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纳米光催化剂TiO_2/Fe_3O_4的制备及表征 总被引:5,自引:3,他引:2
采用两步法制备磁性负载纳米光催化剂TiO2/Fe3O4。首先用液相共沉淀法制备磁性纳米Fe3O4颗粒;然后用溶胶-凝胶法,以钛酸四正丁酯为先驱体,通过水解缩聚在Fe3O4纳米颗粒表面包覆TiO2层,得到易于磁分离回收的复合纳米光催化剂TiO2/Fe3O4,粒径大约为30 nm。利用TEM、XRD、FT-IR、VSM对Fe3O4和TiO2/Fe3O4的结构和性能进行了表征,结果表明,制备的Fe3O4为面心立方晶体(FCC)结构,具有超顺磁性;TiO2为锐钛矿相,包覆在Fe3O4的表面,形成了核-壳式结构的TiO2/Fe3O4复合光催化剂。 相似文献
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采用改进St?ber法制备超顺磁Fe3O4@SiO2复合粒子作为催化剂载体,再通过浸渍法将H3PW12O40(HPW)负载在Fe3O4@SiO2载体上,制备了一系列超顺磁负载型催化剂HPW/Fe3O4@SiO2。并使用X射线衍射(XRD)、傅里叶红外(FT-IR)、氨的程序升温脱附(NH3-TPD)、扫描电镜(SEM)、N2吸附-脱附和振动样品强磁计(VSM)对催化剂进行表征。结果表明,HPW固定并均匀分散在Fe3O4@SiO2载体上,40%HPW/Fe3O4@SiO2催化剂具有较高的饱和磁强度(30.1 emu·g?1)和较大的比表面积(303.6 m2·g?1),并可用外加磁场进行分离。采用40%HPW/Fe3O4@SiO2催化噻吩与1-辛烯组成的模拟汽油的烷基化脱硫反应,在160℃下反应2 h,噻吩转化率达到85.5%,有较好的催化脱硫性能,且可以多次循环利用。 相似文献
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共沉淀法制备纳米Fe3O4影响因素的研究 总被引:2,自引:0,他引:2
利用正交设计的数学方法进行实验设计,采用液相共沉淀法制备纳米级Fe3O4颗粒,考察不同影响因素对微球平均粒径大小的影响,寻找制备纳米颗粒的最佳条件.所考察的因素分别为胶溶化时HCl加入量、Fe3+与Fe2+的比例、共沉淀时的pH值、制备Fe3O4的晶化温度.结果表明,以胶溶化时加入HCl3mL、Fe3+与Fe2+的比例2:3、共沉淀时的pH值11和制备Fe3O4的晶化温度80℃为最佳实验条件为,此时制得的纳米粉体平均粒径可达16.3nm;并利用粒径分析仪和HRTEM对所制备纳米粉进行结构表征. 相似文献
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FeCl2×4H2O和FeCl3×6H2O为原料、NaOH为沉淀剂,采用撞击流-旋转填料床制备Fe3O4纳米颗粒,考察了超重力因子、液体流量和反应物浓度对Fe3O4颗粒粒径的影响及其对Pb(II)和Cd(II)的吸附性能. 结果表明,随超重力因子、液体流量及反应物浓度增加,Fe3O4颗粒的粒径减小,最佳制备条件为超重力因子65.32、液体流量60 L/h及FeCl3×6H2O浓度0.321 mol/L,该条件下所制超顺磁性单分散Fe3O4纳米颗粒的平均粒径约为10 nm,饱和磁化强度为60.5 emu/g. Fe3O4纳米颗粒对Pb(II)和Cd(II)吸附过程符合Langmuir吸附等温模型,计算的最大吸附容量分别为30.47和13.04 mg/g. 相似文献
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ABSTRACT: Magnetic nanoparticles with attractive optical properties have been proposed for applications in such areas as separation and magnetic resonance imaging. In this paper, a simple and novel fluorescent sensor of Zn2+ was designed with 3,5-di-tert-butyl-2-hydroxybenzaldehyde [DTH] covalently grafted onto the surface of magnetic core/shell Fe3O4@SiO2 nanoparticles [NPs] (DTH-Fe3O4@SiO2 NPs) using the silanol hydrolysis approach. The DTH-Fe3O4@SiO2 inorganic-organic hybrid material was characterized by transmission electron microscopy, dynamic light scattering, X-ray power diffraction, diffuse reflectance infrared Fourier transform, UV-visible absorption and emission spectrometry. The compound DTH exhibited fluorescence response towards Zn2+ and Mg2+ ions, but the DTH-Fe3O4@SiO2 NPs only effectively recognized Zn2+ ion by significant fluorescent enhancement in the presence of various ions, which is due to the restriction of the N-C rotation of DTH-Fe3O4@SiO2 NPs and the formation of the rigid plane with conjugation when the DTH-Fe3O4@SiO2 is coordinated with Zn2+. Moreover, this DTH-Fe3O4@SiO2 fluorescent chemosensor also displayed superparamagnetic properties, and thus, it can be recycled by magnetic attraction. 相似文献
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Core-shell Fe3O4@SiO2 nanoparticles synthesized with well-dispersed hydrophilic Fe3O4 seeds 总被引:1,自引:0,他引:1
Silica coated magnetite (Fe3O4@SiO2) core-shell nanoparticles (NPs) with controlled silica shell thicknesses were prepared by a modified St?ber method using 20 nm hydrophilic Fe3O4 NPs as seeds. The core-shell NPs were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), selected area electron diffraction (SAED), and UV-Vis adsorption spectra (UV-Vis). The results imply that NPs consist of a crystalline magnetite core and an amorphous silica shell. The silica shell thickness can be controlled from 12.5 nm to 45 nm by varying the experimental parameters. The reaction time, the ratio of TEOS/Fe3O4, and the concentration of hydrophilic Fe3O4 seeds were found to be very influential in the control of silica shell thickness. These well-dispersed core-shell Fe3O4@SiO2 NPs show superparamagnetic properties at room temperature. 相似文献
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利用3-氨丙基三乙氧基硅烷(APTES)对制备的SiO2包覆Fe3O4复合粒子(Fe3O4@SiO2)进行改性,制备了氨基硅烷功能化磁性材料Fe3O4@SiO2-NH2,将Fe3O4@SiO2-NH2作为载体用于固定化琼胶酶。采用SEM、FTIR、VSM对Fe3O4@SiO2-NH2和固定化琼胶酶进行了表征,对琼胶酶的固定化条件进行了优化,评价了固定化琼胶酶的性能。结果表明,琼胶酶成功固定在载体上。Fe3O4@SiO2-NH2的磁化饱和强度为48.4 emu/g,固定化琼胶酶的磁化饱和强度为42.8 emu/g... 相似文献
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先通过硅酸钠水解在磁性Fe3O4纳米粒子表面包覆二氧化硅,制得磁性硅粒子(Fe3O4@SiO2);然后再通过碳二亚胺活化接枝法在Fe3O4@SiO2纳米粒子表面接枝高脱乙酰度羧甲基化壳聚糖(CMC),制备了一种新型磁性纳米吸附剂(Fe3O4@SiO2@CMC)。通过透射电镜(TEM)、红外光谱(IR)、X射线衍射(XRD)以及振动样品磁强计(VSM)对其进行了表征,着重研究了其对水中Cr(Ⅵ)离子的吸附性能。结果表明:溶液的pH值能显著影响吸附剂对Cr(Ⅵ)离子的吸附效果,pH值为2时效果最佳。结合相应pH值下Cr(Ⅵ)的形态分布,探讨了这种新型材料对Cr(Ⅵ)的吸附机理。结果表明:其吸附机理及吸附容量与Cr(Ⅵ)的离子形式有关,吸附过程以离子交换与静电引力为主。吸附平衡数据分别采用了Langmuir和Freundlich方程进行拟合。结果表明,等温吸附数据更符合Langmuir模型,T=298 K、pH=2、V=5 mL时,吸附剂的饱和吸附容量qm=86.96 mg/g,吸附常数为0.0174 L/mg。 相似文献
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以甲基丙烯酸和丙烯酰胺为功能单体,通过悬浮聚合法制备了氨基和羧基双功能化的磁性复合微球(Fe3 O4@SiO2-NH2/COOH),并探讨了其对水溶液中Cd(Ⅱ)和Pb(Ⅱ)的吸附性能.X-射线衍射(XRD)分析表明,制备的磁性吸附剂内核为Fe3 O4.红外光谱(FT-IR)和扫描电镜(SEM)测试表明,氨基和羧基对Fe3 O4@SiO2表面改性成功.吸附试验显示,Fe3O4@SiO2-NH2/COOH吸附Cd(Ⅱ)和Pb(Ⅱ)的最优pH值分别为5.0和5.5,吸附过程均符合动力学准二级模型和Langmuir吸附等温模型,吸附剂对Cd(Ⅱ)和Pb(Ⅱ)最大吸附量分别为207.807 mg/g和168.995 mg/g.实际饮用水样中Cd(Ⅱ)和Pb(Ⅱ)的吸附表明,去除率分别可达97.74%和91.44%.该磁性吸附剂对两种重金属离子吸附量大、去除率高,具有良好的实际应用潜力. 相似文献
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采用氧化法和正硅酸乙酯水解法制备了Mn3O4@SiO2核壳结构磁性纳米材料,研究了其对水溶液中Mo(VI)离子的吸附效果。运用X射线衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)、红外光谱仪(IR)及磁强计(VSM) 等多种手段对Mn3O4@SiO2核壳磁性复合材料进行了表征,并研究了溶液的初始pH、Mo(VI)离子初始浓度和温度对Mo(VI)吸附量的影响。结果表明:在298 K条件下Mn3O4@SiO2核壳结构磁性复合材料对Mo (VI)的饱和吸附量为145.35 mg/g; Mn3O4@SiO2对Mo (VI)的吸附过程符合Langmuir等温吸附模型,吸附动力学符合准二级动力学模型;吸附热力学分析表明Mn3O4@SiO2复合材料对Mo (VI) 的吸附行为是自发的、放热过程。 相似文献
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为了探究固体颗粒对乳液的稳定作用,采用双亲染料分子罗丹明B对核壳结构的Fe_3O_4@SiO_2纳米颗粒进行疏水改性,并将改性后的纳米颗粒作为稳定剂制备Pickering乳液。通过Zeta电位、FTIR、XRD、SEM、接触角测量、光学显微镜、电导率仪对Fe_3O_4@SiO_2纳米颗粒以及Pickering乳液的结构、形貌和性能进行表征与分析,结果表明:制备的纳米颗粒粒径小,约为150 nm,为单分散球形核壳结构;罗丹明B成功修饰到Fe_3O_4@SiO_2纳米颗粒表面,改性后颗粒接触角由30°增加至120°;随乳化剂颗粒质量浓度的增加,制备的乳液液滴的粒径减小。另外,所得Pickering乳液具有良好的磁场响应性,可通过外加磁场实现对乳液稳定性的可逆调控,且此过程可重复3次以上。 相似文献
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Optomagnetic multifunctional composite based on upconversion luminescence nanomaterial is regarded as a promising strategy for bioimaging,disease diagnosis and targeted delivery of drugs.To explore a mesoporous nanostructure with excellent water dispersibility and high drug-loading capacity,a novel nanorattle-structured Fe3O4@SiO2@NaYF4∶Yb,Er magnetic upconversion nanorattle (MUCNR) was suc-cessfully designed by using Fe3O4 as core and NaYF4∶Yb,Er nanocrystals as shell.The microstructures and crystal phase of the as-prepared MUCNRs were evaluated by transmission electron microscopy,X-ray powder diffraction and N2 adsorption/desorption isotherms.The Kirkendall effect was adapted to explain the formation mechanism of the MUCNRs.The loading content and encapsulation efficiency of doxorubicin hydrochloride (DOX) could reach as high as 18.2% and 60.7%,respectively.Moreover,the DOX loading MUCNR (DOX-MUCNR) system showed excellent sustained drug release and strong pH-dependent performance,which was conducive to drug release at the slightly acidic microenvironment of tumor.Microcalorimetry was used to quantify the interactions between the carrier structure and drug release rate directly.The heat release rates in the heat-flow diagrams are basically consistent with the DOX release rate,thereby showing that microcalorimetry assay not only provides a unique thermody-namic explanation for the structure-activity relationship of Fe3O4@SiO2@NaYF4∶Yb,Er MUCNRs but also provides powerful guidance to avoid the blind selection or design of drug carriers.Therefore,our work firmly provided a comprehensive perspective for using Fe3O4@SiO2@NaYF4∶Yb,Er MUCNRs as a remark-able magnetic targeted drug carrier. 相似文献
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通过溶剂热法制备出高磁性的聚合物微球MnFe_2O_4,经正硅酸乙酯(TEOS)和3-氨基丙基三乙氧基硅烷(APTS)对微球表面进行改性修饰,制备出新型复合材料MnFe_2O_4@SiO_2-NH_2,并将其用于固定青霉素G酰化酶。在Si/Fe比为7 mmol/g、n(TEOS)∶n(APTS)=1∶1时,固定化酶PGA/MnFe_2O_4@SiO_2-NH_2在37℃下水解青霉素G钾合成6-氨基青霉烷酸,表观酶活为1 660 IU/g、载酶量为107.1 mg/g、比酶活为15.5 IU/mg、活性回收率为46.9%。经过6次重复使用,保留初始酶活的81.3%,在使用中固定化酶在磁场的作用下能够快速沉降与产物分离。 相似文献