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1.
This study describes the synthesis and characterization of ethylenediaminetetraacetic acid (EDTA) functionalized magnetic nanoparticles of 20 nm in size – Fe3O4@SiO2‐EDTA – which were used as a novel magnetic adsorbent for Cd(II) and Pb(II) binding in aqueous medium. These nanoparticles were obtained in two‐stage synthesis: covering by tetraethyl orthosilicate and functionalization with EDTA derivatives. Nanoparticles were characterized using TEM, FT‐IR, and XPS methods. Metal ions were detected under optimized experimental conditions using Differential Pulse Anodic Stripping Voltammetry (DPASV) and Hanging Mercury Drop Electrode (HDME) techniques. We compared the ability of Fe3O4@SiO2‐EDTA to bind cadmium and lead in concentration of 553.9 μg L?1 and 647.5 μg L?1, respectively. Obtained results show that the adsorption rate of cadmium binding was very high. The equilibrium for Fe3O4@SiO2‐EDTA‐Cd(II) was reached within 19 min while for the Fe3O4@SiO2‐EDTA‐Pb(II) was reached within 25 minutes. About 2 mg of nanoparticles was enough to bind 87.5 % Cd(II) and 54.1 % Pb(II) content. In the next step the binding capacity of Fe3O4@SiO2‐EDTA nanoparticles was determined. Only 1.265 mg of Fe3O4@SiO2‐EDTA was enough to bind 96.14 % cadmium ions while 5.080 mg of nanoparticles bound 40.83 % lead ions. This phenomenon proves that the studied nanoparticles bind Cd(II) much better than Pb(II). The cadmium ions binding capacity of Fe3O4@SiO2‐EDTA nanoparticles decreased during storage in 0.5 M KCl solution. Two days of Fe3O4@SiO2‐EDTA storage in KCl solution caused the 32 % increase in the amount of nanoparticles required to bind 60 % of cadmium while eight‐days storage caused further increase to 328 %. The performed experiment confirmed that the storage of nanoparticles in solution without any surfactants reduced their binding capacity. The best binding capacity was observed for the nanoparticles prepared directly before the electrochemical measurements.  相似文献   

2.
Dyestuff textile wastewater treatment has become a research hotspot due to its high chroma, poor biodegradability, and low toxicity characteristics. In this paper, we have synthesized magnetic Fe3O4 and core‐shell Fe3O4@SiO2 materials by hydrothermal methods. These materials were characterized by XRD, TEM, N2 adsorption‐desorption and so on. These materials’ heterogeneous Fenton has been applied to dye wastewater treatment. Methylene blue was used as a typical target of dye wastewater. Decolorization ratios of methylene blue were determined by different nanostructure composites catalysts. A serious of results of study showed that decolorization ratios of magnetic nanoparticles and core‐shell composites arrived at above 90 % under the weakly acidic or neutral conditions and room temperature. When these catalysts were reused, the results show that Fe3O4@SiO2 materials were possessed with good cycle performance.  相似文献   

3.
Fe3O4 magnetic nanoparticles (MNPs) were functionalized by aminopropylsilane and reacted with aromatic aldehyde, and Fe3O4‐Si‐[CH2]3‐N=CH‐Aryl and Fe3O4‐Si‐(CH2)3‐NH‐CH2‐Aryl MNPs were prepared as novel magnetic nanocatalysts. Fourier transform infrared (FT‐IR), X‐ray diffraction (XRD), and scanning and transmission electron microscopy (SEM and TEM) were used to identify the MNPs. The catalytic activity of the MNPs was evaluated in the one‐pot synthesis of some novel poly‐substituted pyridine derivatives.  相似文献   

4.
The unique physicochemical properties of ordered mesoporous transition metal oxides have attracted more and more attention. The hydrolysis process of metal oxide precursors is difficult to control, and it is difficult to synthesize an ordered mesoporous transition metal oxide material using the conventional template method. Ordered mesoporous Pt/Fe3O4–CeO2 heterostructure gel materials with excellent catalytic properties were successfully prepared using aerogel technology and the chemical deposition method. The Pt/Fe3O4–CeO2 material was an n–n combined heterostructured semiconductor material which consisted of a magnetic Fe3O4 layer, a CeO2 core and Pt noble metal doped nanoparticles. A layer of Fe3O4 thin film was formed on the surface of ordered mesoporous Pt/CeO2 gel matrix material using the chemical deposition method. The intriguing heterostructural features could facilitate reactant diffusion and exposure of active sites which could enhance synergistic catalytic effects between the Pt nanoparticles and CeO2 nanoparticles. Compared with Pt/CeO2, the prepared Pt/Fe3O4–CeO2 showed enhanced catalytic activity in the reduction of 4-nitrophenol at room temperature. The catalytic activity of the heterostructure catalysts was systematically investigated using 4-nitrophenol reduction as a model reaction. The results showed that the Pt (0.1%)/Fe3O4–CeO2 sample exhibited the optimal catalytic performance toward catalytic reduction of 4-nitrophenol to 4-aminophenol. The study provided a method for the preparation of heterostructure nanocatalysts with high efficiency, which would be effective for application in various catalytic reactions.  相似文献   

5.
We describe the synthesis of a novel Fe3O4/amidoxime (AO)/Pd nanocatalyst by grafting of AO groups on Fe3O4 nanoparticles and subsequent deposition of Pd nanoparticles. Prior to grafting of AO, the 2‐cyanoethyl‐functionalized Fe3O4 nanoparticles prepared through combining 2‐cyanoethyltriethoxysilane and Fe3O4 were treated with hydroxylamine. The AO‐grafted Fe3O4 nanoparticles were then used as a platform for the deposition of Pd nanoparticles. The catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, scanning and transmission electron microscopies, vibrating sample magnetometry, wavelength‐ and energy‐dispersive X‐ray spectroscopies and inductively coupled plasma analysis. Fe3O4/AO/Pd is novel phosphine‐free recyclable heterogeneous catalyst for Sonogashira reactions. Interestingly, the novel catalyst could be recovered in a facile manner from the reaction mixture by applying an external magnet device and recycled seven times without any significant loss in activity. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

6.
《Electroanalysis》2017,29(12):2896-2905
In this study, immobilized hollow nanospheres of Fe3O4 with Palladium, Platinum and Gold nanoparticles (Fe3O4HNS‐PdPtAuNPs) was synthesized by hydrothermal and chemical reduction methods and characterized by various techniques such as field emission scanning electron microscopy, energy dispersive analysis of X‐rays and elemental mapping images. The electrocatalytic activity of the modified glassy carbon electrode (GCE) with Fe3O4HNS‐PdPtAuNPs (GCE/Fe3O4HNS‐PdPtAuNPs) toward methanol electrooxidation was investigated by cyclic voltammetry and chronoamperometry in 1 M NaOH solution. According to the results, Fe3O4HNS‐PdPtAuNPs catalyst demonstrated the highest efficiency for methanol electrooxidation in comparison with Fe3O4HNS‐PdNPs, Fe3O4HNS‐PtNPs, Fe3O4HNS‐PdAuNPs, Fe3O4HNS‐PtAuNPs and Fe3O4HNS‐PdPtNPs. The value of electron transfer coefficient (α ) and the ratio of current densities (If /Ib ) for methanol oxidation on the Fe3O4HNS‐PdPtAuNPs/GC catalyst were calculated 0.61 and 5.13, respectively. The reaction order was discovered to be 0.98 for CH3OH. A direct methanol fuel cell was developed with the suggested catalyst under several conditions.  相似文献   

7.
以十八烯为溶剂、乙酰丙酮铁为铁源,并在油酸、油胺的辅助作用下,通过热分解法成功合成了单分散Fe3O4纳米颗粒。讨论了实验参数如反应温度、表面活性剂的量和种类、溶剂、油酸、油胺对单分散Fe3O4纳米颗粒的尺寸及形貌的影响。利用X射线衍射(XRD)、透射电子显微镜(TEM)、选区电子衍射(SAED)和高分辨透射电子显微镜(HRTEM)对所得产物的物相、结构、尺寸和形貌进行了表征分析。通过振动样品磁强计(VSM)表征产物磁性能,表明在室温下,Fe3O4纳米颗粒的饱和磁化强度(Ms)和矫顽力(Hc)分别为74.0 emu/g,72.6 Oe。  相似文献   

8.
A strategy has been developed for the synthesis, characterization and catalysis of magnetic Fe3O4/P(GMA‐EGDMA)‐NH2/HPG‐COOH‐Pd core‐shell structure supported catalyst. The P(GMA‐EGDMA) polymer layer was coated on the surface of hollow magnetic Fe3O4 microspheres through the effect of KH570. The core‐shell magnetic Fe3O4/P(GMA‐EGDMA) modified by ‐NH2 could be grafted with HPG. Then, the hyperbranched glycidyl (HPG) with terminal ‐OH were modified by ‐COOH and adsorbed Pd nanoparticles. The hyperbranched polymer layer not only protected the Fe3O4 magnetic core from acid–base substrate corrosion, but also provided a number of functional groups as binding sites for Pd nanoparticles. The prepared catalyst was characterized by UV–vis, TEM, SEM, FTIR, TGA, ICP‐OES, BET, XRD, DLS and VSM. The catalytic tests showed that the magnetic Fe3O4/P(GMA‐EGDMA)‐NH2/HPG‐COOH‐Pd catalyst had excellent catalytic performance and retained 86% catalytic efficiency after 8 consecutive cycles.  相似文献   

9.
In this time researchers make a great efforts to develop new hybrid nanoparticles for medical and pharmaceutical applications. Fe3O4‐Au hybrid heterodimers have been prepared with superior properties for various claims. Unfortunately, Fe3O4‐Au heterodimers are not stable in the physiological medium. In this study, we employed the albumin macromolecules as a stabilizer of Fe3O4‐Au hybrid nanoparticles (noted as Fe3O4‐Au‐BSA hybrid nanoparticles). After characterization of synthesized nanoparticles by FTIR, UV–Vis, TEM, DLS, DSC, VSM and XRD techniques, the in vitro and in vivo biocompatibility of these nanoparticles were also evaluated. We encountered with an amazing result which confirmed nanoparticles could be stabilized by linking the BSA on the surface of Fe3O4‐Au heterodimers. Also, intravenous injection of Fe3O4‐Au‐BSA hybrid nanoparticles up to 400 mg/kg to Balb C mice show that these nanoparticles were non‐toxic. The biocompatibility and stereological study had been performed for more than 30 days after nanoparticles administration, using hystomorphometric analysis. Remarkably, to the best of our knowledge, it was the first time the biocompatibility and biodegradability of Fe3O4‐Au were studied and evaluated by stereological technique. Further promotion and biomedical usage of this type of hybrid nanoparticles are underway in our laboratory.  相似文献   

10.
Polyethersulfone (PES) and poly(1‐vinylpyrrolidone) (PVP) were used to prepare ultrafiltration membranes with grafted Fe3O4 magnetic nanoparticles (PVP‐g‐Fe3O4@SiO2). The structure of synthesized PVP‐g‐Fe3O4@SiO2 was confirmed by FT‐IR and SEM analysis. Physical properties of blend membranes such as thermal resistance, Tensile strength, water uptake, and hydrophilicity were also investigated. Blended membranes of PES/PVP‐g‐Fe3O4@SiO2 have exhibited higher thermal resistance due to increasing the modified nanoparticle content. The hydrophilicity of the synthesized PES/PVP‐g‐Fe3O4@SiO2 membranes also improved by increasing the PVP‐g‐Fe3O4@SiO2 content. As expected, increasing the hydrophilicity of blended membrane, caused enhancement of fouling resistance in membranes. Results showed that the content of PVP‐g‐Fe3O4@SiO2 has different effects on the properties of synthesized composite membranes. Despite increasing the content of PVP‐g‐Fe3O4@SiO2 has a negative effect on elongation, positive effects on maximum stress was observed. Moreover, the water uptake of synthesized membranes was significantly enhanced in comparison to other similar studies.  相似文献   

11.
Novel Pd nanoparticles were prepared in five successive stages: 1) preparation of the Fe3O4 magnetic nanoparticles (Fe3O4 MNPs), 2) coating of Fe3O4 MNPs with SiO2 (Fe3O4@SiO2), 3) functionalization of Fe3O4@SiO2 with 3‐chloropropyltrimethoxy‐ silane (CPTMS) ligand (Fe3O4@SiO2@CPTMS), 4) further functionalization with 3,5‐diamino‐1,2,4‐triazole (DAT) ligand (Fe3O4@SiO2@CPTMS @DAT), and 5) the complexation of Fe3O4@SiO2@CPTMS@DAT with PdCl2 (Fe3O4@SiO2@CPTMS@ DAT@Pd). Then, the obtained Pd nano‐catalyst characterized by different methods such as the elemental analysis (CHN), FT‐IR, XRD, EDX, SEM, TEM, TG‐DTA and VSM. Finally, the Pd catalyst was applied for the synthesis of various 2‐imino‐3‐phenyl‐2,3‐dihydrobenzo[d]oxazol‐5‐ols.  相似文献   

12.
This study reports the structural and spectroscopic characterization of a novel metal organic compound formulated as [Fe (bpy)3] [Fe (dipic)2]2.7H2O ( 1 ) (dipic = pyridine‐2,6‐dicarboxylate and bpy = 2,2‐bipyridine). 1 was investigated by elemental analysis, FT‐IR spectroscopy, powder X‐ray diffraction and single crystal X‐ray diffraction (SC‐XRD), which revealed a triclinic structure of expected composition. Thermal degradation of 1 was also investigated. Complex 1 was used as a precursor to prepare superparamagnetic nanoparticles of Fe3O4 by thermal analysis. The obtained Fe3O4 was characterized by Fourier transformed infrared spectroscopy (FT‐IR), powder X‐ray diffraction (XRD) and scanning electron microscopy (SEM). Fe3O4 nanoparticles were used as a nano‐adsorbent to remove Cd2+ from water at room temperature. The results showed that this nano‐adsorbent is effective in removing Cd2+ from contaminated water sources, and that the maximal effectivity of adsorption occurs at pH = 6. Magnetic measurements of complex 1 and Fe3O4 nanoparticles at room temperature revealed paramagnetic and superparamagnetic behavior, respectively.  相似文献   

13.
In this study, a novel multifunctional poly(arylene ether nitriles)(PEN)/carbon nanotubes/Fe3O4 nanocomposite with high tensile strength, magnetic, and electrical properties was investigated. First, we synthesized the monodisperse Fe3O4 nanoparticles on the surface of the multiwalled carbon nanotubes and then the hybrid material was compounded with PEN through the solution‐casting method. The SEM and TEM images indicated that the monodisperse Fe3O4 nanoparticles, with the diameters of 70∼80 nm, were self‐assembled along CNTs via the covalent bond method, which was confirmed by FTIR and XRD. The results of tensile properties showed that the tensile strength and modulus reached their highest values at the CNTs/Fe3O4 loading content of 1 wt % and both were greatly enhanced after heat treatment. Electrical conductivity of the polymer was dramatically enhanced at the low loading level of CNTs/Fe3O4; the electrical percolation of was in the range of 5∼8 wt % of CNTs/Fe3O4. The magnetic study showed that the saturation magnetization (Ms) of PEN/CNTs/Fe3O4 nanocomposites increased with the increase of CNTs/Fe3O4 loading content, and the coercive force (Hc) of the nanocomposite was independent of the CNTs/Fe3O4 content. © 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2011  相似文献   

14.
Novel magnetic titanium dioxide nanoparticles decorated with methyltrimethoxysilane (Fe3O4@TiO2‐MTMOS) were successfully fabricated via a sol–gel method at room temperature. The synthesized material was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, thermogravimetric analysis and vibrating sample magnetometry. The removal efficiency of the adsorbent was evaluated through the adsorption of methylene blue (MB) dye from water samples. The adsorption isotherm and kinetics were evaluated using various models. The Langmuir model indicated a high adsorption capacity (11.5 mg g?1) of Fe3O4@TiO2‐MTMOS. The nanocomposite exhibited high removal efficiency (96%) and good regeneration (10 times) compared to Fe3O4 and Fe3O4@TiO2 at pH = 9.0. Based on the adsorption mechanism, electrostatic interaction plays a main role in adsorption since MB dye is cationic in nature at pH = 9, whereas the adsorbent acquired an anionic nature. The newly synthesized Fe3O4@TiO2‐MTMOS can be used as a promising material for efficient removal of MB dye from aqueous media.  相似文献   

15.
In this study, the synthesis of sulfonic acid supported on ferrite–silica superparamagnetic nanoparticles (Fe3O4@SiO2@SO3H) as a nanocatalyst with large density of acidic groups is suggested. This nanocatalyst was prepared in three steps: preparation of colloidal iron oxide magnetic nanoparticles (Fe3O4 MNPs), coating of silica on Fe3O4 MNPs (Fe3O4@SiO2) and incorporation of sulfonic acid as a functional group on the surface of Fe3O4@SiO2 nanoparticles (Fe3O4@SiO2@SO3H). The properties of the prepared magnetic nanoparticles were characterized using transmission electron microscopy, infrared spectroscopy, vibrating sample magnetometry, X‐ray diffraction and thermogravimetric analysis. Finally, the applicability of the synthesized magnetic nanoparticles was tested as a heterogeneous solid acid nanocatalyst for one‐pot synthesis of diindolyloxindole derivatives in aqueous medium. Oxindole derivatives were produced by the coupling of indole and isatin compounds with good to high yields (60–98%). Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

16.
In this research, the nanocomposite of multiwalled carbon nanotubes and magnetic metal oxide nanoparticles (Fe3O4/MWCNTs), as enzyme mimetic, was synthesized using an in situ chemical reduction method. The structure, composition and morphology of the prepared Fe3O4/MWCNT nanocomposite materials were characterized using X‐ray diffraction, FT‐IR and scanning electron microscopy with energy dispersive X‐ray spectroscopy, respectively. The magnetic properties of the nanocomposite were investigated by the vibrating sample magnetometer. A colorimetric system involving nanozyme, phenol/4‐aminoantipyrine and H2O2 was utilized for the determination of peroxidase mimetic catalytic assay. The obtained results confirmed that the synthesis of Fe3O4/MWCNTs nanostructures was successful. It was found that Fe3O4/MWCNTs nanohybrid exhibited peroxidase‐like activity without any pH limitation. Colorimetric data demonstrated that the prepared nanocatalyst had higher catalytic activity toward H2O2 than MWCNTs. The kinetic parameters of the nanozyme, Km and Vmax, were estimated to be 8.3 mm and 1.4 mm min?1, respectively. The Fe3O4/MWCNTs nanostructures were also successfully applied for glucose detection. In addition, peroxidase‐like activity of the nanozyme increased in the presence of butyl‐imidazolium bromide ionic liquid. These biomimetic catalysts have some advantages, such as simplicity, stability, reusability and cost effectiveness, which makes them great candidates to be used in various fields of biotechnology applications.  相似文献   

17.
Graphene‐Fe3O4 nanoparticles were prepared using one‐step solvothermal method and characterized by X‐ray diffraction, FTIR spectroscopy, scanning electron microscopy, and vibrating sample magnetometry. The results demonstrated that Fe3O4 nanoparticles were homogeneously anchored on graphene nanosheets. The as‐synthesized graphene‐Fe3O4 nanoparticles were employed as sorbent for magnetic solid‐phase extraction of sulfonamides in milk prior to capillary electrophoresis analysis. The optimal capillary electrophoresis conditions were as follows: 60 mmol/L Na2HPO4 containing 2 mmol/L ethylenediaminetetraacetic acid disodium salt and 24% v/v methanol as running buffer, separation voltage of 14 kV, and detection wavelength of 270 nm. The parameters affecting extraction efficiency including desorption solution, the amount of graphene‐Fe3O4 nanoparticles, extraction time, and sample pH were investigated in detail. Under the optimal conditions, good linearity (5–200 μg/L) with correlation coefficients ≥0.9910 was obtained. The limits of detection were 0.89–2.31 μg/L. The relative standard deviations for intraday and interday analyses were 4.9–8.5 and 4.0–9.0%, respectively. The proposed method was successfully applied to the analysis of sulfonamides in milk samples with recoveries ranging from 62.7 to 104.8% and relative standard deviations less than 10.2%.  相似文献   

18.
A novel magnetic binary‐metal‐oxide‐coated nanocataly composing of a hollow Fe3O4 core and CeO2‐La2O3 shells with Au nanoparticles encapsulated has been created in this work. The structural features of catalysts were characterized by several techniques, including SEM, TEM, UV‐vis, FTIR, XRD, XPS and TGA analyses. After the coating of CeO2‐La2O3 layer, CeO2‐La2O3/Au/C/Fe3O4 microspheres showed a superior thermal stability and catalytic reactivity compared with a pure CeO2 or La2O3 layer. Accompanied by the burning of carbon layer, the specific surface could be increased by the formation of double‐shelled structure. Besides, the desired samples could be separated by magnet, implying the superior recycle performance. Using the reduction of 4‐nitrophenol by NaBH4 as a model reaction, the microspheres exhibited highly reusability, superior catalytic activity, thermal stability, which are attributed to the unique double‐shelled structure of the support, uniform distribution of Au nanoparticles, the highly thermal stability of CeO2‐La2O3 layer and mixed oxide synergistic effect. As a consequence, the unique nanocatalyst will open a promising way in the fabrication of the double‐shelled hollow binary‐metal‐oxide materials for future research and has great potential in other applications.  相似文献   

19.
A novel chiral magnetic nanocatalyst was prepared by the surface modification of Fe3O4 magnetic nanoparticles (MNPs) with a chloropropylsilane and further by arginine to form Fe3O4@propylsilan‐arginine (Fe3O4@PS‐Arg). After the structural confirmation of Fe3O4@PS‐Arg synthesized MNPs by Fourier transform‐infrared, X‐ray diffraction, field emission‐scanning electron microscopy, transmission electron microscopy, vibrating‐sample magnetometry and thermogravimetric analyses, their catalytic activity was evaluated for one‐pot enantioselective synthesis of 3‐amino‐1‐aryl‐1H‐benzo[f]chromene‐2‐carbonitrile derivatives. The results showed that in the presence of 0.07 g Fe3O4@PS‐Arg nanocatalyst and ethanol as solvent, the best reaction yield (96%) was obtained in the least time (5 min). Easy operation, reusability and stability, short reaction time, high reaction yields and good enantioselectivity are the major advantages of the newly synthesized nanocatalyst. Also, this study provides a novel strategy for further research and investigation on the synthesis of new reusable enantioselective catalysts and chiral compounds.  相似文献   

20.
In this study, two types of magnetic polyurethane (PU) elastomer nanocomposites using polycaprolactone (PCL) and polytetramethylene glycol (PTMG) as polyols were synthesized by incorporating thiodiglycolic acid surface modified Fe3O4 nanoparticles (TSM‐Fe3O4) into PU matrices through in situ polymerization method. TSM‐Fe3O4 nanoparticles were prepared using in situ coprecipitation method in alkali media and were characterized by X‐ray diffraction, Fourier Transform Infrared Spectrophotometer, Transmission Electron Microscopy, and Vibrating Sample Magnetometer. The effects of PCL and PTMG polyols on the properties of the resultant PUs were studied. The morphology and dispersion of the nanoparticles in the magnetic nanocomposites were studied by Scanning Electron Microscope. It was observed that dispersion of nanoparticles in PTMG‐based magnetic nanocomposite was better than PCL‐based magnetic nanocomposite. Furthermore, the effect of polyol structure on thermal and mechanical properties of nanocomposite was investigated by Thermogravimetric Analysis and Dynamic Mechanical Thermal Analysis. A decrease in the thermal stability of magnetic nanocomposites was found compared to pure PUs. Furthermore, DMTA results showed that increase in glass transition temperature of PTMG‐based magnetic nanocomposite is higher than PCL‐based magnetic nanocomposite, which is attributed to better dispersion of TSM‐Fe3O4 nanoparticles in PTMG‐based PU matrix. Additionally, magnetic nanocomposites exhibited a lower level of hydrophilicity compared to pure PUs. These observations were attributed to the hydrophobic behavior of TSM‐Fe3O4 nanoparticles. Moreover, study of fibroblast cells interaction with magnetic nanocomposites showed that the products can be a good candidate for biomedical application. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

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