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Volume 10, February

Inorganics, Volume 10, Issue 3 (March 2022) – 14 articles

Cover Story (view full-size image): Introduction: Iron–sulfur clusters (Fe–S or ISC) are essential inorganic cofactors that are required for a number of biological pathways. In mammals, the synthesis of Fe–S relies on mitochondrial function and a group of evolutionarily conserved mitochondrial proteins constituting the ISC pathway. The first step of the ISC pathway requires the de novo assembly of Fe–S within a dynamic core complex. Here, we review recent data on the function and association of different Fe–S core complex components and provide a model of the Fe–S assembly. We also briefly describe the genetic diseases that result from mutations in the Fe–S core complex components, including Friedreich’s ataxia. View this paper
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Review
A Comprehensive Study on the Applications of Clays into Advanced Technologies, with a Particular Attention on Biomedicine and Environmental Remediation
Inorganics 2022, 10(3), 40; https://doi.org/10.3390/inorganics10030040 - 21 Mar 2022
Viewed by 820
Abstract
In recent years, a great interest has arisen around the integration of naturally occurring clays into a plethora of advanced technological applications, quite far from the typical fabrication of traditional ceramics. This “second (technological) life” of clays into fields of emerging interest is [...] Read more.
In recent years, a great interest has arisen around the integration of naturally occurring clays into a plethora of advanced technological applications, quite far from the typical fabrication of traditional ceramics. This “second (technological) life” of clays into fields of emerging interest is mainly due to clays’ peculiar properties, in particular their ability to exchange (capture) ions, their layered structure, surface area and reactivity, and their biocompatibility. Since the maximization of clay performances/exploitations passes through the comprehension of the mechanisms involved, this review aims at providing a useful text that analyzes the main goals reached by clays in different fields coupled with the analysis of the structure-property correlations. After providing an introduction mainly focused on the economic analysis of clays global trading, clays are classified basing on their structural/chemical composition. The main relevant physicochemical properties are discussed (particular attention has been dedicated to the influence of interlayer composition on clay properties). Lastly, a deep analysis of the main relevant nonconventional applications of clays is presented. Several case studies describing the use of clays in biomedicine, environmental remediation, membrane technology, additive manufacturing, and sol-gel processes are presented, and results critically discussed. Full article
(This article belongs to the Special Issue New Advances into Nanostructured Oxides)
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Article
Improved Electrochemical Behavior and Thermal Stability of Li and Mn-Rich Cathode Materials Modified by Lithium Sulfate Surface Treatment
Inorganics 2022, 10(3), 39; https://doi.org/10.3390/inorganics10030039 - 20 Mar 2022
Viewed by 879
Abstract
High-energy cathode materials that are Li- and Mn-rich lithiated oxides—for instance, 0.35Li2MnO3.0.65LiNi0.35Mn0.45Co0.20O2 (HE-NCM)—are promising for advanced lithium-ion batteries. However, HE-NCM cathodes suffer from severe degradation during cycling, causing gradual capacity loss, [...] Read more.
High-energy cathode materials that are Li- and Mn-rich lithiated oxides—for instance, 0.35Li2MnO3.0.65LiNi0.35Mn0.45Co0.20O2 (HE-NCM)—are promising for advanced lithium-ion batteries. However, HE-NCM cathodes suffer from severe degradation during cycling, causing gradual capacity loss, voltage fading, and low-rate capability performance. In this work, we applied an effective approach to creating a nano-sized surface layer of Li2SO4 on the above material, providing mitigation of the interfacial side reactions while retaining the structural integrity of the cathodes upon extended cycling. The Li2SO4 coating was formed on the surface of the material by mixing it with nanocrystalline Li2SO4 and annealing at 600 °C. We established enhanced electrochemical behavior with ~20% higher discharge capacity, improved charge-transfer kinetics, and higher rate capability of HE-NCM cathodes due to the presence of the Li2SO4 coating. Online electrochemical mass spectrometry studies revealed lower CO2 and H2 evolution in the treated samples, implying that the Li2SO4 layer partially suppresses the electrolyte degradation during the initial cycle. In addition, a ~28% improvement in the thermal stability of the Li2SO4-treated samples in reactions with battery solution was also shown by DSC studies. The post-cycling analysis allowed us to conclude that the Li2SO4 phase remained on the surface and retained its structure after 100 cycles. Full article
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Project Report
Antimicrobial Activity of Silver, Copper, and Zinc Ions/Poly(Acrylate/Itaconic Acid) Hydrogel Matrices
Inorganics 2022, 10(3), 38; https://doi.org/10.3390/inorganics10030038 - 18 Mar 2022
Cited by 2 | Viewed by 618
Abstract
The design and use of new potent and specific antimicrobial systems are of crucial importance in the medical field. This will help relieve, fight, and eradicate infections and thus improve human health. The use of metals in various forms as antimicrobial therapeutics has [...] Read more.
The design and use of new potent and specific antimicrobial systems are of crucial importance in the medical field. This will help relieve, fight, and eradicate infections and thus improve human health. The use of metals in various forms as antimicrobial therapeutics has been known since ancient times. In this sense, polymeric hydrogel matrices as multifunctional materials and in combination with various metal forms can be a great alternative to conventional treatments for infections. Hydrogels possess high hydrophilicity, specific three-dimensional networks, fine biocompatibility, and cell adhesion and are therefore suitable as materials for the loading of active antimicrobial agents and acting in antimicrobial areas. The biocompatible nature of hydrogels’ matrices makes them a convenient starting platform to develop biocompatible, selective, active controlled-release antimicrobial materials. Hydrogels based on acrylate and itaconic acid were synthesized and loaded with silver (Ag+), copper (Cu2+), and zinc (Zn2+) ions as a controlled release and antimicrobial system to test release properties and antimicrobial activity in contact with microbes. The metal ions/hydrogel systems exhibited favorable biocompatibility, release profiles, and antimicrobial activity against methicillin-sensitive Staphylococcus aureus (MSSA), methicillin-resistant Staphylococcus aureus (MRSA), Staphylococcus aureus, Escherichia coli, and Candida albicans microbes, and have shown that they have the capacity to “fight” with the life-threatening infections. Antimicrobial activity depends on types of metal ions, the composition of polymeric matrices, as well as the types of microbes. Designed metal ions/poly(acrylate/itaconic acid) antimicrobial systems have shown to have good potential as antimicrobial therapeutics and suitable biomaterials for medical applications. Full article
(This article belongs to the Special Issue Metal-Based Antimicrobials)
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Article
Binuclear Heteroleptic Ru(III) Dithiocarbamate Complexes: A Step towards Tunable Antiproliferative Agents
Inorganics 2022, 10(3), 37; https://doi.org/10.3390/inorganics10030037 - 17 Mar 2022
Viewed by 818
Abstract
Binuclear dithiocarbamate complexes of Ru(III) are promising candidates in the search for outstanding metal-based anticancer agents. While different dithiocarbamates have shown ligand-dependent cytotoxicity in homoleptic binuclear Ru(III) complexes, the properties of heteroleptic analogues with different dithiocarbamate (DTC) ligands have yet to be explored. [...] Read more.
Binuclear dithiocarbamate complexes of Ru(III) are promising candidates in the search for outstanding metal-based anticancer agents. While different dithiocarbamates have shown ligand-dependent cytotoxicity in homoleptic binuclear Ru(III) complexes, the properties of heteroleptic analogues with different dithiocarbamate (DTC) ligands have yet to be explored. We herein propose the introduction of heteroleptic ligands as tunable features for the development of improved ruthenium-based antiproliferative agents and report a synthetic strategy for their synthesis as well as the evaluation of the cytotoxic activity of a selection of binuclear heteroleptic Ru(III) compounds towards MDA-MB-231 and PC3 cells. Full article
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Article
Nitrogen-Doped Carbon Flowers with Fe and Ni Dual Metal Centers for Effective Electroreduction of Oxygen
Inorganics 2022, 10(3), 36; https://doi.org/10.3390/inorganics10030036 - 11 Mar 2022
Viewed by 735
Abstract
Carbon-based nanocomposites have been attracting extensive attention as high-performance catalysts in alkaline media towards the electrochemical reduction of oxygen. Herein, polyacrylonitrile nanoflowers are synthesized via a free-radical polymerization route and used as a structural scaffold and precursor, whereby controlled pyrolysis leads to the [...] Read more.
Carbon-based nanocomposites have been attracting extensive attention as high-performance catalysts in alkaline media towards the electrochemical reduction of oxygen. Herein, polyacrylonitrile nanoflowers are synthesized via a free-radical polymerization route and used as a structural scaffold and precursor, whereby controlled pyrolysis leads to the ready preparation of carbon nanocomposites (FeNi-NCF) doped with both metal (Fe and Ni) and nonmetal (N) elements. Transmission electron microscopy studies show that the FeNi-NCF composites retain the flower-like morphology, with the metal species atomically dispersed into the flaky carbon petals. Remarkably, despite a similar structure, elemental composition, and total metal content, the FeNi-NCF sample with a high Fe:Ni ratio exhibits an electrocatalytic performance towards oxygen reduction reaction (ORR) in alkaline media that is similar to that by commercial Pt/C, likely due to the Ni to Fe electron transfer that promotes the adsorption and eventual reduction of oxygen, as evidenced in X-ray photoelectron spectroscopic measurements. Results from this study underline the importance of the electronic properties of metal dopants in the manipulation of the ORR activity of carbon nanocomposites. Full article
(This article belongs to the Special Issue Inorganic Materials for Fuel Cell Electrocatalysts)
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Article
Phenolic 3° Phosphine Oxides as a Class of Metal-Free Catalysts for the Activation of C–O Bonds in Aliphatic Alcohols: Direct Synthesis of Catalyst Candidates, and Kinetic Studies
Inorganics 2022, 10(3), 35; https://doi.org/10.3390/inorganics10030035 - 11 Mar 2022
Viewed by 1197
Abstract
It was recently reported that a (2-hydroxybenzyl)phosphine oxide (2-HOBPO) can serve as a phosphorus-centered catalyst for the stereo-invertive coupling of aliphatic alcohols and acidic pronucleophiles (akin to a Mitsunobu reaction, but without additional reagents). Herein, we report an improved synthesis, which provides direct [...] Read more.
It was recently reported that a (2-hydroxybenzyl)phosphine oxide (2-HOBPO) can serve as a phosphorus-centered catalyst for the stereo-invertive coupling of aliphatic alcohols and acidic pronucleophiles (akin to a Mitsunobu reaction, but without additional reagents). Herein, we report an improved synthesis, which provides direct access to systematically varied 2-HOBPOs in a single step from commercially available precursors (salicylaldehydes and secondary phosphines). The efficiency and generality of the synthetic method enabled limited structure–activity relationship (SAR) studies, from which it was determined that substituents on both the phenolic and phosphine oxide portions can exert significant influence on the turnover frequency (TOF) of each catalyst. Importantly, for all catalytically active 2-HOBPOs examined, the molecularity of catalyst in the rate law of the alcohol coupling was determined to be <1. Thus, for high catalyst loadings, differences in catalytic activity between 2-HOBPOs appear to be dominated by differences in catalytic auto-inhibition, while for low catalyst loadings, differences are attributed to inherent differences in the energetic span of the catalytic cycle, ignoring off-cycle species, in good agreement with density functional theory (DFT) modeling at the ωB97X-D/6-311G(d,p) level. Full article
(This article belongs to the Special Issue Bond Activation and Catalysis Using Main-Group Elements)
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Article
Bimetallic Copper-Silver Systems Supported on Natural Clinoptilolite: Long-Term Changes in Nanospecies’ Composition and Stability
Inorganics 2022, 10(3), 34; https://doi.org/10.3390/inorganics10030034 - 04 Mar 2022
Viewed by 728
Abstract
Long-term changes in species of copper-silver bimetallic systems on natural clinoptilolite obtained by ion exchange of Cu2+ and Ag+ and then reduced at different temperatures were studied. Even after storage under ambient conditions, XRD and UV-Vis diffuse reflectance spectra indicate the [...] Read more.
Long-term changes in species of copper-silver bimetallic systems on natural clinoptilolite obtained by ion exchange of Cu2+ and Ag+ and then reduced at different temperatures were studied. Even after storage under ambient conditions, XRD and UV-Vis diffuse reflectance spectra indicate the presence of nanospecies and larger particles of reduced copper and silver. Scanning electron microscopy of aged bimetallic samples, reduced at the highest temperature (450 °C) and the pristine sample for their preparation, also aged, showed the presence of silver particles with a size of about 100 nm. They are formed in the initial ion-exchanged sample (without reduction) due to the degradation of Ag+ ions. The particles in the reduced sample are larger; in both samples they are evenly distributed over the surface. The presence of silver affects the stability and the mechanism of decomposition/oxidation of reduced copper species, and this stability is higher in bimetallic systems. The decomposition pattern of recently reduced species includes the formation of smaller nanoparticles and few-atomic clusters. This can occur, preceding the complete oxidation of Cu to ions. Quasicolloidal silver, which is present in fresh bimetallic samples reduced at lower temperatures, transforms after aging into Ag8 clusters, which indicates the stability of these nanospecies on natural clinoptilolite. Full article
(This article belongs to the Section Inorganic Solid-State Chemistry)
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Article
Low-Temperature and Additive-Free Synthesis of Spherical MIL-101(Cr) with Enhanced Dye Adsorption Performance
Inorganics 2022, 10(3), 33; https://doi.org/10.3390/inorganics10030033 - 04 Mar 2022
Viewed by 691
Abstract
The chromium-benzenedicarboxylate metal–organic framework (MOF), MIL-101(Cr), is one of the most well-investigated and widely used prototypical MOFs. Regarding its synthesis, the use of a toxic modulator (usually HF) and high reaction temperature (220 °C) are the main factors hindering its further expansion of [...] Read more.
The chromium-benzenedicarboxylate metal–organic framework (MOF), MIL-101(Cr), is one of the most well-investigated and widely used prototypical MOFs. Regarding its synthesis, the use of a toxic modulator (usually HF) and high reaction temperature (220 °C) are the main factors hindering its further expansion of production and utilization. In fact, high quality MIL-101(Cr) crystals can be prepared at a much lower temperature (160 °C) with spherical morphology via an additive-free approach. Compared to traditional octahedral MIL-101(Cr), the spherical MIL-101(Cr) possesses higher adsorption performance toward dye molecules, including methyl orange (MO) and rhodamine B (RB). The results suggest that toxic additives and high reaction temperatures are not essential in the synthesis of MIL-101(Cr), and the fabrication of spherical MIL-101(Cr) may offer a facile and effective pathway for the large-scale industrial application of MIL-101(Cr). Full article
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Article
One-Dimensional Gadolinium (III) Complexes Based on Alpha- and Beta-Amino Acids Exhibiting Field-Induced Slow Relaxation of Magnetization
Inorganics 2022, 10(3), 32; https://doi.org/10.3390/inorganics10030032 - 03 Mar 2022
Cited by 1 | Viewed by 733
Abstract
Gadolinium (III) complexes exhibiting slow relaxation of magnetization are uncommon and have been much less studied than other compounds based on anisotropic lanthanide (III) ions. We prepared two one-dimensional gadolinium (III) complexes based on α-glycine (gly) and β-alanine (β-ala) amino acids, with the [...] Read more.
Gadolinium (III) complexes exhibiting slow relaxation of magnetization are uncommon and have been much less studied than other compounds based on anisotropic lanthanide (III) ions. We prepared two one-dimensional gadolinium (III) complexes based on α-glycine (gly) and β-alanine (β-ala) amino acids, with the formula {[Gd2(gly)6(H2O)4](ClO4)6·5H2O}n (1) and {[Gd2(β-ala)6(H2O)4](ClO4)6·H2O}n (2), which were magneto-structurally characterized. Compounds 1 and 2 crystallize in the triclinic system (space group Pī). In complex 1, two Gd (III) ions are eight-coordinate and bound to six oxygen atoms from six gly ligands and two oxygen atoms from two water molecules, the metal ions showing different geometries (bicapped trigonal prism and square antiprism). In complex 2, two Gd (III) ions are nine-coordinate and bound to seven oxygen atoms from six β-ala ligands and two oxygen atoms from two water molecules in the same geometry (capped square antiprism). Variable-temperature dc magnetic susceptibility measurements performed on microcrystalline samples of 1 and 2 show similar magnetic behavior for both compounds, with antiferromagnetic coupling between the Gd (III) ions connected through carboxylate groups. Ac magnetic susceptibility measurements reveal slow relaxation of magnetization in the presence of an external dc field in both compounds, hence indicating the occurrence of the field-induced single-molecule magnet (SMM) phenomenon in both 1 and 2. Full article
(This article belongs to the Special Issue Lanthanide Single-Molecule Magnets)
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Review
Mitochondrial De Novo Assembly of Iron–Sulfur Clusters in Mammals: Complex Matters in a Complex That Matters
Inorganics 2022, 10(3), 31; https://doi.org/10.3390/inorganics10030031 - 26 Feb 2022
Viewed by 1071
Abstract
Iron–sulfur clusters (Fe–S or ISC) are essential cofactors that function in a wide range of biological pathways. In mammalian cells, Fe–S biosynthesis primarily relies on mitochondria and involves a concerted group of evolutionary-conserved proteins forming the ISC pathway. In the early stage of [...] Read more.
Iron–sulfur clusters (Fe–S or ISC) are essential cofactors that function in a wide range of biological pathways. In mammalian cells, Fe–S biosynthesis primarily relies on mitochondria and involves a concerted group of evolutionary-conserved proteins forming the ISC pathway. In the early stage of the ISC pathway, the Fe–S core complex is required for de novo assembly of Fe–S. In humans, the Fe–S core complex comprises the cysteine desulfurase NFS1, the scaffold protein ISCU2, frataxin (FXN), the ferredoxin FDX2, and regulatory/accessory proteins ISD11 and Acyl Carrier Protein (ACP). In recent years, the field has made significant advances in unraveling the structure of the Fe–S core complex and the mechanism underlying its function. Herein, we review the key recent findings related to the Fe–S core complex and its components. We highlight some of the unanswered questions and provide a model of the Fe–S assembly within the complex. In addition, we briefly touch on the genetic diseases associated with mutations in the Fe–S core complex components. Full article
(This article belongs to the Special Issue Assembly and Reactivity of Iron–Sulfur Clusters)
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Article
Hydrogenation of Carbon Dioxide to Formate Using a Cadmium-Based Metal–Organic Framework Impregnated with Nanoparticles
Inorganics 2022, 10(3), 30; https://doi.org/10.3390/inorganics10030030 - 25 Feb 2022
Viewed by 973
Abstract
The burning of fossil fuels to meet energy demands has increased carbon dioxide (CO2) in the atmosphere, causing global warming and associated climate change. Therefore, new materials are being developed to capture CO2 effectively, limit its impact on the environment, [...] Read more.
The burning of fossil fuels to meet energy demands has increased carbon dioxide (CO2) in the atmosphere, causing global warming and associated climate change. Therefore, new materials are being developed to capture CO2 effectively, limit its impact on the environment, and store and/or utilise it as an abundant C1 building block. In this study, we investigate a cadmium(II) metal–organic framework, [Cd(bdc)(DMF)]n (MOF1), synthesised by treating benzene-1,4-dicarboxylic acid with four equivalents of [Cd(NO3)2]. MOF1 was then used to support Pd, Ni, and Pt nanoparticles in forming MOF1/Pd MOF1/Ni and MOF1/Pt, respectively. These MOF-based materials were characterised using powder X-ray diffraction (PXRD), Fourier-transform infrared (FTIR), energy-dispersive X-ray spectroscopy (EDX), selected area electron diffraction (SAED), and high-resolution transmission electron microscopy (HR-TEM). MOF1/Pd MOF1/Ni and MOF1/Pt proved highly active in the catalytic hydrogenation of CO2 to formate selectively; in contrast, MOF1 did not hydrogenate CO2 to formate. The MOF1/Pd, MOF1/Ni, and MOF1/Pt catalysts produced formate selectively, with the highest TON of 1500 (TOF of 69 h−1) achieved using MOF1/Pd as the catalyst at 170 °C within 2 h. A formate yield of 98% was obtained, which demonstrates that the combination of nanoparticles and MOFs greatly enhances the catalytic activity of the active sites. Full article
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Article
A High-Performing Nanostructured Ir Doped-TiO2 for Efficient Photocatalytic Degradation of Gaseous Toluene
Inorganics 2022, 10(3), 29; https://doi.org/10.3390/inorganics10030029 - 25 Feb 2022
Cited by 2 | Viewed by 871
Abstract
TiO2-based photocatalysts still have some limitations such as large bandgap and low surface area, leading to low efficiency in the photocatalytic degradation of VOCs and limiting it to use in sunlight. Here we report that the nanostructured Ir-doped TiO2 as [...] Read more.
TiO2-based photocatalysts still have some limitations such as large bandgap and low surface area, leading to low efficiency in the photocatalytic degradation of VOCs and limiting it to use in sunlight. Here we report that the nanostructured Ir-doped TiO2 as an efficient photocatalyst generates an excellent risk-reduction material of gaseous toluene. We have succeeded in developing a nanostructured Ir-doped TiO2 and initially found that excellent efficient photocatalytic VOC decomposition can be achieved in our materials The nanostructured Ir-doped TiO2 was synthesized by a one pot, low temperature hydrothermal process with different ratios of Ir doped into the TiO2. It exhibited a high surface area, uniformly spherical morphology of 10–15 nm. Its activity for the photocatalytic degradation of gaseous toluene exhibited up to 97.5% under UV light. This enhancement could be explained by iridium doping which created a high concentration oxygen vacancy and changed the recombination rate of the photogenerated charge carriers. More generally, our study indicates a strategic way to develop the novel nanostructured material for numerous applications. Full article
(This article belongs to the Special Issue Novel Functional Ceramics)
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Article
Trigonal Bipyramidal Rhodium(I) Methyl and Phenyl Complexes: Precursors of Oxidative Methyl and Phenyl Radical Generation
Inorganics 2022, 10(3), 28; https://doi.org/10.3390/inorganics10030028 - 24 Feb 2022
Viewed by 710
Abstract
The new complexes [Rh(Me)(trop3P)] (2) and [Rh(Ph)(trop3P)] (3) (trop = 5H-dibenzo[a,d]cyclohepten-5-yl) were synthesised by addition of organolithium reagents (MeLi and PhLi) to the parent pentacoordinated chloride complex [RhCl(trop3P)]. The [...] Read more.
The new complexes [Rh(Me)(trop3P)] (2) and [Rh(Ph)(trop3P)] (3) (trop = 5H-dibenzo[a,d]cyclohepten-5-yl) were synthesised by addition of organolithium reagents (MeLi and PhLi) to the parent pentacoordinated chloride complex [RhCl(trop3P)]. The compounds have a trigonal bipyramidal structure with olefin-only ligands in the equatorial position and the methyl or phenyl substituent in the axial position. Oxidation of complexes 2 and 3 leads to the liberation of methyl and phenyl radicals, which were indirectly detected by reaction with common spin trapping reagents. Full article
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Article
Synthesis of MOFs for RhB Adsorption from Wastewater
Inorganics 2022, 10(3), 27; https://doi.org/10.3390/inorganics10030027 - 24 Feb 2022
Viewed by 678
Abstract
Fe-MOFs were prepared using a solvothermal method, and were characterized by scanning electron microscopy. We explored the application of Fe-MOFs as an adsorbing material for the removal of Rhodamine B (RhB) from aqueous solutions. The experimental data were simulated by dynamics and the [...] Read more.
Fe-MOFs were prepared using a solvothermal method, and were characterized by scanning electron microscopy. We explored the application of Fe-MOFs as an adsorbing material for the removal of Rhodamine B (RhB) from aqueous solutions. The experimental data were simulated by dynamics and the results showed that the pseudo–second-order kinetics model was appropriate for analysis of RhB removal. We studied the adsorption capacity of MOF materials under different masses, concentrations, and pH conditions. When the pH was 6, the maximum adsorption capacity within 4 h was 135 mg/g. In summation, the removal of RhB from wastewater using MOFs is feasible, inexpensive, and effective. Hence, our findings indicate that MOFs have a broad application in the purification of wastewater. Full article
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