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1.
Magnetic core–shell titanium dioxide nanoparticles (Fe3O4@SiO2@TiO2) were applied for the efficient preparation of 1,2,4,5‐tetrasubstituted imidazole derivatives by the one‐pot multi‐component condensation of benzil with aldehydes, primary amines and ammonium acetate under solvent‐free conditions. The catalyst was synthesized and studied using several techniques including X‐ray diffraction, transmission electron microscopy, field‐emission scanning electron microscopy and energy‐dispersive X‐ray spectroscopy. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

2.
Iron oxide (Fe3O4) magnetic nanoparticles as movable cores were used to synthesize yolk–shell nanoparticles with pH‐responsive shell composed of ethylene glycol dimethacrylate (EGDMA)‐crosslinked poly(acrylic acid) (PAA) via two different routes. In the first more common route, Fe3O4 nanoparticles were coated with silica layer via the Stöber process to yield Fe3O4@SiO2 core–shell nanoparticles, subsequently used as seeds in the distillation precipitation copolymerization of AA and EGDMA to yield Fe3O4@SiO2@P(AA‐EGDMA). The silica layer was selectively removed through alkali etching to yield Fe3O4@air@P(AA‐EGDMA). In the second route, Fe3O4 nanoparticles without any stabilization were used as seeds in the distillation precipitation copolymerization of AA and EGDMA to yield Fe3O4@P(AA‐EGDMA) core–shell nanoparticles. The nanoparticles were subsequently dispersed in acidic medium of pH = 2. Yolk–shell Fe3O4@air@P(AA‐EGDMA) nanoparticles were formed through deswelling of crosslinked PAA because of protonation of carboxyl groups at low pH values. Various techniques were utilized to investigate the characteristics of the synthesized core–shell nanoparticles. Formation of yolk–shell nanostructure was observed for both synthesis routes, namely etching of silica layer and deswelling approaches, from vibrating sample magnetometry and transmission electron microscopy results. Both types of nanoparticles showed pH‐responsive behaviour, i.e. decrease in absorption with increase in pH, as examined using UV–visible spectroscopy.  相似文献   

3.
A copper catalyst has been explored as an efficient and recyclable catalyst to effect Sonogashira and Suzuki cross‐coupling reactions. After modification of 2‐(((piperazin‐1‐ylmethyl)imino)methyl)phenol (PP) on the surface of amorphous silica‐coated iron oxide (Fe3O4@SiO2@Cl) magnetic core–shell nanocomposite, copper(II) chloride was employed to synthesize the Fe3O4@SiO2@PP‐Cu catalyst, affording a copper loading of 1.52 mmol g−1. High yield, low reaction times, non‐toxicity and recyclability of the catalyst are the main merits of this protocol. The catalyst was characterized using Fourier transform infrared, X‐ray photoelectron, energy‐dispersive X‐ray and inductively coupled plasma optical emission spectroscopies, X‐ray diffraction, scanning and transmission electron microscopies, and vibrating sample magnetometry.  相似文献   

4.
Magnetic Fe3O4/SiO2 composite core–shell nanoparticles were synthesized, characterized, and applied for the surfactant‐assisted solid‐phase extraction of five benzodiazepines diazepam, oxazepam, clonazepam, alprazolam, and midazolam, from human hair and wastewater samples before high‐performance liquid chromatography with diode array detection. The nanocomposite was synthesized in two steps. First, Fe3O4 nanoparticles were prepared by the chemical co‐precipitation method of Fe(III) and Fe(II) as reaction substrates and NH3/H2O as precipitant. Second, the surface of Fe3O4 nanoparticles was modified with shell silica by Stober method using tetraethylorthosilicate. The Fe3O4/SiO2 composite were characterized by X‐ray diffraction, scanning electron microscopy, Fourier transform infrared spectroscopy, and vibrating sample magnetometry. To enhance their adsorptive tendency toward benzodiazepines, cetyltrimethylammonium bromide was added, which was adsorbed on the surface of the Fe3O4/SiO2 nanoparticles and formed mixed hemimicelles. The main parameters affecting the efficiency of the method were thoroughly investigated. Under optimum conditions, the calibration curves were linear in the range of 0.10–15 μgmL?1. The relative standard deviations ranged from 2.73 to 7.07%. The correlation coefficients varied from 0.9930 to 0.9996.  相似文献   

5.
Urea was successfully immobilized on the surface of chloropropyl‐modified Fe3O4@SiO2 core–shell magnetic nanoparticles, then supported by MgBr2 and acts as a unique catalyst for oxidation of benzylic alcohols to aldehydes and ketones, and ortho‐formylation of phenols to salicylaldehydes. The prepared catalyst was characterized by FT‐IR, transmission electron microscopy, scanning electron microscopy, X‐ray powder diffraction, dispersive X‐ray spectroscopy, CHN and TGA. It was found that Fe3O4@SiO2 ~ urea/MgBr2 showed higher catalytic activity than homogenous MgBr2, and could be reused several times without significant loss of activity.  相似文献   

6.
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   

7.
A facile and efficient strategy for the synthesis of hierarchical yolk–shell microspheres with magnetic Fe3O4 cores and dielectric TiO2 shells has been developed. Various Fe3O4@TiO2 yolk–shell microspheres with different core sizes, interstitial void volumes, and shell thicknesses have been successfully synthesized by controlling the synthetic parameters. Moreover, the microwave absorption properties of these yolk–shell microspheres, such as the complex permittivity and permeability, were investigated. The electromagnetic data demonstrate that the as‐synthesized Fe3O4@TiO2 yolk–shell microspheres exhibit significantly enhanced microwave absorption properties compared with pure Fe3O4 and our previously reported Fe3O4@TiO2 core–shell microspheres, which may result from the unique yolk–shell structure with a large surface area and high porosity, as well as synergistic effects between the functional Fe3O4 cores and TiO2 shells.  相似文献   

8.
A simple method, air‐assisted dispersive micro‐solid‐phase extraction‐based supramolecular solvent was developed for the preconcentration of tramadol in biological samples prior to gas chromatography–flame ionization detection. A new type of carrier liquid, supramolecular solvent based on a mixture of 1‐dodecanol and tetrahydrofuran was combined with layered double hydroxide coated on a magnetic nanoparticle (Fe3O4@SiO2@Cu–Fe–LDH). The supramolecular solvent was injected into the solution containing Fe3O4@SiO2@Cu–Fe–LDH in order to provide high stability and dispersion of the sorbent without any stabilizer agent. Air assisted was applied to enhance the dispersion of the sorbent and solvent. A number of analytical techniques such as Fourier transform‐infrared spectrometry, field emission scanning electron microscope, energy‐dispersive X‐ray spectroscopy and X‐ray diffraction measurements were applied to assess the surface chemical characteristics of Fe3O4@SiO2@Cu–Fe–LDH nanoparticles. The effects of important parameters on the extraction recovery were also investigated. Under optimized conditions, the limits of detection and quantification were obtained in the range of 0.9–2.4 and 2.7–7.5 μg L?1 with preconcentration factors in the range of 450–472 in biological samples. This method was used for the determination of tramadol in biological samples (plasma, urine and saliva samples) with good recoveries.  相似文献   

9.
A new method is applied to prepare stable aqueous dispersion of magnetic iron oxide nanoparticles (MNPs) by biocompatible maleate polymers. Fe3O4 magnetic core–shell nanoparticles are obtained via forming an inclusion complex between carboxylic acid groups of maleated biocompatible polymers shell and Fe3O4 MNPs core surface. Maleate polymers are synthesized via esterification of poly(ethylene glycol), poly(vinyl alcohol) and starch with maleic anhydride (MA). The Fe3O4 magnetic core–shell nanoparticles are characterized by Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy and vibrating sample magnetometer. The obtained magnetic core–shell nanoparticles exhibit superparamagnetic property and reveal long‐term aqueous stability. This work represents a valid methodology to produce highly stable aqueous dispersion of Fe3O4 MNPs ferrofluids which can be expected to have great potential as contrast agent for magnetic resonance imaging. Furthermore, the shell composition of biocompatible maleate polymers with double bond of MA as crosslinker agent allows the polymerization with other monomers to design preferred drug delivery systems. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

10.
An effective one‐pot, convenient process for the synthesis of 1‐ and 5‐substituted 1H‐tetrazoles from nitriles and amines is described using1,4‐dihydroxyanthraquinone–copper(II) supported on Fe3O4@SiO2 magnetic porous nanospheres as a novel recyclable catalyst. The application of this catalyst allows the synthesis of a variety of tetrazoles in good to excellent yields. The preparation of the magnetic nanocatalyst with core–shell structure is presented by using nano‐Fe3O4 as the core, tetraethoxysilane as the silica source and poly(vinyl alcohol) as the surfactant, and then Fe3O4@SiO2 was coated with 1,4‐dihydroxyanthraquinone–copper(II) nanoparticles. The new catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscopy, field emission scanning electron microscopy, dynamic light scattering, thermogravimetric analysis, vibration sample magnetometry, X‐ray photoelectron spectroscopy, nitrogen adsorption–desorption isotherm analysis and inductively coupled plasma analysis. This new procedure offers several advantages such as short reaction times, excellent yields, operational simplicity, practicability and applicability to various substrates and absence of any tedious workup or purification. In addition, the excellent catalytic performance, thermal stability and separation of the catalyst make it a good heterogeneous system and a useful alternative to other heterogeneous catalysts. Also, the catalyst could be magnetically separated and reused six times without significant loss of catalytic activity. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

11.
Octakis[3‐(3‐aminopropyltriethoxysilane)propyl]octasilsesquioxane (APTPOSS) as a polyhedral oligomeric silsesquioxane derivative was prepared and used as a pioneer reagent to obtain a novel core–shell composite using magnetic iron oxide nanoparticles as the core and the inorganic–organic hybrid polyhedral oligomeric silsesquioxane as the shell. Fe3O4@SiO2/APTPOSS were confirmed using Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, dynamic light scattering, thermogravimetric analysis, X‐ray diffraction and vibrating sample magnetometry. The inorganic–organic hybrid polyhedral oligomeric silsesquioxane magnetic nanoparticles were used as an efficient new heterogeneous catalyst for the one‐pot three‐component synthesis of 1,3‐thiazolidin‐4‐ones under solvent‐free conditions. Moreover, these nanoparticles could be easily separated using an external magnet and then reused several times without significant loss of catalytic activity. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

12.
A yolk–shell-structured sphere composed of a superparamagnetic Fe3O4 core and a carbon shell (Fe3O4@HCS) was etched from Fe3O4@SiO2@carbon by NaOH, which was synthesized through the layer-by-layer coating of Fe3O4. This yolk–shell composite has a shell thickness of ca. 27 nm and a high specific surface area of 213.2 m2 g?1. Its performance for the magnetic removal of tetracycline hydrochloride from water was systematically examined. A high equilibrium adsorption capacity of ca. 49.0 mg g?1 was determined. Moreover, the adsorbent can be regenerated within 10 min through a photo-Fenton reaction. A stable adsorption capacity of 44.3 mg g?1 with a fluctuation <10% is preserved after 5 consecutive adsorption–degradation cycles, demonstrating its promising application potential in the decontamination of sewage water polluted by antibiotics.  相似文献   

13.
SiO2‐coated Fe3O4 (Fe3O4@SiO2) nanocomposites were prepared by sol–gel method, and the anticorrosion performance of composite coatings was discussed. The structure of the Fe3O4@SiO2 nanocomposites was verified through Fourier transform infrared, X‐ray diffraction, and scanning electron microscopy. Composite epoxy coatings with same concentrations of Fe3O4 and Fe3O4@SiO2 were measured by scanning electron microscopy contact angle meter. More importantly, the Fe3O4@SiO2 nanocomposites not only obtained a homogeneous dispersion and compatibility in epoxy resin but also exhibited an obvious superiority in enhancing the anticorrosion performance of epoxy coatings. Furthermore, the anticorrosion mechanism of Fe3O4@SiO2/epoxy composite coating was tentatively discussed. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

14.
A protein imprinting approach for the synthesis of core–shell structure nanoparticles with a magnetic core and molecularly imprinted polymer (MIP) shell was developed using a simple distillation–precipitation polymerization method. In this work, Fe3O4 magnetic nanoparticles were first synthesized through a solvothermal method and then were conveniently surface‐modified with 3‐(methacryloyloxy)propyltrimethoxylsilane as anchor molecules to donate vinyl groups. Next a high‐density MIP shell was coated onto the surface of the magnetic nanoparticles by the copolymerization of functional monomer acrylamide (AAm), cross‐linking agent N,N′‐methylenebisacrylamide (MBA), the initiator azodiisobutyronitrile (AIBN), and protein in acetonitrile heated at reflux. The morphology, adsorption, and recognition properties of the magnetic molecularly imprinted nanoparticles were investigated by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), vibrating sample magnetometer (VSM), and rebinding experiments. The resulting MIP showed a high adsorption capacity (104.8 mg g?1) and specific recognition (imprinting factor=7.6) to lysozyme (Lyz). The as‐prepared Fe3O4@Lyz‐MIP nanoparticles with a mean diameter of 320 nm were coated with an MIP shell that was 20 nm thick, which enabled Fe3O4@Lyz‐MIP to easily reach adsorption equilibrium. The high magnetization saturation (40.35 emu g?1) endows the materials with the convenience of magnetic separation under an external magnetic field and allows them to be subsequently reused. Furthermore, Fe3O4@Lyz‐MIP could selectively extract a target protein from real egg‐white samples under an external magnetic field.  相似文献   

15.
The core–shell structure Fe3O4/SiO2 magnetic microspheres were prepared by a sol–gel method, and immobiled with iminodiacetic acid (IDA) as metal ion affinity ligands for protein adsorption. The size, morphology, magnetic properties and surface modification of magnetic silica nanospheres were characterized by various modern analytical instruments. It was shown that the magnetic silica nanospheres exhibited superparamagnetism with saturation magnetization values of up to 58.1 emu/g. Three divalent metal ions, Cu2+, Ni2+ and Zn2+, were chelated on the Fe3O4@SiO2–IDA magnetic microspheres to adsorb lysozyme. The results indicated that Ni2+‐chelating magnetic microspheres had the maximum adsorption capacity for lysozyme of 51.0 mg/g, adsorption equilibrium could be achieved within 60 min and the adsorbed protein could be easily eluted. Furthermore, the synthesized Fe3O4@SiO2–IDA–Ni2+ magnetic microspheres were successfully applied for selective enrichment lysozyme from egg white and His‐tag recombinant Homer 1a from the inclusion extraction expressed in Escherichia coli. The result indicated that the magnetic microspheres showed unique characteristics of high selective separation behavior of protein mixture, low nonspecific adsorption, and easy handling. This demonstrates that the magnetic silica microspheres can be used efficiently in protein separation or purification and show great potential in the pretreatment of the biological sample. Copyright © 2015 John Wiley & Sons, Ltd.  相似文献   

16.
A novel heterogenized organometallic catalyst was synthesized by coordinating palladium with polyvinyl alcohol‐functionalized Fe3O4@SiO2 nanospheres. This novel catalyst was characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, transmission electron microscope, field emission scanning electron microscope, dynamic light scattering, UV–vis spectroscopy, X‐ray photoelectron spectroscopy, energy dispersive X‐ray analysis, thermogravimetric analysis and inductively coupled plasma analysis. The prepared palladium nanoparticles supported on polyvinyl alcohol functionalized Fe3O4@SiO2 nanoparticles were successfully applied as a magnetically recyclable catalyst in Heck and Sonogashira coupling reactions in water. They showed remarkable activity toward aryl halides (I, Br, Cl) using very low palladium loading in excellent yields and demonstrated high TONs (mmol of product per mmol of catalyst). Also, the catalyst could be magnetically separated and reused seven times without any appreciable loss of catalytic activity.  相似文献   

17.
Magnetic mesoporous silica was prepared via embedding magnetite nanoparticles between channels of mesoporous silica (SBA‐15). The prepared composite (Fe3O4@SiO2‐SBA) was then reacted with 3‐chloropropyltriethoxysilane, sodium imidazolide and 2‐bromopyridine to give 3‐(pyridin‐2‐yl)‐1H‐imidazol‐3‐iumpropyl‐functionalized Fe3O4@SiO2‐SBA as a supported pincer ligand for Pd(II). The functionalized magnetic mesoporous silica was further reacted with [PdCl2(SMe2)2] to produce a supported N‐heterocyclic carbene–Pd(II) complex. The obtained catalyst was characterized using Fourier transform infrared spectroscopy, scanning electron microscopy, energy‐dispersive X‐ray analysis, vibrating sample magnetometry, Brunauer–Emmett–Teller surface area measurement and X‐ray diffraction. The amount of the loaded complex was 80.3 mg g?1, as calculated through thermogravimetric analysis. The formation of the ordered mesoporous structure of SBA‐15 was confirmed using low‐angle X‐ray diffraction and transmission electron microscopy. Also, X‐ray photoelectron spectroscopy confirmed the presence of the Pd(II) complex on the magnetic support. The prepared magnetic catalyst was then effectively used in the coupling reaction of olefins with aryl halides, i.e. the Heck reaction, in the presence of a base. The reaction parameters, such as solvent, base, temperature, amount of catalyst and reactant ratio, were optimized by choosing the coupling reaction of 1‐bromonaphthalene and styrene as a model Heck reaction. N‐Methylpyrrolidone as solvent, 0.25 mol% catalyst, K2CO3 as base, reaction temperature of 120°C and ultrasonication of the catalyst for 10 min before use provided the best conditions for the Heck cross‐coupling reaction. The best results were observed for aryl bromides and iodides while aryl chlorides were found to be less reactive. The catalyst exhibited noticeable stability and reusability.  相似文献   

18.
A novel polydentate ligand supported on Fe3O4@SiO2 was designed and demonstrated for the synthesis of Cu nanorods. The Fe3O4@SiO2/EP.EN.EG@Cu was characterized using X‐ray diffraction, thermogravimetric analysis, transmission electron microscopy, energy‐dispersive X‐ray spectroscopy and vibrating sample magnetometry. The Fe3O4@SiO2/EP.EN.EG@Cu showed excellent catalytic efficiency for the cross‐coupling reaction of nitrogen‐containing heterocycles with aryl halides. The catalyst could be effectively separated from the reaction mixture by simply applying an external magnetic field and reused at least five times without loss of activity.  相似文献   

19.
Magnetic Ni0.5Zn0.5Fe2O4‐crosslinked polyaniline composites with a core–shell structure were prepared in the presence of Ni0.5Zn0.5Fe2O4 magnetic powder in a toluene solution containing iron chloride as a surfactant and dopant. Structural characterization by Fourier transform infrared, X‐ray diffraction, scanning electron microscopy, and transmission electron microscopy proved that Ni0.5Zn0.5Fe2O4 in the composites was responsible for the ferromagnetic behavior of the composites. The effects of the polyaniline and temperature on the magnetic properties of the Ni0.5Zn0.5Fe2O4/polyaniline composites were studied with electron paramagnetic resonance and superconducting quantum interference device techniques. A clear evolution from ferromagnetic resonance to electron paramagnetic resonance was observed as a function of temperature, which was related to the passage through the Curie point (~420 K). The magnetic properties of the resulting composites showed ferromagnetic behavior, such as high‐saturated magnetization (saturation magnetization = 35–39 emu/g), low coercive force (coercivity = 22–28 G), and low blocking temperatures (~23 K). © 2006 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 2657–2664, 2006  相似文献   

20.
The surface of Fe3O4@SiO2 nanoparticles was modified using l ‐arginine as a green and available amino acid to trap palladium nanoparticles through a strong interaction between the metal nanoparticles and functional groups of the amino acid. The proposed green synthetic method takes advantage of nontoxic reagents through a simple procedure. Characterization of Fe3O4@SiO2@l ‐arginine@Pd(0) was done using Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, X‐ray diffraction, vibrating sample magnetometry and inductively coupled plasma analysis. The catalytic activity of Fe3O4@SiO2@l ‐arginine@Pd(0) as a new nanocatalyst was investigated in C – C coupling reactions. Waste‐free, use of green medium, efficient synthesis leading to high yield of products, eco‐friendly and economic catalyst, excellent reusability of the nanocatalyst and short reaction time are the main advantages of the method presented. Copyright © 2016 John Wiley & Sons, Ltd.  相似文献   

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