Separation of Arsenic from Aqueous Solutions by Amino-Functionalized γ-Fe2O3-β-Zeolite

In this research, γ-Fe₂O₃-β-zeolite nanocomposite was synthesized and functionalized by 3-amino propyl trimethoxysilane. The magnetic functionalized adsorbent was characterized by FTIR, X-ray diffraction, thermal analysis, vibrating sample magnetometry, scattering electron microscopy, and N₂ adsorption-desorption techniques. The adsorbent was then used for adsorption of arsenic from aqueous solutions. At optimized conditions the adsorption capacity of 30 mg.g^?1 was obtained, which was higher than the previously reported values. The loaded adsorbent was easily separated from the solution by applying an external magnetic field. Regeneration of the adsorbent by NaOH solution indicated that 97% of the initial capacity was remained after four adsorption-regeneration cycles.     

Tunable structural and electrical impedance properties of ordered and disordered iron oxide phases for capacitive applications

Having extensive knowledge of room temperature and temperature dependent dielectric and impedance properties of iron oxide nanostructures will help in extending the field of application from biomedical sciences to microelectronics industry. This aspect of iron oxide has long been neglected and the attention is mostly focused on magnetic investigations. To explore and extend the field of application of iron oxide this study is focused on detailed investigation of structural as well as temperature dependent (30–210?°C) dielectric along with impedance analysis. Iron oxide nanostructures are prepared using template free oleic acid assisted sol-gel method with variation in molarity of the finally synthesized sol in the range of 0.2–2.0?mM (interval 0.2?mM). Magnetite (Fe₃O₄) phase is observed at molarity of 0.2?mM whereas, vacancy ordered and disordered maghemite (γ-Fe₂O₃) phases are observed at molarities of 0.8–1.0?mM and 1.4–2.0?mM, respectively. Dielectric constant of 104.6, 74.5 and 98.43 (log f = 5.0) is observed at molarities of 0.2?mM, 1.0?mM and 2.0?mM for Fe₃O₄ and vacancy ordered (V_o) & disordered (V_d) γ-Fe₂O₃ phase, respectively. Zview software is used for the fitting of Nyquist plots. Fitted data reveals that dielectric constant strongly depends on grain boundary resistance (R_gb). Activation energy of 0.25?eV and 0.296?eV (log f = 5) is observed for Fe₃O₄ and V_d γ-Fe₂O₃ phase at 0.2?mM and 2.0?mM molarity of the final iron oxide sol.     

Activated carbon/iron oxide magnetic composites for the adsorption of contaminants in water

In this work the adsorption features of activated carbon and the magnetic properties of iron oxides were combined in a composite to produce magnetic adsorbents. These magnetic particles can be used as adsorbent for a wide range of contaminants in water and can subsequently be removed from the medium by a simple magnetic procedure. Activated carbon/iron oxide magnetic composites were prepared with weight ratios of 2:1, 1.5:1 and 1:1 and characterized by powder XRD, TG, magnetization measurements, chemical analyses, TPR, N₂ adsorption-desorption isotherms, Mössbauer spectroscopy and SEM. The results suggest that the main magnetic phase present is maghemite (γ-Fe₂O₃) with small amounts of magnetite (Fe₃O₄). Magnetization enhancement can be produced by treatment with H₂ at 600 °C to reduce maghemite to magnetite. N₂ adsorption measurements showed that the presence of iron oxides did not significantly affect the surface area or the pore structure of the activated carbon. The adsorption isotherms of volatile organic compounds such as chloroform, phenol, chlorobenzene and drimaren red dye from aqueous solution onto the composites also showed that the presence of iron oxide did not affect the adsorption capacity of the activated carbon.     

Electrodeposition of iron oxide nanorods on carbon nanofiber scaffolds as an anode material for lithium-ion batteries

Iron oxide film with spaced radial nanorods is formed on the VGCF (vapor-grown carbon nanofiber) scaffolds by means of anodic electrodeposition. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy show that the iron oxide film deposited on the VGCF surface is α-Fe₂O₃ and consists of spaced radial nanorods having 16-21 nm in diameter after annealing at 400 °C. Galvanostatic charge/discharge results indicate that the α-Fe₂O₃/VGCF anode (970 mAh g⁻¹) has higher capacity than bare α-Fe₂O₃ anode (680 mAh g⁻¹) at 10 C current discharge. VGCF scaffolds fabricated by electrophoretic deposition favor the electron conduction, and the spaced radial nanorods on VGCFs facilitate the migration of lithium ion from the electrolyte. Electrochemical reactions between α-Fe₂O₃ and lithium ion are therefore improved significantly by this tailored architecture.     

Adsorptive removal of methyl orange using mesoporous maghemite

In this work, mesoporous maghemite (γ-Fe₂O₃) was prepared by the thermal decomposition of [Fe(CON₂H₄)₆](NO₃)₃ with the aid of cetyltrimethyl ammonium bromide (CTAB), and its adsorption ability for the removal of methyl orange (MO) from wastewater was investigated. X-Ray powder diffraction (XRD) together with nitrogen adsorption–desorption measurements show the formation of mesoporous γ-Fe₂O₃ with an average pore size of 3.5 nm and a specific surface area of 93.0 m²/g. Magnetic measurements show that the mesoporous γ-Fe₂O₃ exhibits ferrimagnetic characteristics with the coercivity of 141.5 Oe and remanent magnetization of 7.3 emu/g and has the maximum saturation magnetization of 55.2 emu/g. The adsorption of MO on the mesoporous γ-Fe₂O₃ reaches the maximum adsorbed percentage of ca. 90% within a few minutes, showing that most of MO can be removed in a short time when the mesoporous γ-Fe₂O₃ is used as an adsorbent. When the pH of MO solution is varied from 3 to 11, the adsorbed percentage of MO decreases from ca. 90 to ca. 81%, showing that the adsorption is slightly influenced by solution pH. The adsorption data for MO fit well with either Langmuir or Freundlich adsorption models. The maximum adsorption capacity of the mesoporous γ-Fe₂O₃ for MO is determined to be 385 mg/g, which suggests that the material could be an excellent magnetic adsorbent for MO.     

Effects of drying conditions on physicochemical properties of epoxide sol−gel derived α-Fe2O3 and NiO: A comparison between xerogels and aerogels

A simple and easily operated supercritical CO₂ dryer was designed and manufactured with the aim of producing high-surface-area mesoporous α-Fe₂O₃ (hematite) and NiO aerogels. The gels were synthesized by a sol?gel method with the aid of propylene oxide (PO), as the gelation agent, and then dried and calcined at different conditions. The effects of drying and calcination conditions on the physicochemical properties of the final aerogels were investigated using X-ray diffraction (XRD), N₂ adsorption-desorption, Fourier-transformed infrared spectroscopy (FT-IR), and field emission scanning electron microscopy (FE-SEM) analyses. It was demonstrated that α-Fe₂O₃ and NiO aerogels with high surface areas and mesoporosities could be successfully synthesized using the home-made supercritical CO₂ dryer. Supercritical drying of the gels resulted in α-Fe₂O₃ (186 m²/g) and NiO (178 m²/g) aerogels with 186% and 34% higher surface areas, respectively, than xerogels obtained via simple drying at 80°C using a laboratory oven. In addition, the results showed that supercritical CO₂ drying could enhance preservation of the porous network of the oxide nanostructures at high calcination temperatures via suppression of sintering phenomenon. Calcination of α-Fe₂O₃ and NiO aerogels at 600°C yielded 225% and 53% higher surface areas than the corresponding xerogel, confirming the significance of drying step in the sol?gel method. Asphaltene adsorption from a model oil with asphaltene concentration of 3000 ppm indicated that the aerogels possessed higher adsorption capacities for the bulky asphaltene molecules than xerogels calcined at the same temperature of 600°C, which was due to their enhanced textural properties.     

Adsorptive removal of alizarin dye from wastewater using maghemite nanoadsorbents

ABSTRACT

This is an investigation of the adsorptive removal of anthraquinone dyes, resembled by Alizarin, by utilizing maghemite iron oxide (γ-Fe₂O₃) nanoparticles in aqueous media. The adsorption process was affected by several parameters such as solution pH, adsorbent amount, contact time, and temperature. After optimizing the parameters affecting the adsorption, the process was successful in removing Alizarin dye with an efficiency exceeding 95%. Best adsorption results were achieved at a pH of 11 and contact time of 60 min. The adsorption was shown to follow the Langmuir model suggesting a monolayer and homogeneous coverage. The maximum adsorption capacity (q_m ) was found to be 23.2 mg/g at pH = 11. A thermodynamic study showed that the adsorption process is exothermic and spontaneous at room temperature. The Gibbs free energy of adsorption (-6.79 kJ/mol) obtained in this study suggests a physisorption process. This finding has facilitated the regeneration of the Fe₂O₃ nanocatalyst. Both NaOH and HNO₃ at dilute levels were tested for the regeneration of the nanocatalyst. Regeneration with HNO₃ was successful up to four successive removal cycles with an efficiency >80%. Photodegradation experiments utilizing a UV light were also successful in maximizing the adsorption removal efficiency. A sorption mechanism based on the results obtained in this work is also proposed.     

Polyacrylonitrile/α-Fe2O3 Hybrid Photocatalytic Composite Adsorbents for Enhanced Dye Removal

The potential of a novel α-Fe₂O₃/polyacrylonitrile (PAN) hybrid composite adsorbent to eliminate methylene blue (MB) from aqueous solution was evaluated. PAN was selected as the base composite. The presence of α-Fe₂O₃ as nanophotocatalyst on the surface of PAN introduced an efficient photocatalytic hybrid composite adsorbent for degrading MB. Effects of α-Fe₂O₃ nanopowder loading, pH, temperature, MB initial concentration, solar light, and contact time were investigated. Langmuir, Freundlich, and Temkin isotherms were applied to analyze the adsorption behavior. The Freundlich equation provided the best correlation with experimental data. Pseudo-first-order, pseudo-second-order, and intraparticle models were employed. Thermodynamic studies indicated an endotherm and spontaneous adsorption process in a defined temperature range.     

Synthesis of magnetic citric‐acid‐functionalized graphene oxide and its application in the removal of methylene blue from contaminated water

A magnetic nanocomposite of citric‐acid‐functionalized graphene oxide was prepared by an easy method. First, citric acid (CA) was covalently attached to acyl‐chloride‐functionalized graphene oxide (GO). Then, Fe₃O₄ magnetic nanoparticles (MNPs) were chemically deposited onto the resulting adsorbent. CA, as a good stabilizer for MNPs, was covalently attached to the GO; thus MNPs were adsorbed much more strongly to this framework and subsequent leaching decreased and less agglomeration occurred. The attachment of CA onto GO and the formation of the hybrid were confirmed by Fourier transform infrared spectroscopy, scanning electron microscopy, X‐ray diffraction spectrometry and transmission electron microscopy. The specific saturation magnetization of the magnetic CA‐grafted GO (GO‐CA‐Fe₃O₄) was 57.8 emu g^?1 and the average size of the nanoparticles was found to be 25 nm by transmission electron microscopy. The magnetic nanocomposite was employed as an adsorbent of methylene blue from contaminated water. The adsorption tests demonstrated that it took only 30 min to attain equilibrium. The adsorption capacity in the concentration range studied was 112 mg g^?1. The GO‐CA‐Fe₃O₄ nanocomposite was easily manipulated in an external magnetic field which eases the separation and leads to the removal of dyes. Thus the prepared nanocomposite has great potential in removing organic dyes. © 2014 Society of Chemical Industry     

Catalytic ozonation process using PAC/γ-Fe2O3 to Alizarin Red S degradation from aqueous solutions: a batch study

In the catalytic ozonation process used in this study, adsorption and chemical reactions were performed at the catalyst surface. This process can increase the efficiency of plain ozonation. The main aim of this study was to investigate the efficiency of the catalytic ozonation process in removing Alizarin Red S dye from colored water by Fe₂O₃ coated on PAC. In this work, activated carbon powder/γ-Fe₂O₃ nano-composite was modified. The BET results showed that the surface area in PAC and PAC-γ-Fe₂O₃ nano-composite was 654 and 450?m² g^?1, respectively. In this study, the best pH for removal of ARS was found to be 9. At a higher pH, the efficiency of the process decreased gradually. According to studies, catalysts increase surface area and active sites for more ozone degradation. Also, the characterization of the catalyst will play a very important role in the COP. Also, the maximum removal efficiency was observed in catalyst dose 1.1?g l^?1. The study results showed that the highest mineralization rate in ARS degradation was related to O₃/PAC/γ-Fe₂O₃. The amount of mineralization in the SOP, O₃-PAC, and O₃/PAC/γ-Fe₂O₃ was 13, 25, and 40%, respectively. The finding of mineralization of ARS using the SOP reflected the low power of the ozonation process for the mineralization of pollutants.     

Nanosized α-Fe2O3 and Li-Fe composite oxide electrodes for lithium-ion batteries

Nanosized α-Fe₂O₃ (ca. 50 nm) and Li-Fe composite oxides (ca. 29 nm) powders were synthesized via gel polymer route. The gels were obtained with thermal polymerization of acrylic acid solutions of iron and lithium nitrates. The calcination of these gels at temperatures from 300 °C to 500 °C results in α-Fe₂O₃ from Fe(NO₃)₃ precursor and Li-Fe composite oxides Li₂O-Fe₃O₄-LiFeO₂ from a mixed precursors of Fe(NO₃)₃ and LiNO₃. Thermal gravimetric analysis, X-ray diffraction and transmission electron microscopy were used to investigate the precursors and products. The electrochemical performance of the Fe-based oxides was also evaluated. After 200 cycles, their capacity can be as high as 1300 mAh/g for α-Fe₂O₃ and 1400 mAh/g for Li-Fe oxide while the initial capacity loss is as low as 21.8%. The Li-Fe oxide electrodes exhibit better capacity retention than the α-Fe₂O₃ electrodes. They are interesting negative electrodes for high energy density lithium-ion batteries.     

Iron oxide synthesis using a continuous hydrothermal and solvothermal system

Iron oxide synthesis via a continuous hydrothermal and solvothermal reaction were studied. In the hydrothermal synthesis, fine α-Fe₂O₃ (hematite) particles were obtained at 250–420 °C and 30 MPa. The α-Fe₂O₃ crystals were grown in sub-critical water via a dissolution and precipitation process. The growth of α-Fe₂O₃ crystals in supercritical water was suppressed due to the rather low solvent power of water. Crystalline Fe₃O₄ was obtained as the temperature was raised above the supercritical state in the solvothermal preparation. Isopropanol (IPA) was oxidized in acetone which provided a reducing atmosphere. Acetone molecule adsorption onto the Fe₃O₄ particle surface inhibited crystallite growth.     

An investigation on room temperature synthesis of vertically oriented arrays of iron oxide nanotubes by anodization of iron

Formation of iron oxide nanotubes on to pure iron substrate by an electrochemical anodization method was investigated in fluoride containing electrolytes. Anodization of iron foil in fluoride containing borate solution resulted in stacked nano-ring type oxide morphology. Nanoporous oxide layer was observed at low pH and a granular oxide layer was formed at higher pH of phosphate + fluoride solutions. Formation of either nanoporous or nanotubular oxide layer was observed in ethylene glycol (EG) solution containing 0.05-0.1 M fluoride + 1.5-3.0 vol.% water. Transition from nanoporous structure to nanotubular structure was critically controlled by anodization potential, water addition and fluoride concentration of the EG solution. The potential required for this transition decreased with increase in the water content up to 7 vol.% beyond which enhanced dissolution occurred. Annealing of the nanotubes at 500 °C resulted in predominantly α-Fe₂O₃ crystal structure. The annealed Fe₂O₃ samples consisting of a single layer of nanotubular structure showed a photo current density of 0.4 mA/cm² at 0.5 V Ag/AgCl in 1 M KOH solution under simulated solar light illumination.     

Synthesis of graphene oxide decorated with strontium oxide (SrO/GO) as an efficient nanocomposite for removal of hazardous ammonia from wastewater

ABSTRACT

In this research, graphene oxide decorated with strontium oxide (SrO/GO) is introduced as a new adsorbent material for the efficient removal of ammonia from industrial wastewater. The new adsorbent was thoroughly studied in terms of morphology, crystallography and chemical composition using characterization techniques such as Fourier transform infrared (FTIR), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and zeta potential analysis. Several parameters such as pH, adsorbent dosage, contact time, and ammonia initial concentration were investigated and optimized. Ammonia adsorption onto SrO/GO was validated with kinetics and adsorption isotherms by adopting different models. The results revealed that ammonia adsorption kinetic was of pseudo-second order (R² = 0.999) implying that chemisorption behavior and the equilibrium isotherm follows Langmuir model. This behavior shows a high maximum monolayer sorption capacity of 90.1 mg g^?1 at pH equal to 7 and contact time of 120 min pointing out the synergism advantageous effect. The abundant oxygen functional groups on the graphene oxide surface and the integrated Sr-O nanoparticles could efficiently interact with ammonia species creating a surface for more favorable and efficient removal of ammonia.     

Synthesis and characterization of an iron oxide poly(styrene-co-carboxybutylmaleimide) ferrimagnetic composite

In situ precipitation of iron oxide nanoparticles within the cross-linked styrene-(N-4-carboxybutylmaleimide) copolymer was carried out by an ion-exchange method. The resulting composite was studied by X-ray photoelectron (XPS) and Fourier transform infrared (FTIR) spectroscopies. FTIR analysis showed the evolution of iron oxide deposition and the formation of sodium carboxylate due to the deposition treatment. In addition, XPS analysis indicated the complete oxidation of iron(II) to iron(III) by the presence of the representative peaks of iron oxide and iron oxyhydroxide. X-ray diffraction analysis was used to identify the inorganic phases. The results showed the formation of maghemite (γ-Fe₂O₃), and after several deposition cycles, goethite (α-FeOOH). The morphology and spatial distribution of iron oxide particles within the copolymer matrix were determined by transmission electron microscopy. The mean particle size of the iron oxide was of 14 nm as determined from wide-angle X-ray diffraction using the Scherrer equation. The evolution of magnetic properties with the number of deposition cycles was investigated by magnetometry at room temperature. The poly(styrene-co-N-4-carboxybutylmaleimide)/γ-Fe₂O₃/α-FeOOH/composite showed a soft ferrimagnetic behavior and, after the third deposition cycle, showed a saturation magnetization of 8.04 emu/g at 12 kOe and coercivity field of 51 Oe.     

Adsorption and kinetic studies of methylene blue on modified HUSY zeolite and an amorphous mixture of γ-alumina and silica

ABSTRACT

Our work focuses on the study of the adsorption of methylene blue (MB) on adsorbents based on zeolite HUSY and (γAl₂O₃-SiO₂). To optimize the process of removing MB onto Ni/Co USY, different parameters were studied such as contact time, initial pH, initial dye concentration, zero charge’s point, and adsorbent dosage. The adsorption isotherm follows the Langmuir model. The maximum adsorption capacities of MB were 59.88 mg g^?1 for Ni/Co USY and 43.86 mg g^?1 for Ni/Co (γAl-Si) at 298°K. The thermodynamic parameters and activation energy’s values obtained suggested that the adsorption was a physical process, spontaneous, and endothermic in nature. MB adsorption on Ni/Co USY may occur via electrostatic interaction, hydrogen bonding, and Lewis acid–base interaction.     

Flotation of α-iron(III) oxide by cetyltrimethylammonium bromide and its activation by phosphates

The zero point of charge, z.p.c., of chemically prepared α-Fe₂O₃ was found at pH 6.9. The adsorption isotherms of cetyltrimethylammonium bromide, CTAB, had a Langmuir shape and shifted to higher adsorption density as the pH increased above the z.p.c. The variation of the adsorption plateau with pH could be correlated with the change in ζ potential accompanying the adsorption of CTAB. The graphs of the recovery of α-Fe₂O₃ floated by CTAB plotted against its equilibrium concentration exhibited maxima, which became higher as the pH increased from 6 to 10. The adsorption capacity of α-Fe₂O₃ for phosphate ions markedly decreased and their desorption increased as the pH increased. The drop in ζ potential of α-Fe₂O₃ in phosphate solution became smaller as the pH increased. In presence of phosphate ions, the adsorption capacity of α-Fe₂O₃ for CTAB markedly increased at pH 6, the enhancement becoming less marked as the pH increased. The enhancement paralleled the phosphate adsorption. In presence of phosphate ions, the recovery of α-Fe₂O₃ floated by CTAB was higher, the activation decreasing as the pH increased. The maximum recovery was shifted to lower CTAB concentration compared to the recovery of unactivated α-Fe₂O₃.     

Synergistic Effect of Maghemite and Titania Nanoparticles in PVA-Alginate Encapsulated Beads for Photocatalytic Reduction of Pb(II)

In this paper, maghemite (γ-Fe₂O₃) and titanium oxide (TiO₂) nanoparticles were synthesized by hydrothermal and coprecipitation methods, respectively. These nanoparticles were combined together in various ratios (1:10, 1:20, 1:60, 1:80, and 1) and embedded in polyvinyl alcohol (PVA)-alginate beads. These beads were tested for photocatalytic behavior in eliminating toxic Pb(II) from the aqueous solution. The photocatalytic experiments were performed under sunlight irradiation and without sunlight. Several operating conditions such as initial Pb(II) concentration, pH, contact time, and TiO₂: γ-Fe₂O₃ ratios were investigated to evaluate their effect on the process. The recycling attributes of these beads were also investigated. The results revealed that 100% of the Pb(II) was eliminated in 100 min at pH 7 under sunlight when the ratio of TiO₂:γ-Fe₂O₃ was kept to 1. The PVA-alginate maghemite and titania beads showed better efficiency for Pb(II) removal than PVA-alginate titania beads and PVA-alginate maghemite beads. X-ray photoelectron spectroscopy (XPS) analysis also revealed that Pb(II) removal was via photocatalytic reduction due to the presence of Pb(0) in the high-resolution scan at 130–160 eV. Also, the PVA-alginate titania and maghemite beads can be readily isolated from the aqueous solution after the photocatalytic process and reused for at least 6 times without significant losses in their initial properties. The reduction of Pb(II) with PVA-alginate titania and maghemite beads fitted the Langmuir–Hinshelwood (L–H) kinetic model at a correlation coefficient (R²) of 0.9923.     

Synthesis of Magnetic Fe3O4 Modified Graphene Nanocomposite and its Application on the Adsorption of some Dyes from Aqueous Solution

A novel magnetic Fe₃O₄ modified reduced graphene oxide nanocomposite (Fe₃O₄@SiO₂-rGO) was prepared by a covalent bonding method. The morphology and properties of the Fe₃O₄@SiO₂-rGO were characterized by transmission electron microscopy and X-ray diffraction. The prepared Fe₃O₄@SiO₂-rGO was tested as an efficient adsorbent for the removal of some dyes from aqueous solution for the first time. The performance of Fe₃O₄@SiO₂-rGO was evaluated using methylene blue and neutral red as model compounds. Experiments were carried out to investigate the adsorption kinetics and adsorption capacity of the adsorbent and the effect of the adsorbent dosage and sample solution pH on the removal of the dyes. Kinetic data were well fitted by pseudo second-order model. The Langmuir model and the Freundlich model were used to study the adsorption isotherms. The Fe₃O₄@SiO₂-rGO nanocomposite showed to be a highly efficient adsorbent with the advantage of separation convenience. The thermodynamic parameters indicated that the adsorption of the dyes onto the Fe₃O₄@SiO₂-rGO was a spontaneous process.