Cu(II)‐supported graphene quantum dots modified NiFe2O4: A green and efficient catalyst for the synthesis of 4H‐pyrimido[2,1‐b]benzothiazoles in water

NiFe₂O₄ nanoparticles are modified by graphene quantum dots (GQDs) and utilized to stabilize the Cu(II) nanoparticles as a novel magnetically retrievable catalytic system (Cu(II)/GQDs/NiFe₂O₄) for green formation of 4H‐pyrimido[2,1‐b]benzothiazoles. The prepared catalyst can be isolated assisted by an outer magnet and recovered for five courses without significant reduction in its efficiency. The as‐prepared magnetic heterogeneous nanocomposite was characterized by UV–Vis, FT‐IR, XRD, EDS, VSM, TEM, and ICP. Performing the reactions in environmentally friendly and affordable conditions (water), the low catalyst percentage, high yield of products, short reaction times, and easy workup are the merits of this protocol.     

Nanocomposite based on epoxy and MWCNTs modified with NiFe2O4 nanoparticles as efficient microwave absorbing material

In order to make a microwave absorbent material with good dielectric and magnetic properties, well dispersed microwave absorbing hybrid epoxy polymer composites containing nickel doped Fe₃O₄ nanocrystals coated on carbon nanotubes (NiFe₂O₄‐MWCNTs/epoxy) were synthesized by the combined precipitation‐hydrothermal method in 1‐30 wt.% of nanoparticles. Nickel possess well interaction with microwave radiation and represents fine electromagnetic interference (EMI) shielding and by dopping it into ferrite spinel structures, does not show any tendency to oxidation. Well‐dispersed NiFe₂O₄–MWCNTs/epoxy nanocomposite prepared by new in‐situ polymerization method. First, NiFe₂O₄–MWCNT nanoparticles ultrasonicated in acetone and after mixing with epoxy resin ultrasonicated again. Finally, hardner added to the composite and tuned temperature for evaporating solvent. X‐ray diffraction (XRD) and energy dispersive spectroscopy (EDS) confirmed the synthesizing NiFe₂O₄ nanoparticles. Saturation magnetization value of NiFe₂O₄‐MWCNTs is about 29 emu/g with very low remanence and coercivity content, which revealed that the NiFe₂O₄‐MWCNTs is ferromagnetic nanocrystal. Transmission electron microscopy (TEM) used to characterize the distribution of NiFe₂O₄ nanocrystals on the surface of MWCNTs. The TEM images show that NiFe₂O₄ nanocrystals have a mean size of 12 nm, and completely coated on the exterior surface of MWCNTs. The obtained results of reflection loss revealed that the maximum values of reflection loss of the NiFe₂O₄‐MWCNTs/epoxy increase by enhancing the content of nanoparticles until 10 wt.% and decreases in 30 wt.%.     

Spinel copper ferrite nanoparticles: Preparation,characterization and catalytic activity

The magnetic CuFe₂O₄ nanoparticles have been synthesized and characterized by various spectroscopic methods, including X‐ray diffraction (XRD), O K, Cu and Fe K ‐edge X‐ray absorption near edge structure (XANES), energy dispersive X‐ray analysis (EDX), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The azide‐alkyne cycloaddition by the reaction of various phenylacetylenes with a mixture of benzyl halides and NaN₃ and also three component (A³) coupling reaction of aldehyde, alkyne and amine catalyzed by CuFe₂O₄ nanoparticles under aerobic conditions led to the formation of the 1,4‐disubstituted‐1,2,3‐triazoles and propargylamines in excellent yields. The catalyst can be recovered by applying an external magnetic field for the subsequent cycloaddition reactions and reused without any tangible loss in catalytic efficiency.     

Preparation of Magnetic Photocatalyst TiO2 Supported on NiFe2O4 and Effect of Magnetic Carrier on Photocatalytic Activity

A magnetic photocatalyst TiO₂/NiFe₂O₄ (TN) with typical ferromagnetic hysteresis was prepared by a sol‐gel method, which is easy to be separated from a slurry‐type photoreactor under the application of an external magnetic field, being one of promising photocatalysts for wastewater treatment. The analysis of XRD indicated that the highly dispersed NiFe₂O₄ nanoparticles prevented the formation of rutile phase to some extent. A transmission electron microscope (TEM) was used to characterize the structure of the photocatalyst, indicating that the NiFe₂O₄ nanoparticles highly dispersed among TiO₂ nanoparticles. The prepared photocatalyst showed high photocatalytic activity for the degradation of methyl orange in water. The degradation results revealed that the NiFe₂O₄ nanoparticles played the role of recombination centre of photogenerated electrons and holes for the TN photocatalyst, which gave rise to the decrease in photocatalytic activity. Moreover, the experiment on recycled use of TN demonstrated a good repeatability of the photocatalytic activity.     

Synthesis of Imatinib‐loaded chitosan‐modified magnetic nanoparticles as an anti‐cancer agent for pH responsive targeted drug delivery

Targeted drug delivery is a promising approach to overcome the limitations of classical chemotherapy. In this respect, Imatinib‐loaded chitosan‐modified magnetic nanoparticles were prepared as a pH sensitive system for targeted delivery of drug to tumor sites by applying a magnetic field. The proposed magnetic nanoparticles were prepared through modification of magnetic Fe₃O₄ nanoparticles with chitosan and Imatinib. The structural, morphological and physicochemical properties of the synthesized nanoparticles were determined by different analytical techniques including energy‐dispersive X‐ray spectroscopy (EDS), field emission scanning electron microscopy (FESEM), Fourier‐transform infrared (FTIR) spectroscopy, high resolution transmission electron microscopy (HR‐TEM), vibrating sample magnetometry (VSM), X‐ray diffraction (XRD) and X‐ray photoelectron spectroscopy (XPS). UV/visible spectrophotometry was used to measure the Imatinib contents. Thermal stability of the prepared particles was investigated and their efficiency of drug loading and release profile were evaluated. The results demonstrated that Fe₃O₄@CS acts as a pH responsive nanocarrier in releasing the loaded Imatinib molecules. Furthermore, the Fe₃O₄@CS/Imatinib nanoparticles displayed cytotoxic effect against MCF‐7 breast cancer cells. Results of this study can provide new insights in the development of pH responsive targeted drug delivery systems to overcome the side effects of conventional chemotherapy.     

Synthesis and characterization of sulfamic acid supported on Fe3O4 nanoparticles: A green,versatile and magnetically separable acidic catalyst for oxidation reactions and Knoevenagel condensation

Sulfamic acid immobilized on diethylenetriamine functionalized Fe₃O₄ nanoparticles (SA‐DETA‐Fe₃O₄) was successfully prepared and characterized by X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FT‐IR), vibrating sample magnetometer (VSM), thermo gravimetric analysis (TGA), X‐Ray diffraction (XRD) and scanning electron microscopy (SEM). The sulfamic acid was found as a magnetically separable and highly active catalyst for the oxidative coupling thiols, oxidation of sulfides. Furthermore, the SA‐DETA‐Fe₃O₄ showed the high catalytic activity in Knoevenagel condensation of aromatic aldehydes with active methylene compounds (malononitrile and ethyl cynoacetate). The nanosolid catalyst could be easily recovered by a simple magnetic separation and reused for many cycles without deterioration in catalytic activity.     

One‐pot synthesis of magnetic palladium–NiFe2O4–graphene oxide composite: an efficient and recyclable catalyst for Heck reaction

A magnetically separable NiFe₂O₄@GO–Pd composite (GO = graphene oxide) was successfully prepared by a facile one‐pot hydrothermal strategy. This new kind of hybrid material was fully characterized using powder X‐ray diffraction, Raman spectroscopy, X‐ray photoelectron spectroscopy, transmission electron microscopy and vibrating sample magnetometry. Structural characterizations confirmed the formation of NiFe₂O₄ and Pd nanocrystals, and the close anchoring between nanoparticles and GO sheets. Additionally, the as‐prepared NiFe₂O₄@GO–Pd nanocomposite was effectively employed in the palladium‐catalyzed Heck reaction in an ethanol–water system as a green solvent. The catalyst was completely recoverable with the simple application of an external magnetic field and with no obvious loss of catalytic activity even after six repeated cycles. Copyright © 2016 John Wiley & Sons, Ltd.     

Synthesis and characterization of NiFe2O4 nanoparticles using the hydrothermal method as magnetic catalysts for electrochemical detection of norepinephrine in the presence of folic acid

In this article, we present a simple and efficient method to synthesize a magnetic NiFe₂O₄ nanocatalyst under hydrothermal conditions. Fourier transform infrared spectroscopy (FT‐IR), X‐ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X‐ray spectroscopy (EDX) analyses confirmed the synthesis of NiFe₂O₄ nanoparticles. These nanoparticles showed satisfactory catalytic activity for determination of norepinephrine (NE) in the presence of folic acid (FA) using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) methods. Differential pulse voltammetry peak currents of NE increased linearly with their concentrations in the range of 1.0 × 10^?7–5.0 × 10^?4 M, and the detection limit for NE was 2.3 × 10^?8 M, respectively. The modified electrode displayed strong function for resolving the overlapping voltammetric responses of NE and FA into two well‐defined voltammetric peaks. In the mixture containing NE and FA, the two compounds can well separate from each other with a potential difference of 510 mV between NE and FA, which was large enough to determine NE and FA individually and simultaneously. Additionally, the prepared electrochemical sensor demonstrated a practical feasibility for real sample determination.     

Magnetically thiamine palladium complex nanocomposites as an effective recyclable catalyst for facile sonochemical cross coupling reaction

The carbon–carbon cross coupling reactions through transition‐metal‐catalyzed processes has been significantly developed for their important synthetic applications. In this research, we have shown that NiFe₂O₄@TASDA‐Pd(0) is a highly active, novel and reusable catalyst with excellent performance for the Mizoroki–Heck coupling reaction of several types of iodo, bromo, and even aryl chlorides in DMF under ultrasound irradiation. The novel palladium catalyst prepared and characterized by using FT‐IR spectrum, X‐ray diffraction (XRD), scanning electron microscopy (SEM), Energy‐dispersive X‐ray spectroscopy (EDX), thermo gravimetric analysis (TGA) and vibrating sample magnetometer (VSM). The catalyst can be recovered and recycled several times without marked loss of activity.     

Fe3O4/MIL‐101(Fe) nanocomposite as an efficient and recyclable catalyst for Strecker reaction

A highly porous metal‐organic framework, MIL‐101(Fe), was prepared by a solvothermal method in the presence of amino‐modified Fe₃O₄@SiO₂ nanoparticles, in order to achieve Fe₃O₄/MIL‐101(Fe) nanocomposite, which was characterized by XRD, FT‐IR, SEM, TEM, BET, and VSM. This hybrid magnetic nanocomposite was employed as heterogeneous catalyst for α‐amino nitriles synthesis through three‐component condensation reaction of aldehydes (ketones), amines, and trimethylsilyl cyanide in EtOH, at room temperature. The recoverability and reusability was admitted for the heterogeneous magnetic catalyst; no significant reduction of catalytic activity was observed even after five consecutive reaction cycles.     

Ni(II)‐Adenine complex coated Fe3O4 nanoparticles as high reusable nanocatalyst for the synthesis of polyhydroquinoline derivatives and oxidation reactions

In the present study, Fe₃O₄ nanoparticles were prepared via simple and versatile procedure. Then, a novel and green catalyst was synthesized by the immobilization of Ni on Fe₃O₄ nanoparticles coated with adenine. The activity of this nanostructure compound was examined for the oxidation of sulfides, oxidative coupling of thiols and synthesis of polyhydroquinolines. The prepared catalyst was characterized by Fourier transform infrared spectroscopy (FT‐IR), scanning electron microscopy (SEM), energy‐dispersive X‐ray spectroscopy (EDS), inductively coupled plasma optical emission spectroscopy (ICP‐OES), X‐ray Diffraction (XRD), thermal gravimetric analysis (TGA), and vibrating sample magnetometer (VSM) measurements. This organometallic catalyst was recovered by the assistance of an external magnetic field from the reaction mixture and reused for seven continuous cycles without noticeable change in its catalytic activity.     

Core shell‐structured NiFe2O4@TiO2 nanoparticle‐anchored reduced graphene oxide for rapid degradation of rhodamine B

In this work, the NiFe₂O₄@TiO₂/reduced graphene oxide (RGO) ternary nanocomposites with high saturation magnetization and catalytic efficiency have been synthesized through the following steps. First, graphene oxide was prepared using the modified Hummer's method. Second, the NiFe₂O₄ nanoparticles were successfully prepared using the hydrothermal method. Third, the core shell‐structured NiFe₂O₄@TiO₂/RGO nanocomposite precursors were easily obtained through hydrolysis reaction. The morphology of NiFe₂O₄@TiO₂/RGO nanocomposites was characterized from scanning electron microscope (SEM) and transmission electron microscope (TEM) images. Moreover, the results of X‐ray diffraction (XRD) patterns proved that the TiO₂ coating shell consisted of anatase. The vibrating sample magnetometer (VSM) measurements showed that the saturation magnetization value of NiFe₂O₄@TiO₂/RGO ternary nanocomposites was 25 emu/g. The X‐ray photoelectron spectroscopy (XPS) analysis confirmed that only part of the graphite oxide (GO) was reduced to RGO in the ternary nanocomposite. The degradation experiments proved that NiFe₂O₄@TiO₂/RGO nanocomposite exhibited the high catalytic efficiency and outstanding recyclable performance for rhodamine B (RhB).     

Synthesis and characterization of micron‐sized monodisperse superparamagnetic polymer particles with amino groups

Micron‐sized monodisperse superparamagnetic polyglycidyl methacrylate (PGMA) particles with functional amino groups were prepared by a process involving: (1) preparation of parent monodisperse PGMA particles by the dispersion polymerization method, (2) chemical modification of the PGMA particles with ethylenediamine (EDA) to yield amino groups, and (3) impregnation of iron ions (Fe²⁺ and Fe³⁺) inside the particles and subsequently precipitating them with ammonium hydroxide to form magnetite (Fe₃O₄) nanoparticles within the polymer particles. The resultant magnetic PGMA particles with amino groups were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), X‐ray diffractometry (XRD), and vibrating sample magnetometry (VSM). SEM showed that the magnetic particles had an average size of 2.6 μm and were highly monodisperse. TEM demonstrated that the magnetite nanoparticles distributed evenly within the polymer particles. The existence of amino groups in the magnetic polymer particles was confirmed by FTIR. XRD indicated that the magnetic nanoparticles within the polymer were pure Fe₃O₄ with a spinel structure. VSM results showed that the magnetic polymer particles were superparamagnetic, and saturation magnetization was found to be 16.3 emu/g. The Fe₃O₄ content of the magnetic particles was 24.3% based on total weight. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 3433–3439, 2005     

Fe3O4@NCs/BF0.2: A magnetic bio‐based nanocatalyst for the synthesis of 2,3‐dihydro‐1H‐perimidines

Nanocellulose (NC) materials have some unique properties, which make them attractive as organic or inorganic supports for catalytic applications. Nanocatalysts with diameters of less than 100 nm are difficult to separate from the reaction mixture, therefore, magnetic nanoparticles (MNPs) were used as catalysts to overcome this problem. Fe₃O₄@NCs/BF_0.2 as a green, bio‐based, eco‐friendly, and recyclable catalyst was synthesized and characterized using fourier‐transform infrared spectroscopy (FT‐IR), vibrating sample magnetometer (VSM), X‐ray diffraction (XRD), X‐ray fluorescence (XRF), Brunauer–Emmett–Teller (BET), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and thermal gravimetric analysis (TGA) techniques. Fe₃O₄@NCs/BF_0.2 was employed for the synthesis of 2,3‐dihydro‐1H‐perimidine derivatives via a reaction of 1,8‐diaminonaphthalene with various aldehydes at room temperature under solvent‐free conditions. The present procedure offers several advantages including a short reaction time, excellent yields, easy separation of catalyst, and environmental friendliness.     

Phytochemical analysis and Enzyme Inhibition Assay of Aerva javanica for Ulcer

Background

Nickel ferrite, a kind of soft magnetic materials is one of the most attracting class of materials due to its interesting and important properties and has many technical applications, such as in catalysis, sensors and so on. In this paper the synthesis of NiFe₂O₄ nanoparticles by the hydrothermal method is reported and the inhibition of surfactant (Glycerol or Sodium dodecyl sulfate) on the particles growth is investigated.

Methods

For investigation of the inhibition effect of surfactant on NiFe₂O₄ particles growth, the samples were prepared in presence of Glycerol and Sodium dodecyl sulfate. The X-ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometer (VSM) and inductively coupled plasma atomic emission spectrometer (ICP-AES) techniques were used to characterize the samples.

Results

The results of XRD and ICP-AES show that the products were pure NiFe₂O₄ and also nanoparticles grow with increasing the temperature, while surfactant prevents the particle growth under the same condition. The average particle size was determined from the Scherrer's equation and TEM micrographs and found to be in the range of 50-60 nm that decreased up to 10-15 nm in presence of surfactant. The FT-IR results show two absorption bands near to 603 and 490 cm^-1 for the tetrahedral and octahedral sites respectively. Furthermore, the saturated magnetization and coercivity of NiFe₂O₄ nanoparticles were in the range of 39.60 emu/g and 15.67 Q_e that decreased for samples prepared in presence of surfactant. As well as, the nanoparticles exhibited a superparamagnetic behavior at room temperature.

Conclusions

Nanosized nickel ferrite particles were synthesized with and without surfactant assisted hydrothermal methods. The results show that with increasing of temperature, the crystallinity of nanoparticles is increased. In the presence of surfactants, the crystallinity of NiFe₂O₄ nanoparticles decreased in comparison with surfactant- free prepared samples. All of the nickel ferrite nanoparticles were superparamagnetic at room temperature.

Graphical abstract

     

Palladium nanoparticles supported on modified hollow Fe3O4@TiO2: Preparation,characterization, and catalytic activity in Suzuki cross‐coupling reactions

Hollow Fe₃O₄@TiO₂‐NH₂/Pd as a light‐weight, magnetically heterogeneous catalyst was successfully prepared, and characterized by using different techniques including X‐ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT‐IR), field‐emission scanning electron microscopy (FE‐SEM), transmission electron microscopy (TEM), energy‐dispersive X‐ray spectroscopy (EDX), vibrating sample magnetometer (VSM) measurements, and thermogravimetric analysis (TGA). Then this heterogeneous catalyst was tested in the Suzuki cross‐coupling reaction, and the results confirmed the success of this method. The catalyst could be separated easily using an external magnet and reused at least in five runs successfully without any appreciable loss in its catalytic activity.     

Hydrothermal Synthesis of g‐C3N4/NiFe2O4 Nanocomposite and Its Enhanced Photocatalytic Activity

Herein, for the first time, a direct Z‐scheme g‐C₃N₄/NiFe₂O₄ nanocomposite photocatalyst was prepared using facile one‐pot hydrothermal method and characterized using XRD, FT‐IR, DRS, PL, SEM, EDS, TEM, HRTEM, XPS, BET and VSM characterized techniques. The result reveals that the NiFe₂O₄ nanoparticles are loaded on the g‐C₃N₄ sheets successfully. The photocatalytic activities of the as‐prepared photocatalysts were evaluated for the degradation of methyl orange (MO) under visible light irradiation. It was shown that the photocatalytic activity of the g‐C₃N₄/NiFe₂O₄ nanocomposite is about 4.4 and 3 times higher than those of the pristine NiFe₂O₄ and g‐C₃N₄ respectively. The enhanced photocatalytic activity could be ascribed to the formation of g‐C₃N₄/NiFe₂O₄ direct Z‐scheme photocatalyst, which results in efficient space separation of photogenerated charge carriers. More importantly, the as‐prepared Z‐scheme photocatalyst can be recoverable easily from the solution by an external magnetic field and it shows almost the same activity for three consecutive cycles. Considering the simplicity of preparation method, this work will provide new insights into the design of high‐performance magnetic Z‐scheme photocatalysts for organic contaminate removal.     

Characterization of NiFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles synthesized by various methods

Microwave-induced combustion with glycine, CTAB-assisted hydrothermal process with NaOH and NH3, EDTA assisted-hydrothermal methods have been applied to prepare NiFe₂O₄ nanoparticles for the first time. Structural and magnetic properties of the products were investigated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmison electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), and electron spin resonance spectrometry (EPR). TEM measurements showed that morphology of the product depends on the synthesis method employed. The average cystallite size of NiFe₂O₄ nanoparticles was in the range of 14–59 nm as measured by XRD. The uncoated sample (Method A) had an EPR linewidth of 1973 Oe, the coated samples reached lower values. The magnetic dipolar interactions existing among the Ni ferrite nanoparticles are reduced by the coatings, which could cause the decrease in the linewidth of the EPR signals. Additionally, the linewidth increases with an increase in the size and the size distribution of nanoparticles.     

Preparation and characterization of palladium immobilized on silica‐coated Fe3O4 and its catalytic performance for Suzuki reaction under microwave irradiation

Supported palladium catalyst (Pd/Fe₃O₄@SiO₂) was easily prepared by supporting PdCl₂ on silica‐coated magnetic nanoparticles Fe₃O₄ in ethylene glycol. The as‐prepared sample was characterized by infrared spectroscopy (IR), X‐ray diffraction (XRD) and X‐ray photoelectron spectrometer (XPS). The formation of active specie Pd(0) was confirmed by XRD and XPS, and the Pd loading for the fresh and recovered catalyst was determined by atomic absorption spectroscopy (AAS). Pd/Fe₃O₄@SiO₂ was employed for the synthesis of biphenyl derivatives via Suzuki reaction. In terms of the yield of biphenyl, the supported catalyst displayed nearly equal catalytic performance to that of homologous PdCl₂ under microwave irradiation for 30 min but higher than that obtained by traditional heating method for 12 h. The catalytic performance of Pd/Fe₃O₄@SiO₂ for Suzuki reactions involving various aryl halides and arylboronic acids were also examined. Impressive yield of biphenyl at 68.2% was obtained even in the presence of unreactive aryl chlorides. Pd/Fe₃O₄@SiO₂ was recovered by a permanent magnet and directly reused in the next run, and no obvious deactivation was observed for up to 6 times. Copyright © 2016 John Wiley & Sons, Ltd.     

Flash microwave synthesis of trevorite nanoparticles

Nickel ferrite nanoparticles have several possible applications as cathode materials for rechargeable batteries, named “lithium-ion” batteries. In this study, NiFe₂O₄ was prepared by microwave induced thermohydrolysis. The obtained nanoparticles were characterized by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), BET method, transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS). All the results show that the microwave one-step flash synthesis leads in a very short time to NiFe₂O₄ nanoparticles with elementary particles size close to 4-5 nm, and high specific surfaces (close to 240 m²/g). Thus, microwave heating appears as an efficient source of energy to produce quickly nanoparticles with complex composition as ferrite.