Mixture Of FeCl3 Research Articles

Iron-Catalyzed sp3 C-H Alkylation of Fluorene with Primary and Secondary Alcohols: A Borrowing Hydrogen Approach.

The utilization of earth-abundant, cheap, and nontoxic transition metals in important catalytic transformations is essential for sustainable development, and iron has gained significant attention as the most abundant transition metal. A mixture of FeCl2 (3 mol %), phenanthroline (6 mol %), and KOtBu (0.4 eqivalent) was used as an effective catalyst for the sp3 C-H alkylation of fluorene using alcohol as a nonhazardous alkylating partner, and eco-friendly water was formed as the only byproduct. The substrate scope includes a wide range of substituted fluorenes and substituted benzyl alcohols. The reaction is equally effective with challenging secondary alcohols and unactivated aliphatic alcohols. Selective mono-C9-alkylation of fluorenes with alcohols yielded the corresponding products in good isolated yields. Various postfunctionalizations of C-9 alkylated fluorene products were performed to establish the practical utility of this catalytic alkylation. Control experiments suggested a homogeneous reaction path involving borrowing hydrogen mechanism with the formation and subsequent reduction of 9-alkylidene fluorene intermediate.

Polymeric laser rods based on modified poly(methyl methacrylate) matrix synthesized by FeIII complex catalyzed atom transfer radical polymerization with enhanced optical gain and Photostability

AbstractThe investigation of fabricating ultra‐compact solid‐state dye laser (SSDL) using N'N‐dimethylformamide (DMF) modified poly(methyl methacrylate) (PMMA) as the polymeric matrix was carried out. Atom transfer radical polymerization (ATRP) was introduced to manipulate the polymerization process of PMMA. By adjusting the additive amount of the FeIII complex (mixture of FeCl3 and 2,2’‐Bipyridyl (bPy)), the polymerization degree of PMMA was coordinated to gain better amplified spontaneous emission (ASE) properties of the embedded laser dye, Lumogen Orange 240 (LO). The ASE threshold of the FeIII complex catalyzed sample decreased as high as ~75%, from 225.3 ± 11.2 μJ cm−2 to 57.2 ± 2.9 μJ cm−2, comparing to that measured in common PMMA matrix. Additionally, a secondary dye, Stilbene 420 was added in the system for sharing excess excitation energy and oxidization damage, to overcome the photostability problem caused by the oxygen‐rich solvent, DMF. The operational lifetime of the resulted sample increased 200%, to the similar level of that without DMF component. Finally, by mechanical polishing and coating a thin film of silver at one end of the PMMA rod, an analogous Fabry‐Perot resonator was structured within the rod. Decent laser emission was obtained from the resulted SSDL without complex external cavities.

Reduction of Ferric Chloride in Yeast Growth Media, by Sugars and Aluminum

Iron compounds can be used in antimicrobial applications by exploiting the toxicity of divalent iron to living organisms due to the Fenton reaction. In this study, the growth inhibitory effects of ferrous sulfate FeSO4·7H2O and ferric chloride FeCl3·6H2O were observed on Metschnikowia clade and Saccharomyces cerevisiae yeast cells. The relatively high amount of reduced Fe3+ to Fe2+ in the growth medium determined by Mössbauer spectroscopy may contribute to the antimicrobial activity of ferric chloride. In order to test the reducing ability of sugars in the growth media of yeasts, the reaction of ferric chloride FeCl3·6H2O with sugars was investigated. In mixtures of FeCl3·6H2O and fructose, approximately two thirds of Fe3+ can be reduced to Fe2+. When the mixture of FeCl3·6H2O and fructose is placed on the surface of aluminum foil, an iron film is formed on the surface of the aluminum due to the reduction by both fructose and aluminum. The relative amount of Fe3+ which was reduced to Fe0 reached 68%.

Highly-efficient process for recovering gold from discarded mobile phones using pretreatment and mild extraction

Existing methods for recovering gold from electronic waste are based on mechanical and hydrometallurgy approaches. However, these methods usually use toxic chemicals and demonstrate low gold extraction efficiency (Ge) due to the negative influence of organic materials and other industrial metals also present in the waste. In this work, a more efficient and more environmentally friendly process is proposed that can achieve a high Ge from electronic waste by pre-treatment and pre-extraction before gold extraction. The powdered waste was first pre-treated by a supercritical water oxidation (SWO) process to remove organic materials and then pre-extracted using a mixture of FeCl3 and HCl to remove industrial metals. The solid powder thus produced was then re-extracted by a DMF-CuCl2-NaCl mild extraction system to complete the recovery of the gold content. Experimental results indicated that pre-treatment temperature, pre-treatment time, and the concentration of the FeCl3 and HCl solutions all significantly influenced the amount of gold extracted. The optimal parameters for achieving the highest Ge extraction (99.6%) using the DMF-CuCl2-NaCl extraction system were determined as follows: an extraction temperature of 65 °C, an extraction time of 70 min, a stirring speed of 420 rpm, a sample size of ≤ 850 µm, a solid/liquid (S/L) ratio of 1:12 g·mL−1, a CuCl2 concentration of 0.8 mol·L−1, and a NaCl concentration of 1.6 mol·L−1. After gold extraction, water was then used to precipitate the gold in the form of nanoparticles. Under optimal conditions (70%v/v water, 80 min), over 98.4% of the gold could be recovered in this way.

Incorporation of Targeting Biomolecule Improves Interpolymer Complex-Superparamagnetic Iron Oxide Nanoparticles Attachment to and Activation of T2 MR Signals in M2 Macrophages.

Inflammatory diseases are the leading cause of death in the world, accounting for 3 out of 5 deaths. Despite the abundance of diagnostic tools for detection, most screening and diagnostic methods are indirect and insufficient as they are unable to reliably discriminate between high-risk or low-risk stages of inflammatory diseases. Previously, we showed that the selective activation of interpolymer complexed superparamagnetic iron oxide nanoparticles (IPC-SPIOs) under oxidative conditions can be detected by a change in T2 magnetic resonance (MR) contrast. In this work, IPC-SPIOs were further modified by incorporating mannose as a targeting biomolecule to enhance nanoparticle delivery to M2 macrophages at inflammatory sites. Uncoated SPIOs were synthesized via coprecipitation from a mixture of FeCl2 and FeCl3, PEGylated by adsorbing PEG 300 kDa (40 mg/mL in water) to SPIOs (3 mg/mL in water) over 24 hours, and complexed by mixing 0.25 mg/mL aqueous poly(gallol) with 2 mg/mL PEG-SPIOs and adding 1 M of phosphate buffer in a 9:9:2 ratio. Mannose-PEG attachment was accomplished conducting a second complexation of mannose-PEG to IPC-SPIOs. M2 macrophages were treated with 150, 100, and 75 µg/mL of IPC-SPIOs and mannose-IPC-SPIOs to investigate activation of T2 MRI signals. Surface modification resulted in a slight reduction in ROS scavenging capacity; however, nanoparticle uptake by M2 macrophages increased by over 50%. The higher uptake did not cause a reduction in cellular viability. In fact, mannose-IPC-SPIOs induced significant T2 MR contrast in M2 macrophages compared to IPC-SPIOs and nanoparticles exposed to M1 macrophages. M2 macrophages activated over 30% of mannose-IPC-SPIOs after 6 hours of exposure compared to M1 macrophages and untargeted M2 macrophages. These findings demonstrated that mannose-IPC-SPIOs specifically targeted M2 macrophages and scavenged cellular ROS to activate T2 MR signal, which can be used to detect inflammation.

An efficient, multi-stage process for recovering gold from electronic waste involving autoclave pre-treatment and industrial-metal pre-extraction

In recent years, the recovery of gold from electronic waste, especially waste printed circuit boards (PCBs), has grown in importance. PCBs consist of organic epoxy resins overlaid with valuable metals. The first step in recovering metals from waste PCBs is the removal of these resins. In this paper, autoclave-assisted alkaline pretreatment employing NaOH was used to remove resins from the PCBs. The process is shown to remove epoxy efficiently when conducted at 350 °C for 18 h using 0.8 mol·L−1 NaOH, 18 bar, and a liquid-to-solid (L/S) ratio of 18 mL·g−1. After autoclaving, the solid-phase sample (autoclaved powder) was treated with a mixture of FeCl3 and HCl solutions – a process known as “FeH extraction” – to remove industrial metals. Under the optimal conditions (0.8 mol·L−1 FeCl3, 0.6 mol·L−1 HCl, L/S 24 mL·g−1, 50 °C, 100 min, 300 rpm), this process proved highly efficient in removing industrial metals. Following this treatment, a KClO3-HCl-CaCl2 extraction system was employed to extract gold from the FeH-extracted sample. With this system, a 99.5% gold extraction efficiency was achieved under the optimal conditions (0.55 mol·L−1 KClO3, 1.2 mol·L−1 HCl, 1.5 mol·L−1 CaCl2, 60 °C, 80 min, L/S 12 mL·g−1, 350 rpm). Gold ions (AuCl4−) in the extracted solution were subsequently recovered by using hydroquinone as a reducing agent to form gold nanoparticles (AuNPs) with the assistance of NaOH. Finally, the AuNPs were stabilized using benzoquinone (an oxidized product of hydroquinone).

Fluorous Metal–Organic Frameworks with Unique Cage-in-Cage Structures Featuring Fluorophilic Pore Surfaces for Efficient C 2 H 2 /CO 2 Separation

Fluorous Metal–Organic Frameworks with Unique Cage-in-Cage Structures Featuring Fluorophilic Pore Surfaces for Efficient C ₂ H ₂ /CO ₂ Separation

Removal of arsenic from aqueous solution by novel iron and iron–zirconium modified activated carbon derived from chemical carbonization of Tectona grandis sawdust: Isotherm, kinetic, thermodynamic and breakthrough curve modelling

The aim of the present study was: development of activated carbon modified with iron (Fe@AC) and modified with iron and zirconium (Fe–Zr@AC) from the Tectona grandis sawdust (TGS) waste biomass and its potential applicability for the removal of As (III) from contaminated water by batch and column mode. The biomass waste was pre-treated with ferric chloride (FeCl3) and the mixture of FeCl3 and zirconium oxide (ZrO2) and then pyrolyzed at 500 °C for 2 h. The properties of both bioadsorbents were comprehensively characterized by using Scanning electron microscopy (SEM), Energy dispersive X-ray (EDX), Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), Particle Size analysis (PSA), point of zero charge (pHZPC), Brunauer–Emmett–Teller (BET) to prove successful impregnation of the Fe and Zr on the surface of AC of TGS. FTIR analysis clearly indicates the Fe and Fe–Zr complexation on biosorbents surface and biosorption of As (III). The results revealed that maximum As (III) removal was achieved 86.35% by Fe–Zr@AC (3 g/L dose, pH-7.0, temperature-25 °C and concentration 0.5 mg/L). However, maximum removal of As (III) was attained ~75% by Fe@AC (with dose-4g/L, pH-7.0, temperature-25 °C and concentration 0.5 mg/L) at the initial concentration of 0.5 mg/L of As (III). Fe–Zr@AC exhibits higher efficiency with qmax value 1.206 mg/g than Fe@AC with the qmax value 0.679 mg/g for the removal of As(III). While in the column study, Fe–Zr@AC exhibited 98.8% removal at flow rate of 5 mL/min and bed height of 5 cm. Biosorption Isotherm and Kinetics were fitted good with Langmuir isotherm (R2 ≥ 0.99) and followed pseudo-second-order (R2 ≥ 0.99). The regeneration study indicates that the prepared biosorbents efficiently recycled up to five cycles. Therefore, Fe@AC and Fe–Zr@AC derived from TGS has been showed to be novel, effective, and economical biosorbent. The collective benefits of easy development, good affinity towards As (III), good separability, reusability, and inexpensive of magnetized Fe@AC and Fe–Zr@AC make it a novel biosorbent. The application of Fe–Zr@AC for the removal of As (III) from the water was very efficient its concentration in the solution after treatment was found below the 10 μg/L as per the guideline WHO.

Phyto-fabrication of Iron Nanoparticles: Characterization and Antibacterial Capacity

Introduction: Fabrication of iron nanoparticles (FeNPs) has recently gained a great concern for their varied applications in remediation technologies of the environment. Objective: The current study aimed to develop a green technology approach to fabricate FeNPs by using extracts from two different plant sources, Azadirachta indica leaf and Calligonum comosum root. Methods: A mixture of FeCl2 and FeCl3 was used to react with the plant extracts which are considered as reducing and stabilizing agents for the generation of FeNPs in one step. Spectroscopy and microscopy techniques were used for the characterization of the FeNPs. Results: Immediately after mixing the iron solution and the plant extracts, the color of the solution changed to dark brown indicating conversion of Fe ions to FeNPs. This fabrication of FeNPs was confirmed by Zetasizer, transmission electron microscopy, and scanning electron microscopy. FeNPs fabricated by C. comosum were smaller than those fabricated by A. indica. For both plant sources, FeNPs fabricated using the aqueous extract were smaller than those fabricated with the ethanolic extract. Furthermore, antibacterial ability against two bacterial species was demonstrated. Conclusion: The current results indicated that, at room temperature plant extracts fabricated Fe ion to Fe nanoparticles, suggesting its probable usage for large scale production as well as its suitability against bacteria. It could also be recommended for antibiotic resistant bacteria.

Modification of Activated Carbon from Elaeis Guineensis Jacq Shell with Magnetite (Fe3O4) Particles and Study Adsorption-Desorption on Ni(II) Ions in Solution

Activated carbon coated with magnetite (ACA-Fe3O4) was synthesized in this study. Activated carbon was synthesized using an Elaeis Guineensis Jacq (EGJ) as a raw material followed by physical and chemical activation. Physical activation is carried out by heating at a temperature of 700°C and followed by a reaction with H3PO4 solution as chemical activation. Furthermore, the activated carbon was reacted with a mixture of FeCl3 and FeSO4 solution then followed by the addition of NaOH solution up to a pH of 10. Characterization with X-Ray Diffraction (XRD) and Scanning Electron Microscopy - Energy Dispersive X-Ray (SEM-EDX) on ACA-Fe3O4 was done to confirm that magnetite has succeeded to coating on ACA. Brunauer-Emmett-Teller Surface Area Method (SBET) confirmed that pore volume and average pore diameter increase with the presence of magnetite. Optimum conditions for Ni(II) ion adsorption with ACA-Fe3O4 was under conditions of 0.5 grams adsorbent, 25 mL of Ni(II) ion solution 100 ppm, and contact time of 1 hour with the acquisition of 99.11%. Adsorption process more suitable with pseudo-second-order and Langmuir adsorption isotherm pattern. Desorption of Ni(II) ion of 70.84% using HCl.

In Situ Biosynthesized Superparamagnetic Iron Oxide Nanoparticles (SPIONS) Induce Efficient Hyperthermia in Cancer Cells

Despite the promising role of magnetic hyperthermia in cancer therapy, its use in patients has been restricted by hurdles that include inefficient targeting of magnetic particles to the tumor site, limited bioavailability, and high toxicity, etc. Taking advantage of the unique metabolic property of cancer cells, we explored the potential of these cells to biosynthesize magnetic nanoparticles for potential hyperthermia applications. Treatment of cancer cells with a mixture of FeCl2 and zinc gluconate resulted in a significant increase in intracellular Fe and Zn content in these cells. Exposure of these cells to an alternating magnetic field (AMF) for 30 min resulted in a substantial temperature rise of 5-6 °C. The in situ formed particles were identified as iron oxide and ZnO nanoparticles. Based on the magnetic property and size, the iron oxide nanoparticles were classified as superparamagnetic iron oxide nanoparticles (SPIONS) comprising a mixture of magnetite (Fe3-δO4) and maghemite (γ-Fe2O3). The role of reactive oxygen species (H2O2) and the involvement of the glycolytic pathway in the biosynthesis of the nanoparticles were confirmed using appropriate in vitro studies. The simplicity of treatment, the specificity of cells capable of synthesis of SPIONS, and the hyperthermia response observed in cancer cells indicate a promising strategy to achieve effective magnetic hyperthermia for cancer therapy.

Synthesis, Structure and Magnetic Study of a Di-Iron Complex Containing N-N Bridges

The iron (II) coordination compound, {[Fe(3,6 pzdc)](H2O)2}2. (1) has been synthesized from a mixture of FeCl2.4H2O and pyridazinedicarboxylate (3,6 pzdc). The molecular structure of complex 1 was determined by single crystal X-ray diffraction study. It reveals that the dinuclear structure contains a pyridazine bridge in between the two metal centers. The variable temperature magnetic study results in g = 2.496(8), J = −2.50(8) cm−1, Ɵ = −0.1 K values, by fitting the magnetic data in a simple dinuclear Fe-Fe model which indicates that the major exchange pathway through the N-N bridge. Presence of dense H-bonding interaction leads to supramolecular network formation.

Facile approach to develop durable and reusable superhydrophobic/superoleophilic coatings for steel mesh surfaces

Oil spills on the surfaces of bodies of water are now a great concern as they affect marine creatures and the ecosystem. Therefore, a facile technique for removal of oil from water is of much interest. In this study, superhydrophobic and superoleophilic coating is synthesized on stainless steel mesh via chemical etching using a mixture of FeCl3 and HCl followed by treatment with hexadecyltrimethoxysilane. Surface morphology analysis shows the presence of flower like microstructures on the surface after treatment. Superhydrophobic and superoleophilic properties have been achieved on stainless steel mesh with water static contact angle of 167° ± 3°, water tilting angle of 6° ± 1°, and oil static contact angle of nearly 0°. The coating shows excellent thermal, chemical and mechanical stability. Kerosene-water and hexane-water mixtures were successfully separated via a simple filtering process using coated steel mesh with a separation efficiency of more than 98%. This approach can be implemented on any shape or size of stainless steel mesh and will have industrial applications.

Characteristics and toxic dye adsorption of magnetic activated carbon prepared from biomass waste by modified one-step synthesis

Magnetic activated carbons (MACs) were synthesized by modified one-step method under CO2 atmosphere for the purification of toxic dye, using the mixture of FeCl3·6H2O and peanut shells as precursor. Textural characterization showed that the CO2-MACs synthesized were high surface area carbons and micro-mesoporous structure accounted for a large proportion in the MAC samples as a result of the etching effect of iron oxides and drastic C-CO2 reaction. XRD analysis indicated that magnetite nanoparticles were formed and the presence of CO2 promoted the formation of thermodynamically stable Fe3O4. SEM images showed that the nanoparticles were well-dispersed on the surface MACs, which occupied some of the void spaces and led to the decrease in adsorption potential and surface area if excessive FeCl3 was impregnated. Superparamagnetic behavior derived from the magnetically active magnetite enabled easy removal of the spent MAC with malachite green (MG) dye from solutions by a simple bar magnet. The best fit of PSO kinetic model and Freundlich isotherm model suggested that the adsorption on the heterogeneous surface was influenced by physisorption and chemisorption might be the rate-limiting step, and the diffusion process was mainly controlled by film diffusion and intraparticle diffusion. Spontaneous (ΔGo<0) and exothermic (ΔHo<0) nature was obtained in the entropy-controlled adsorption process through thermodynamic study. FT-IR investigation on the fresh and spent MAC coupled with pH experiments showed that interactions between CO2-MAC10 and MG could be electrostatic attraction and π-π stacking.

Hydrothermal synthesis of nanostructured Cr-doped hematite with enhanced photoelectrochemical activity

Using the easily applicable hydrothermal method Cr-doped hematite thin films have been deposited polycrystalline on conductive glass substrates. The hydrothermal bath consisted of an aqueous solution containing a mixture of FeCl3·6H2O and NaNO3 at pH = 1.5. The samples were introduced in an autoclave and heated for a fixed time at a fixed temperature and then annealed in air at 550 °C. The concentration of the incorporated Cr atoms (Cr4+ ions) was controlled by varying the concentration of the Cr(ClO4)3 precursor solution, varied from 0% to 20%. All samples followed morphological and structural studies using field-emission scanning electron microscopy, high-resolution transmission electron microscopy and X-ray diffraction. Chronoamperometry measurements showed that Cr-doped hematite films exhibited higher photoelectrochemical activity than the undoped films. The maximum photocurrent density and incident photon conversion efficiencies (IPCE) were obtained for 16 at.% Cr-doped films. This high photoactivity can be attributed to both the large active surface area and increased donor density caused by Cr-doping in the α-Fe2O3 films. All samples reached their best IPCE at 400 nm. IPCE values for 16 at.% Cr-doped hematite films were thirty times higher than that of undoped samples. This high photoelectrochemical performance of Cr-doped hematite films is mainly attributed to an improvement in charge carrier properties.

Remediation of metal-contaminated paddy soils by chemical washing with FeCl3 and citric acid

Batch extraction experiments were conducted to investigate the chemical washing of metal-contaminated paddy soils using mixtures of ferric chloride (FeCl3) and citric acid (CTA). The effects of the extractants (FeCl3, CTA, or FeCl3 + CTA) and washing cycles (single-step or multistep washing) on the metal removal efficiency were studied. FeCl3 + CTA increased metal removal efficiency to some extent compared to single FeCl3 or CTA. When the liquid-to-solid ratio was 2:1 with three washes and two rinses, a mixture of 10 mmol L−1 FeCl3 and 20 mmol L−1 CTA removed 78.9% Cd, 15.8% Cu, 34.0% Zn, and 18.1% Pb from a Typic Fe–accumuli–Stagnic Anthrosols. Using multistep washing instead of single-step increased the metal extraction effect. Moreover, the removal efficiency and speciation of metals in different soils and changes in soil properties in washed soils were also studied. The removal rate of Cd was higher than that of Zn, Cu, or Pb because of the higher proportions of acid-soluble forms of Cd in the soils. The removal of metals from different soils depended on the distribution of metal speciation and soil type. Soil pH, CEC, exchangeable Ca, and exchangeable Mg decreased significantly after soil washing. We conclude that chemical washing of metal-contaminated paddy soils with mixtures of FeCl3 and citric acid may be a feasible technique for soil remediation.

Treatment of the Iron Surface and its Corrosion Resistance

Preparation and corrosion resistance of iron plate with micro-nano-structure were investigated. A clean iron plate was etched with a mixture of FeCl3, H2O, hydrochloric acid, H2O2 and H3PO4 to form a super hydrophilic surface which was treated with fatty acid solution to form a micro-nano-structure surface on which the water contact angle was about 147°. The super hydrophilic surface was treated with 3-aminopropyltriethoxysilane solution and then fatty acid solution (test plate) to turn to a super hydrophobic surface and the water contact angle was greater than 150°. This test plate coated with alkyd vamish exhibited better corrosion resistance to H2SO4 than blank iron plate.

An in depth study of solvent effects on yield and average molecular weight in poly(3-hexylthiophene)

Poly(3-hexylthiophene) was synthesized by chemical oxidation using FeCl3 in chloroform, dichloromethane, acetonitrile, nitromethane, nitrobenzene and mixtures of these solvents. Comparative reactions for 1 day at room temperature were carried out to investigate solvent effects. Polymer samples and the remaining reaction solutions were analyzed by MALDI-MS and LDI-MS to determine Mw and reaction completeness, respectively. Solubilities of FeCl3, FeCl2, and P3HT in each pure solvent were measured and correlated to the results. Open circuit potentials of FeCl3 and mixtures of FeCl3 and FeCl2 in pure solvents were measured and compared to the experimentally determined oxidation potential of 3-hexylthiophene. An optimized solvent system for reproducible synthesis of high Mw P3HT with quantitative yields is proposed based on MS analysis results.

ChemInform Abstract: Solvothermal Synthesis of Pyrite FeS2 Nanocubes and Their Superior High Rate Lithium Storage Properties.

AbstractThe title nanocubes with particle sizes of around 80—120 nm are solvothermally synthesized from mixtures of FeCl2, sulfur powder, 1,2‐dodecanediol, and oleylamine (autoclave, 180 °C, 18 h), and characterized by powder XRD, SEM, TEM, Raman spectroscopy, and electrochemical measurements.

Study in synthesis and characterization of carbon nanotubes decorated by magnetic iron oxide nanoparticles

Magnetic nanoparticles iron oxide with average sizes of 6 nm were synthesized by a chemical coprecipitation method from mixtures of FeCl2·4H2O and FeCl3·6H2O. For preparation, multi-walled carbon nanotubes (MWCNTS) with outer diameter of 50 nm, wall thickness from 1 to 2 nm and length from 500–2,000 nm were used. Characterization of the MWCNT–Fe3O4 by X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscope (SEM), transmission electron microscope (TEM), thermo-gravimetric analysis (TGA) and magnetic characterization was conducted on a vibrating sample magnetometer (VSM).