柑橘皮提取液绿色合成纳米Fe3O4及其吸附水中孔雀石绿的性能研究

以柑橘皮提取液为还原剂和稳定剂,绿色合成Fe3O4纳米材料,利用扫描电子显微镜(SEM)、X射线衍射图谱(XRD)、傅立叶变换红外光谱(FT-IR)等手段对材料进行表征,并考察了其对孔雀石绿(MG)的吸附性能。结果表明:绿色合成纳米Fe3O4呈不规则圆球体,分散性和结晶度较好。在投加量为1.0 g/L、初始pH为4、温度为25℃、初始浓度为20 mg/L时,对孔雀石绿的吸附率达到95.33%。纳米Fe3O4对MG的吸附过程分别符合准二级动力学方程和Langmuir等温方程。热力学研究表明,纳米Fe3O4吸附MG是自发吸热过程。绿色合成纳米Fe3O4重复利用4次吸附率仍在70%以上。

基于Fe3O4@Au模拟酶智能手机比色法检测牛奶中尿酸的研究

目的 利用Fe3O4@Au的过氧化物模拟酶活性构建检测牛奶中过量尿酸的智能手机比色传感器。方法 通过单因素正交实验获取模拟酶比色和智能手机比色的最佳检测条件,利用紫外分光光度法和智能手机比色法测定不同浓度的尿酸溶液,同时评估体系的灵敏度、抗干扰性和稳定性。结果 Fe3O4@Au最优催化体系为反应温度60℃,反应时间50min及Fe3O4@Au添加量0.015g。智能手机比色体系最优相机分辨率为12 MP,光圈f值为4.00 mm,感光度(photosensibility, ISO)值为800及快门速度为0.002 s;基于智能手机比色法检测尿酸最优条件下,尿酸浓度在0.075~7.500mmol/L范围内显现出良好的线性关系,工作曲线为Y1=-47.362X1+494.35(r2=0.9918),检出限为0.043μmol/L。在实际样品检测中,加标回收率在96.90%~112.81%之间,相对标准偏差均低于4.00%。结论 基于Fe3O4@Au模拟酶活性建立的智能手机比色检测体系,具有极高的灵敏度,良好的抗干扰性和稳定性,该研究成果将为尿酸等食品成分的分析检测提供一条新的渠道。

Preparation and Analysis of Fe3O4 Magnetic Nanoparticles Used as Targeted-drug Carriers

Fe3O4 磁性的 nanoparticles 被 FeCl3 · 6 H2O 和 FeCl2 · 4 H2O 的水的一起沉淀与铵氢氧化物的增加准备。为 Fe3O4 磁性的 nanoparticles 的准备的条件被优化，并且获得的 Fe3O4 磁性的 nanoparticles 借助于传播电子显微镜(TEM ) 系统地被描绘，动态激光散布分析器(DLS ) 和 X 射线衍射(XRD ) 。结果表明磁性的 nanoparticles 是立方的塑造并且散，与狭窄的大小分布和 11.4 的平均直径， nm.It 被发现在经由氨水的落下的率上的控制的解决方案的最适 PH 价值的同类的变化在大小分布起了一个关键作用。在磁场的产品的磁性的反应也被分析并且评估被四种铁磁物质生产的 32.6 mT 磁场被发现足够使离开铁磁物质 2 厘米远的 0.05 g Fe3O4 粉末的偶极矩激动的 carefully.A。在结论，有优秀性质的 Fe3O4 磁性的 nanoparticles 为在未来申请的目标药的磁性的搬运人是能干的。

Surface organic modification of Fe_3O_4 nanoparticles by silane-coupling agents

Fe3O4 nanoparticles were prepared by chemistry co-precipitation and the mean crystal size was 17.9 nm measured by XRD. After it had been treated by silane-coupling agents KH570, magnetic micro-spheres dispersed in organic medium glycol were gained and the mean size of Fe3O4 nanopowders was 33.7 nm. So it can be concluded that magnetic micro-sphere is made of a few Fe3O4 crystals. Many factors of modification were researched, such as the time of ball milling, the content of Fe3O4 and the content of KH570. The modification of Fe3O4 is relative to the time of ball milling, but the dominant function is affected by the content of Fe3O4 and KH570. When the content of Fe3O4 is known, there is a suitable content of KH570. Different content of Fe3O4 will make the different suitable content of KH570, but the range of latter is less than former, which is relative to the distribution of KH570 on Fe3O4 surface or in the solution.

Surface Organic Modification of Fe_3O_4 Magnetic Nanoparticles

The surface organic modification of Fe3O4 nanoparticles with silane coupling reagent KH570 was studied. The modified and unmodified nanoparticles were characterized by FT-IR, XPS and TEM. The spectra of FT-IR and XPS revealed that KH570 was coated onto the surface of Fe3O4 nanoparticles to get Fe-O- Si bond and an organic coating layer also was formed. Fe3O4 nanoparticles were spheres partly with mean size of 18,8 nm studied by TEM, which was consistent with the result 17.9 nm calculated by Scherrer＇s equation. KH570 was adsorbed on surface and formed chemistry bond to be steric hindrance repulsion which prevented nanoparticles from reuniting. Then glycol-based Fe3O4 magnetic liquids dispersed stably was gained.

Fabrication of Poly(γ-glutamic acid)-coated Fe3O4 Magnetic Nanoparticles and Their Application in Heavy Metal Removal

In this study, poly(γ-glutamic acid)-coated Fe3 O4 magnetic nanoparticles(γ-PGA/Fe3 O4 MNPs) were successfully fabricated using the co-precipitation method. Fe3 O4 MNPs were also prepared for comparison. The average size and specific surface area results reveal that γ-PGA/Fe3 O4 MNPs(52.4 nm, 88.41 m2·g 1) have smaller particle size and larger specific surface area than Fe3 O4 MNPs(62.0 nm, 76.83 m2·g 1). The γ-PGA/Fe3 O4 MNPs can remove over 99% of Cr3+, Cu2+and Pb2+, and over 77% of Ni2+in deionized water, much higher than γ-PGA and Fe3 O4 MNPs, attributed to the larger specific surface area of γ-PGA/Fe3 O4 MNPs. With the solution pH higher than 6.0, γ-PGA/Fe3 O4 MNPs demonstrate better removal activity. The adsorption isotherm of γ-PGA/Fe3 O4 MNPs for Cr3+fits the Freundlich model well, with the adsorption capacity of 24.60 mg·g 1. γ-PGA/Fe3 O4 MNPs are strongly attracted by permanent magnet, so it is easy to separate them completely from water. With their high efficiency for heavy metal removal and easier separation, γ-PGA/Fe3 O4 MNPs have great potential applications in water treatment.

Fe3O4 nanoparticles impregnated eggshell as a novel catalyst for enhanced biodiesel production

Biodiesel is a green fuel which can replace diesel while addressing various issues such as scarcity of hydrocarbon fuels and environmental pollution to an extent. The high production cost of biodiesel and the recovery of the catalyst after the transesterification process are the major challenges to be addressed in biodiesel production. In the present work, a cheap and promising solid base oxide catalyst was synthesized from chicken eggshell by calcination at 900 ℃ forming catalyst eggshells(CES) and was impregnated with the nanomagnetic material(Fe3O4) to obtain Fe3O4 loaded catalytic eggshell(CES–Fe3O4). Fe3O4 nanomaterials were synthesized by co-precipitation method and were loaded in catalytic eggshell by sonication, for better recovery of the catalyst after transesterification process. CES–Fe3O4 material was characterized by Thermogravimetric analysis, X-ray diffraction, Fourier transform infrared spectroscopy, a vibrating-sample magnetometer, Brunauer-Emmett-Teller, Dynamic light scattering, and Scanning electron microscopy. Biodiesel was synthesized by transesterification of Pongamia pinnata raw oil with 1:12 oil to methanol molar ratio and 2 wt% catalyst loading for 2 h at a temperature of 65 ℃ and yields were compared. The reusability of the catalyst was studied by the transesterification of the raw oil and its catalytic activity was found to be retained up to 7 cycles with a yield of 98%.

Loading Fe3O4 nanoparticles on paper-derived carbon scaffold toward advanced lithium-sulfur batteries

Lithium-sulfur batteries(LSBs) are regarded as a competitive next-generation energy storage device.However, their practical performance is seriously restricted due to the undesired polysulfides shuttling.Herein, a multifunctional interlayer composed of paper-derived carbon(PC) scaffold, Fe3O4 nanoparticles,graphene, and graphite sheets is designed for applications in LSBs. The porous PC skeleton formed by the interweaving long-fibers not only facilitates fast transfer of Li ions and electrons but also provides a physical barrier for the polysulfide shuttling. The secondary Fe3O4@graphene component can reduce the polarization, boost the attachment of polysulfides, and promote the charging-discharging kinetics. The outer graphitic sheets layers benefit the interfacial electrochemistry and the utilization of S-containing species.The efficient obstruction of polysulfides diffusion is further witnessed via in situ ultraviolet-visible characterization and first-principles simulations. When 73% sulfur/commercial acetylene black is used as the cathode, the cell exhibits excellent capacity retention with high capacities at 0.5 C for 1000 cycles and even up to 10 C for 500 cycles, an ultrahigh rate capability up to 10 C(478 m Ah g-1), and a high arealsulfur loading of 8.05 mg cm-2. The strategy paves the way for developing multifunctional composites for LSBs with superior performance.

Static magnetic field-assisted synthesis of Fe3O4 nanoparticles and their adsorption of Mn(Ⅱ) in aqueous solution

A facile method for synthesis of the magnetic Fe_3O_4 nanoparticles was introduced.Magnetic nanoparticles were prepared via co-precipitation method with(PMF) and without(AMF) 0.15 T static magnetic field.The effects of magnetic field on the properties of magnetic nanoparticles were studied by XRD,TEM,SEM,VSM and BET.The results showed that the magnetic field in the co-precipitation reaction process did not result in the phase change of the Fe_3O_4 nanoparticles but improved the crystallinity.The morphology of Fe_3O_4 nanoparticles was varied from random spherical particles to rod-like cluster structure.The VSM results indicated that the saturation magnetization value of the Fe_3O_4 nanoparticles was significantly improved by the magnetic field.The BET of Fe_3O_4nanoparticles prepared with the magnetic field was larger than the control by 23.5%.The batch adsorption experiments of Mn(Ⅱ) on the PMF and AMF Fe_3O_4 nanoparticles showed that the Mn(II) equilibrium capacity was increased with the pH value increased.At pH 8,the Mn(Ⅱ) adsorption capacity for the PMF and AMF Fe_3O_4 was reached at 36.81 and 28.36 mg·g^(-1),respectively.The pseudo-second-order model fitted better the kinetic models and the Freundlich model fitted isotherm model well for both PMF and AMF Fe_3O_4.The results suggested that magnetic nanoparticles prepared by the magnetic field presented a fairly good potential as an adsorbent for an efficient removal of Mn(Ⅱ) from aqueous solution.

Modification of Fe_3O_4 Magnetic Nanoparticles by L-dopa or Dopamine as an Enzyme Support

Fe3O4 magnetic nanoparticles were prepared by co-precipitation of Fe^2＋ and Fe^3＋ in an ammonia solution, and its size was about 36 nm measured by an atomic force microscope. Fe3O4 magnetic nanoparticles were modified by L-dopa or dopamine using sonication method. The analysis of FTIR clearly indicated the formation of Fe-O-C bond. Direct immobilization of trypsin （EC： 3.4.21.4） on Fe3O4 magnetic nanoparticles with L-dopa and dopamine spacer was investigated using glutaraldehyde as a coupling agent. No significant changes in the size and magnetic property of the three kinds of magnetic nanoparticles linked with or without trypsin were observed. The existence of the spacer molecule on magnetic nanoparticles could greatly improve the activity and the storage stability of bound trypsin through increasing the flexibility of enzyme and changing the microenvironment on nanoparticles surface compared to the naked magnetic nanoparticles.

Fe_3O_4 Magnetic Nanoparticles Modified Electrode as a Sensor for Determination of Nimesulide

A novel type of Fe3O4 nanoparticles modified glass carbon electrode（Fe3O4/GCE） was constructed and the electrochemical properties of N-（4-nitro-2-phenoxyphenyl）methanesulfonamide（nimesulide） were studied on the Fe3O4/GCE.In 0.4mol/L HAc-NaAc buffer solution（pH=5.0）,the electrode process of nimesulide was irreversible at bare GCE and Fe3O4/GCE.The Fe3O4/GCE exhibited a remarkable catalytic and enhancement effect on the reduction of nimesulide.The reduction peak potential of nimesulide shifted positively from-0.683 V at bare GCE to-0.625 V at Fe3O4/GCE,and the sensitivity was increased by ca.3 times.Some experimental conditions were optimized.The linear range between the peak current and the concentration of nimesulide was 2.6×10-6 ＂1.0×10-4mol/L（R=0.993） with a detection limit of 1.3×10-7mol/L.This method has been used to determine the content of nimesulide in medical tablets.The recovery was determined to be 96.9% ＂101.9% by means of standard addition method.The method is comparable to UV-Vis spectrometry.

Characteristics of magnetic Fe_3O_4 nanoparticles encapsulated with human serum albumin

Magnetic nanoparticles （Fe3O4） were prepared by chemical precipitation method using Fe 2+ and Fe 3+ salts with sodium hydroxide in the nitrogen atmosphere. Fe3O4 nanoparticles were coated with human serum albumin（HSA） for magnetic resonance imaging as contrast agent. Characteristics of magnetic particles coated or uncoated were carried out using scanning electron microscopy and X-ray diffraction. Zeta potentials, package effects and distributions of colloid particles were measured to confirm the attachment of HSA on magnetic particles. Effects of Fe3O4 nanoparticles coated with HSA on magnetic resonance imaging were investigated with rats. The experimental results show that the adsorption of HSA on magnetic particles is very favorable to dispersing of magnetic Fe3O4 particles, while the sizes of Fe3O4 particles coated are related to the molar ratio of Fe3O4 to HSA. The diameters of the majority of particles coated are less than 100nm. Fe3O4 nanoparticle coated with HSA has a good biocompatibility and low toxicity. This new contrast agent has some effects on the nuclear magnetic resonance imaging of liver and the lowest dosage is 20μmol/kg for the demands of diagnosis.

基于碳纳米管/L-半胱氨酸/Fe_3O_4@Au纳米复合材料的电流型甲胎蛋白免疫传感器的研究

将DMF(N,N-二甲基甲酰胺)分散的多壁碳纳米管(MWNT)修饰在金电极表面,再将修饰电极依次沉积纳米金和L-半胱氨酸(L-Cys),并通过半胱氨酸中的巯基吸附Fe3O4@Au纳米复合材料,再固载甲胎蛋白抗体(anti-AFP),以牛血清白蛋白(BSA)封闭非特异性吸附位点,构建了高灵敏、稳定的新型电流型甲胎蛋白免疫传感器。实验通过扫描透射电子显微镜(TEM)对DMF-MWNT和Fe3O4@Au复合纳米粒子进行了表征。在优化的实验条件下,此免疫传感器对甲胎蛋白抗原的检测范围为0.1～150μg/L,检出限为0.03μg/L。

基于Fe_3O_4@Au磁性纳米粒子修饰丝网印刷电极的微囊藻毒素免疫传感器研究

将核壳型Fe3O4@Au磁性纳米粒子修饰在丝网印刷工作电极表面,再通过纳米金和微囊藻毒素-(亮氨酸-精氨酸)抗体(anti-MCLR)之间的吸附作用,将抗体固定于电极表面,以牛血清白蛋白(BSA)封闭非特异性吸附位点,制得了检测MCLR的电流型免疫传感器。该传感器基于直接竞争的免疫分析模式,以辣根过氧化物酶偶联的微囊藻毒素(MCLR-HRP)为标记物,用差分脉冲伏安法检测微囊藻毒素,在优化的实验条件下,此免疫传感器响应的峰电流值与微囊藻毒素浓度在0.79～12.9μg/L范围内呈良好的线性关系,检测限为0.38μg/L。对实际水样进行了微囊藻毒素的加标回收实验,回收率在95%～107%之间。此免疫传感器具有测定速度快、灵敏高、携带方便等优点。

Synthesis and Characterization of Superparamagnetic Fe₃O₄@SiO₂Core-Shell Composite Nanoparticles

The Fe3O4@SiO2 composite nanoparticles were obtained from as-synthesized magnetite (Fe3O4) nanoparticles through the modified St?ber method. Then, the Fe3O4 nanoparticles and Fe3O4@SiO2 composite nanoparticles were characterized by means of X-ray diffraction (XRD), Raman spectra, scanning electron microscope (SEM) and vibrating sample magnetometer (VSM). Recently, the studies focus on how to improve the dispersion of composite particle and achieve good magnetic performance. Hence effects of the volume ratio of tetraethyl orthosilicate (TEOS) and magnetite colloid on the structural, morphological and magnetic properties of the composite nanoparticles were systematically investi-gated. The results revealed that the Fe3O4@SiO2 had better thermal stability and dispersion than the magnetite nanoparticles. Furthermore, the particle size and magnetic property of the Fe3O4@SiO2 composite nanoparticles can be adjusted by changing the volume ratio of TEOS and magnetite colloid.

基于Fe_3O_4@Au复合纳米粒子标记抗体的电化学免疫方法用于水体中大肠杆菌的检测

合成了Fe3O4@Au复合纳米粒子作为辣根过氧化酶标记抗体的载体,并将该复合纳米粒子标记物应用于电化学放大免疫分析.将电子媒介体硫堇聚合在玻碳电极表面,以纳米金作为固定大肠杆菌抗体的基底,通过辣根过氧化酶催化溶液中H2O2产生的电流信号来测定大肠杆菌.实验结果表明,该方法对水体中大肠杆菌检测的线性范围为50～1×105cfu/mL,检出限为20 cfu/mL.对过富集后的实际水样进行测定,该法结果表明,对水体中大肠杆菌的检测灵敏度达到2 cfu/mL.

PREPARATION AND MAGNETORHEOLOGICAL PROPERTIES OF AQUEOUS SUSPENSION BASED ON EMULSION DROPLETS CONTAINING Fe_3O_4 NANOPARTICLES

The Fe3O4 nanoparticles with mean size of 10 nm were prepared by chemical common precipitation . The factors influencing the size and shape of Fe3O4 nanoparticles such as the adding rate of NaOII to the mixed solution and the final pH of the solution were studied . The Fe3O4 based magnetorheological(MR) fluid was formed by adding surfactant . The rheological properties of this MR fluid were studied when the magnetic fields with different direction are applied. It has been found that the MR fluid has the magnetic anisotropy.

Formation of Uniform Oil-Soluble Fe_3O_4 Nanoparticles via Oil-Water Interface System

Nowadays,the novel oil water interface method has attracted a considerable attention owing to the advantages of mild reaction conditions,simple operation,low cost,and high efficiency.In this paper,uniform oil-soluble Fe_3O_4 nanoparticles(NPs) were synthesized by oil-water interface method from mixing iron tristearate of 0.067mol/L in cyclohexane with ferrous sulfate in water.The as-prepared products were characterized by X-ray diffraction(XRD),transmission electron microscopy(TEM),vibrating sample magnetometer(VSM),Fourier transform infrared spectroscopy(FT-IR) and thermogravimetric analyzer(TGA).TEM images and XRD profiles showed that the size of the oil-soluble products ranged in 1.7-6.9 nm.VSM indicated that the Fe_3O_4 NPs were superparamagetic.FT-IR and TGA proved that oleic acid was combined to the surface of Fe_3O_4 NPs closely.TEM images and XRD profiles revealed that the most suitable reaction concentration of NH_3·H_2O,oleic acid/water in volume,reaction temperature and reaction time were 4.5 mol/L,50:1 000,80℃ and 6 h,respectively.The formation mechanism of the nearly monodispersed Fe_3O_4 NPs was that the preformed Fe_3O_4 nuclei were capped by oleic acid as early as the nucleation occurred in oil-water interface and subsequently entered into oil phase to stop growing.

Synthesis and Characterization of Biomimetic Fe3O4/Coke Magnetic Nanoparticles Composite Material

A composite material（Fe3O4/Coke）using coke supported Fe3O4 magnetic nanoparticles was successfully prepared via an in-situ chemicaloxidation precipitation method and characterized by SEM,XRD,Raman,and FTIR.The results showed that the Fe3O4 nanoparticles existed steadily on the surface of coke,with better dispersing and smaller particle size.The catalytic ability of Fe3O4/Coke were investigatied by degrading p-nitrophenol（P-NP）.The results showed that the apparent rate constant for the P-NP at 1.0 g·L^-1 catalyst,30 mmol·L^-1 H2O2,pH=3.0,30 ℃ and the best ratio of Coke/Fe3O4 0.6,was evaluated to be 0.027 min^-1,the removalrate of CODCr was 75.47%,and the dissolubility of Fe was 2.42 mg·L^-1.Compared with pure Fe3O4,the catalytic ability of Fe3O4/Coke in the presence of H2O2 was greatly enhanced.And Fe3O4/Coke was a green and environmentalcatalyst with high catalytic activity,showing a good chemicalstability and reusability.

Magnetic field aligned orderly arrangement of Fe3O4 nanoparticles in CS/PVA/Fe3O4 membranes

The CS/PVA/Fe_3O_4 nanocomposite membranes with chainlike arrangement of Fe_3O_4 nanoparticles are prepared by a magnetic-field-assisted solution casting method. The aim of this work is to investigate the relationship between the microstructure of the magnetic anisotropic CS/PVA/Fe_3O_4 membrane and the evolved macroscopic physicochemical property. With the same doping content, the relative crystallinity of CS/PVA/Fe_3O_4-M is lower than that of CS/PVA/Fe_3O_4.The Fourier transform infrared spectroscopy（FT-TR） measurements indicate that there is no chemical bonding between polymer molecule and Fe_3O_4 nanoparticle. The Fe_3O_4 nanoparticles in CS/PVA/Fe_3O_4 and CS/PVA/Fe_3O_4-M are wrapped by the chains of CS/PVA, which is also confirmed by scanning electron microscopy（SEM） and x-ray diffraction（XRD）analysis. The saturation magnetization value of CS/PVA/Fe_3O_4-M obviously increases compared with that of non-magnetic aligned membrane, meanwhile the transmittance decreases in the UV-visible region. The o-Ps lifetime distribution provides information about the free-volume nanoholes present in the amorphous region. It is suggested that the microstructure of CS/PVA/Fe_3O_4 membrane can be modified in its curing process under a magnetic field, which could affect the magnetic properties and the transmittance of nanocomposite membrane. In brief, a full understanding of the relationship between the microstructure and the macroscopic property of CS/PVA/Fe_3O_4 nanocomposite plays a vital role in exploring and designing the novel multifunctional materials.