可高效回收重复使用,经18次循环使用,其催化活性几乎还保持稳定。由于银的存在,γ-Fe2O3@SiO2@TiO2-Ag不但在黑暗条件下有较强的抗菌性,在紫外光照射条件下几乎可以抑制所有细菌的生长。既具有光催化降解有机污染物的能力又具有抑制细菌生长的能力使得γ-Fe2O3@SiO2@TiO2-Ag复合颗粒将会在水处理方面有广阔的应用前景。
The level of production technology improving, along with the improvement of living standards, accompanied with more negative effects appear. Human pollution to the environment more and more serious, ultimately making the type of bacteria increase, accelerates the growth and reproduction of bacteria, resistance to antibiotics increase. This makes the emergence of new antimicrobial with strong antibacterial ability has become very necessary. The efficiency of nano-antibacterial agent is higher, but its recovery and management is inconvenience. In this paper, with magnetic particles as a carrier, modified its surface and loaded antibacterial agents on its surface. Lastly, magnetic composite antibacterial agent was prepared. This will not only ensure the high efficient and also the convenience of recovery and management the antibacterial agent. The structure, morphology and magnetic properties of the samples were characterized by means of X-ray diffraction (XRD),X-ray photoelectron spectroscopy (XPS),scanning electron microscopy (SEM). transmission electron microscopy (TEM). fourier transform infrared spectroscopy (FTIR),X-ray energy dispersive analyzer (EDX),magnetic measurement system (SQUID). We research the antibacterial property of the compound antibacterial agent under different conditions.The main work of this paper was developed from the following three aspects.
1.Synthesis of Fe3O4@C@Ag and Fe3O4@Ag composites by solvothermal method, hydrothermal and chemical reduction. The size of the obtained Fe3O4@C@Ag composites is 250 nm, with strong ferromagnetic and a layer of compacted Ag nanoparticles deposited on its surface, the mean size of the Ag nanoparticle is 15 nm. Contrarily,the Ag nanoparticles on the surface of Fe3O4@Ag are loose and the size distribution is large. The antibacterial testing shows that:The antibacterial property of the compsosites is related to the concentration and size of Ag nanoparticles. When the concentration of Ag nanoparticle is 5μg/mL. the antibacterial properties of Fe3O4@C@Ag composites is the strongest. The magnetic composites can recycle the residual Ag nanoparticles and make the concentration of Ag nanoparticles is higher in special locality. The Fe3O4@C@Ag nanocomposites will have more potential uses in many fields for the catalytic and optical properties of the Ag nanopaerticles.
2. The magnetic particlesγ-Fe2O3 was synthesized by solvothermal method. We found that the reaction temperature and concentration of alkali resource have effect to the phase structure of the production. At 160℃. we obtained the pureγ-Fe2O3,By adjusting the concentration of the FeCl2 at 20,40 and 60 mmol/L. the particles size of theγ-Fe2O3 is 205, 280 and 403 nm respectively. The result of magnetism testing shown that the saturation magnetization of theγ-Fe2O3 was 77.3 emu/g,The strong magnetic makes the composites withγ-Fe2O3 as a carrier with stronger operability.
3. Theγ-Fe2O3@SiO2@TiO2-Ag magnetic nanocomposites were synthesized by combining solvothermal,Stober method and sol-gel hydrothermal method. When the concentration of the methyl orange is 30μg/mL. the concentration of composites catalysts contained TiO2-Ag is 1 mg/mL,under the UV light (250 W) irradiation, after 1 h. almost all the methyl orange was decomposed. For the presence of the magnetic core, the composites catalyst can be efficient recovery and reused, after 18 cycles, the catalysis ability keep stable. For the presence of Ag nanoparticles. the composites has antibacterial ability under dark condition, also it can restrain the growth of all the bacteria under UV irradiation. Both the ability of photocatalytic degradation of organic pollutants and inhibit the growth bacterial, make the composites has broad application in the water treatment area.
引文
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