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Partial substitution of V by other transition metals in Na3 V2 (PO4 )3 (NVP) can improve the electrochemical performance of NVP as a cathode for sodium-ion batteries (SIBs). Herein, phosphate Na-V-Mn-Ni-containing composites based on NASICON (Natrium Super Ionic Conductor)-type structure have been fabricated by sol-gel method. The synchrotron-based X-ray study, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) studies show that manganese/nickel combinations successfully substitute the vanadium in its site within certain limits. Among the received samples, composite based on Na3.83 V1.17 Mn0.58 Ni0.25 (PO4 )3 (VMN-0.5, 108.1 mAh g-1 at 0.2 C) shows the highest electrochemical ability. The cyclic voltammetry, galvanostatic intermittent titration technique, in situ XRD, ex situ XPS, and bond valence site energy calculations exhibit the kinetic properties and the sodium storage mechanism of VMN-0.5. Moreover, VMN-0.5 electrode also exhibits excellent electrochemical performance in quasi-solid-state sodium metal batteries with PVDF-HFP quasi-solid electrolyte membranes. The presented work analyzes the advantages of VMN-0.5 and the nature of the substituted metal in relation to the electrochemical properties of the NASICON-type structure, which will facilitate further commercialization of SIBs.
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Garnet-type Li7 La3 Zr2 O12 (LLZO) solid-state electrolytes hold great promise for the next-generation all-solid-state batteries. An in-depth understanding of the phase transformation during synthetic processes is required for better control of the crystallinity and improvement of the ionic conductivity of LLZO. Herein, the phase transformation pathways and the associated surface amorphization are comparatively investigated during the sol-gel and solid-state syntheses of LLZO using in situ heating transmission electron microscopy (TEM). The combined ex situ X-ray diffraction and in situ TEM techniques are used to reveal two distinct phase transformation pathways (precursors â La2 Zr2 O7 â LLZO and precursors â LLZO) and the subsequent layer-by-layer crystal growth of LLZO on the atomic scale. It is also demonstrated that the surface amorphization surrounding the LLZO crystals is sensitive to the postsynthesis cooling rate and significantly affects the ionic conductivity of pelletized LLZO. This work brings up a critical but often overlooked issue that may greatly exacerbate the Li-ion conductivity by undesired synthetic conditions, which can be leveraged to ameliorate the overall crystallinity to improve the electrochemical performance of LLZO. These findings also shed light on the significance of optimizing surface structure to ensure superior performance of Li-ion conductors.
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We present a study on the green synthesis of undoped and Er-doped ZnO compounds using Mangifera indica gum (MI). A set of tests were conducted to assess the structure of the material. The tests included X-ray diffraction, Raman, and Fourier-transform infrared spectroscopy. Optical properties were studied using diffuse reflectance and photoluminescence. Morphological and textural investigations were done using SEM images and N2 adsorption/desorption. Furthermore, photocatalytic tests were performed with methylene blue (MB), yellow eosin (EY), and the pharmaceutical drug ibuprofen (IBU) under UV irradiation. The study demonstrated that replacing the stabilizing agent with Mangifera indica gum is an effective method for obtaining ZnO nanoparticles. Additionally, the energy gap of the nanoparticles exhibits a slight reduction in value. Photoluminescence studies showed the presence of zinc vacancies and other defects in both samples. In the photocatalytic test, the sample containing Er3+ exhibited a degradation of 99.7% for methylene blue, 81.2% for yellow eosin, and 52.3% for ibuprofen over 120 min. In the presence of methyl alcohol, the degradation of MB and EY dyes is 16.7% and 55.7%, respectively. This suggests that hydroxyl radicals are responsible for the direct degradation of both dyes. In addition, after the second reuse, the degradation rate for MB was 94.08%, and for EY, it was 82.35%. For the third reuse, the degradation rate for MB was 97.15%, and for EY, it was 17%. These results indicate the significant potential of the new semiconductor in environmental remediation applications from an ecological synthesis.
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Mangifera , Nanopartículas , Óxido de Zinco , Amarelo de Eosina-(YS) , Azul de Metileno , Fotólise , Ibuprofeno , CorantesRESUMO
The sol-gel method, adapted to aqueous media, was used for the synthesis of BaMn0.7Cu0.3O3 (BMC) and Ba0.9A0.1Mn0.7Cu0.3O3 (BMC-A, A = Ce, La or Mg) perovskite-type mixed oxides. These samples were fully characterized by ICP-OES, XRD, XPS, H2-TPR, BET, and O2-TPD and, subsequently, they were evaluated as catalysts for CO oxidation under different conditions simulating that found in cars exhaust. The characterization results show that after the partial replacement of Ba by A metal in BMC perovskite: (i) a fraction of the polytype structure was converted to the hexagonal BaMnO3 perovskite structure, (ii) A metal used as dopant was incorporated into the lattice of the perovskite, (iii) oxygen vacancies existed on the surface of samples, and iv) Mn(IV) and Mn(III) coexisted on the surface and in the bulk, with Mn(IV) being the main oxidation state on the surface. In the three reactant atmospheres used, all samples catalysed the CO to CO2 oxidation reaction, showing better performances after the addition of A metal and for reactant mixtures with low CO/O2 ratios. BMC-Ce was the most active catalyst because it combined the highest reducibility and oxygen mobility, the presence of copper and of oxygen vacancies on the surface, the contribution of the Ce(IV)/Ce(III) redox pair, and a high proportion of surface and bulk Mn(IV). At 200 °C and in the 0.1% CO + 10% O2 reactant gas mixture, the CO conversion using BMC-Ce was very similar to the achieved with a 1% Pt/Al2O3 (Pt-Al) reference catalyst.
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In the present investigation of copper ferrite, a CuFe2O4 nanocomposite adsorbent was synthesized using the sol-gel method, and its relevance in the adsorptive elimination of the toxic Congo red (CR) aqueous phase was examined. A variety of structural methods were used to analyze the CuFe2O4 nanocomposite; the as-synthesized nanocomposite had agglomerated clusters with a porous, irregular, rough surface that could be seen using FE-SEM, and it also contained carbon (23.47%), oxygen (44.31%), copper (10.21%), and iron (22.01%) in its elemental composition by weight. Experiments were designed to achieve the most optimized system through the utilization of a central composite design (CCD). The highest uptake of CR dye at equilibrium occurred when the initial pH value was 5.5, the adsorbate concentration was 125 mg/L, and the adsorbent dosage was 3.5 g/L. Kinetic studies were conducted, and they showed that the adsorption process followed a pseudo-second-order (PSO) model (regression coefficient, R2 = 0.9998), suggesting a chemisorption mechanism, and the overall reaction rate was governed by both the film and pore diffusion of adsorbate molecules. The process through which dye molecules were taken up onto the particle surface revealed interactions involving electrostatic forces, hydrogen bonding, and pore filling. According to isotherm studies, the equilibrium data exhibited strong agreement with the Langmuir model (R2 = 0.9989), demonstrating a maximum monolayer adsorption capacity (qmax) of 64.72 mg/g at pH 6 and 302 K. Considering the obtained negative ΔG and positive ΔHads and ΔSads values across all tested temperatures in the thermodynamic investigations, it was confirmed that the adsorption process was characterized as endothermic, spontaneous, and feasible, with an increased level of randomness. The CuFe2O4 adsorbent developed in this study is anticipated to find extensive application in effluent treatment, owing to its excellent reusability and remarkable capability to effectively remove CR in comparison to other adsorbents.
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The rapid depletion of fossil fuels and environmental pollution has motivated scientists to cultivate renewable and green energy sources. The hydrogen economy is an emerging replacement for fossil fuels, and photocatalytic water splitting is a suitable strategy to produce clean hydrogen fuel. Herein, the photocatalyst (PdO.TiO2) is introduced as an accelerated photoelectrochemical oxygen evolution reaction (OER). The catalyst showed significant improvement in the current density magnitude from 0.89 (dark) to 4.27 mA/cm2 (light) during OER at 0.5 V applied potential. The as-synthesized material exhibits a Tafel slope of 170 mVdec-1 and efficiency of 0.25% at 0.93 V. The overall outcomes associated with the photocatalytic activity of PdO.TiO2 demonstrated that the catalyst is highly efficient, thereby encouraging researchers to explore more related catalysts for promoting facile OER.
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Spinel LiMn2O4 (LMO) is a state-of-the-art cathode material for Li-ion batteries. However, the operating voltage and battery life of spinel LMO needs to be improved for application in various modern technologies. Modifying the composition of the spinel LMO material alters its electronic structure, thereby increasing its operating voltage. Additionally, modifying the microstructure of the spinel LMO by controlling the size and distribution of the particles can improve its electrochemical properties. In this study, we elucidate the sol-gel synthesis mechanisms of two common types of sol-gels (modified and unmodified metal complexes)-chelate gel and organic polymeric gel-and investigate their structural and morphological properties and electrochemical performances. This study highlights that uniform distribution of cations during sol-gel formation is important for the growth of LMO crystals. Furthermore, a homogeneous multicomponent sol-gel, necessary to ensure that no conflicting morphologies and structures would degrade the electrochemical performances, can be obtained when the sol-gel has a polymer-like structure and uniformly bound ions; this can be achieved by using additional multifunctional reagents, namely cross-linkers.
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The accumulation of Cr(VI) ions in water can cause serious influences on the environment and human health. This work reports a humble synthesis of ZnSe nanoparticles anchored to the sol-gel prepared TiO2for visible-light-driven photocatalytic reduction of Cr(VI) ions. The 7.9 nm ZnSe nanoparticles were attached to TiO2surfaces at a content of 1.0-4.0 wt% as experiential by TEM investigation. The designed nanocomposite unveiled mesostructured surfaces exhibiting surface areas of 176-210 m2g-1. The impregnation of ZnSe amended the visible-light absorption of TiO2due to the bandgap decrease from 3.14 to 2.90 eV. The photocatalytic reduction of Cr(VI) applying the optimized portion of 3.0 wt% ZnSe/TiO2was achieved at 177µmol min-1. This photocatalytic activity is higher than the common Degussa P25 and pristine TiO2by 20 and 30 times, respectively. The improved performance is signified by the efficient interfacial separation of charge carriers by the introduction of ZnSe. This innovative ZnSe/TiO2has also shown photocatalytic stability for five consecutive runs.
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Currently, metal oxide photocatalysts is a green and facile tool for the elimination of emerging pollutants utilizing light illumination. Though, the wide bandgap energy (Eg), rapid recombination of photogenerated carriers, and photostability of these oxides represent critical issues before the actual application. Herein, we familiarise a sol-gel based synthesis of ZnO hexagonal nanoplatelets modified with CoFe2O4 (CFO) nanoparticles at minor loading (1.0-4.0 wt %) to yield CFO/ZnO nanoheterojunctions. The CFO/ZnO unveiled mesostructured surfaces at surface areas of 102-120 m2 g-1 and photoactive in the visible region with high. The CFO addition to ZnO reduced its Eg from 3.14 to 2.66 eV. The formed nanoheterojunctions were applied to remediate ciprofloxacin (CPF), as an antibiotic pollutant in wastewater. The 2.4 g L-1 3.0 wt % CFO-added ZnO exhibited a 100% removal of 10-ppm CPF within 45 min of visible-light irradiation and sustainable recycling ability for five consecutive runs at 97%. The sustainable performance of CFO/ZnO is ascribed to the suppression of photogenerated carriers and reduction of E by p-n nanoheterojunction formation. This study broadens the way for nanoheterojunction oxides for the destruction of pharmaceutical wastes under visible-light illumination.
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Óxido de Zinco , Catálise , Ciprofloxacina , Cobalto , Compostos Férricos , Luz , ÁguaRESUMO
Hexanary high-entropy oxides (HEOs) were synthesized through the mechanochemical sol-gel method for electrocatalytic water oxidation reaction (WOR). As-synthesized catalysts were subjected to characterization, including X-ray diffraction (XRD), Fourier transforms infrared (FTIR) analysis, and scanning electron microscopy (SEM). All the oxide systems exhibited sharp diffraction peaks in XRD patterns indicating the defined crystal structure. Strong absorption between 400-700 cm-1 in FTIR indicated the formation of metal-oxide bonds in all HEO systems. WOR was investigated via cyclic voltammetry using HEOs as electrode platforms, 1M KOH as the basic medium, and 1M methanol (CH3OH) as the facilitator. Voltammetric profiles for both equiatomic (EHEOs) and non-equiatomic (NEHEOs) were investigated, and NEHEOs exhibited the maximum current output for WOR. Moreover, methanol addition improved the current profiles, thus leading to the electrode utility in direct methanol fuel cells as a sequential increase in methanol concentration from 1M to 2M enhanced the OER current density from 61.4 to 94.3 mA cm-2 using NEHEO. The NEHEOs comprising a greater percentage of Al, ([Al0.35(Mg, Fe, Cu, Ni, Co)0.65]3O4) displayed high WOR catalytic performance with the maximum diffusion coefficient, D° (10.90 cm2 s-1) and heterogeneous rate constant, k° (7.98 cm s-1) values. These primary findings from the EC processes for WOR provide the foundation for their applications in high-energy devices. Conclusively, HEOs are proven as novel and efficient catalytic platforms for electrochemical water oxidation.
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Hybrid tannic acid-silica-based porous nanoparticles, TA-SiO2 NPs, have been synthesized under mild conditions in the presence of green and renewable tannic acid biopolymer, a glycoside polymer of gallic acid present in a large part of plants. Tannic acid (TA) was exploited as both a structuring directing agent and green chelating site for heavy metal ions recovery from aqueous solutions. Particles morphologies and porosity were easily tuned by varying the TA initial amount. The sample produced with the largest TA amount showed a specific surface area an order of magnitude larger than silica nanoparticles. The adsorption performance was investigated by using TA-SiO2 NPs as adsorbents for copper (II) ions from an aqueous solution. The effects of the initial Cu2+ ions concentration and the pH values on the adsorption capability were also investigated. The resulting TA-SiO2 NPs exhibited a different adsorption behaviour towards Cu2+, which was demonstrated through different tests. The largest adsorption (i.e., ~50 wt% of the initial Cu2+ amount) was obtained with the more porous nanoplatforms bearing a higher final TA content. The TA-nanoplatforms, stable in pH value around neutral conditions, can be easily produced and their use would well comply with a green strategy to reduce wastewater pollution.
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Metais Pesados , Nanopartículas , Adsorção , Nanopartículas/química , Dióxido de Silício/química , Taninos/químicaRESUMO
The aim of this investigation was to synthesize high porosity TiO2 aerogel by applying sol-gel and subcritical drying methods and to identify the influence of reagent's nature and synthesis conditions on their structural and optical properties. Methods of XRD, FT-IR, BET, STA, SEM, and UV-vis were applied to investigate and compare the properties of synthesized TiO2 aerogels and to determine the most effective synthesis route. The structural parameters of the synthesized materials can be varied by changing the precursor type (titanium (IV), isopropoxide (TIP), or tetrabutylorthotitanate (TBOT)) and the nature of the solvent used for additional exchange (n-hexane (nH), cyclohexane (CH), or diethyl ether (DE)). All of the subcritical dried samples show the amorphous structure, which tends to crystallize into the anatase phase after calcination. The number of micro and mesopores and the specific surface area depends on the synthesis conditions. The pores with the highest diameter have been found for additionally nH exchanged and aged aerogel synthesized from precursor TIP. Despite the imperfections in the structure, the produced aerogels show structural and optical properties typical of the TiO2 structures mentioned in the literature.
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Nitrogen-doped and heteroatom multi-doped carbon materials are considered excellent metal-free catalysts, superior catalyst supports for transition metal particles and single metal atoms (single-atom catalysts), as well as efficient sorbents for gas- and liquid-phase substances. Acid-catalyzed sol-gel polycondensation of hydroxybenzenes with heterocyclic aldehydes yields cross-linked thermosetting resins in the form of porous organic polymers (i.e., organic gels). Depending on the utilized hydroxybenzene (e.g., phenol, resorcinol, phloroglucinol, etc.) and heterocyclic aldehyde variety of heteroatom-doped organic polymers can be produced. Upon pyrolysis, highly porous and heteroatom-doped carbons are obtained. Herein, polycondensation of phloroglucinol with imidazole-2-carboxaldehyde (and other, similar heterocyclic aldehydes with two heteroatoms in the aromatic ring) is utilized to obtain porous, N-doped organic and carbon gels with N-content of up to 16.5 and 12 wt.%, respectively. Utilization of a heterocyclic aldehyde with two different heteroatoms yields dually-doped carbon materials. Upon pyrolysis, the porous polymers yield ultramicroporous N-doped and N,S co-doped carbons with specific surface areas of up to 800 m2g-1. The influence of the initial composition of reactants and the pyrolysis temperature on the structure and chemical composition of the final doped organic and carbon materials is studied in detail.
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Carbono/química , Imidazóis/química , Nitrogênio/química , Polímeros/química , Catálise , Géis/química , Porosidade , Pirólise , TemperaturaRESUMO
Efficient Lewis-acid-catalyzed direct conversion of aldehydes to 1,2-diketones in the liquid phase was enabled by using newly designed and developed ceria-zirconia-based high-entropy oxides (HEOs) as the actual catalysts. The synergistic effect of various cations incorporated in the same oxide structure (framework) was partially responsible for the efficiency of multicationic materials compared to the corresponding single-cation oxide forms. Furthermore, a clear, linear relationship between the Lewis acidity and the catalytic activity of the HEOs was observed. Due to the developed strategy, exclusively diketone-selective, recyclable, versatile heterogeneous catalytic transformation of aldehydes can be realized under mild reaction conditions.
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Organosilicas with chemically immobilized 3-aminopropyl and Methyl Red-containing surface groups were prepared by sol-gel condensation of tetraethyl orthosilicate and (3-aminopropyl)triethoxysilane in the presence of dye as part of the mixed micelles or dye-containing silane as silica source. The hexagonally arranged mesoporous structure of synthesized materials was confirmed by low-temperature nitrogen adsorption-desorption, x-ray diffraction, and TEM studies. Chemical composition of MCM-41-type organosilicas was established by FT-IR spectroscopy and chemical analysis of surface layer. Sorption of Methyl Red by organosilicas was studied from diluted phosphate buffer solutions in dependence of medium pH, duration of contact, and equilibrium concentration of dye. It was found that effective removal of Methyl Red takes place at pH values within a range of 2.5-5. Kinetic curves of Methyl Red sorption on organosilicas were analyzed by the Lagergren, Ho-McKey, and Weber-Morris kinetic models. It was found that the pseudo-second-order model fits the kinetics of Methyl Red sorption on all synthesized materials and the intraparticle diffusion is not the only one mechanism controlling the rate of Methyl Red sorptive removal. The parameters of equilibrium sorption of Methyl Red on organosilicas of MCM-41 type were calculated using Langmuir, Freundlich, Redlich-Peterson, and Brunauer-Emmett-Teller models. Sorption of acid dyes with geometry similar or substantially different from Methyl Red on mesoporous silicas was studied from single and binary component mixtures in aqueous solutions with pH 4.8 and 5.5. It was found that selective sorption process is highly dependent on the structural characteristics and protolytic state of silica surface as well as acid dye.
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Compostos Azo , Dióxido de Silício , Adsorção , Concentração de Íons de Hidrogênio , Cinética , Soluções , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Organosilanes (e.g., R'-SiOR3) provide hydrophobic functionality in thin-film coatings, porous gels, and particles. Compared with tetraalkoxysilanes (SiOR4), organosilanes exhibit distinct reaction kinetics and assembly mechanisms arising from steric and electronic properties of the R' group on the silicon atom. Here, the hydrolysis and condensation pathways of n-propyltrimethoxy silane (nPM) and a tri-fluorinated analog of nPM, 3,3,3-trifluoropropyl trimethoxy silane (3F), were investigated under aqueous conditions at pH 1.7, 2.0, 3.0, and 4.0. Prior to hydrolysis, 3F and nPM are insoluble in water and form a lens at the bottom (3F) or top (nPM) of the solutions. This phase separation was employed to follow reaction kinetics using a Turbiscan instrument to monitor hydrolysis through solubilization of the neat silane lens while simultaneously tracking condensation-induced turbidity throughout the bulk solution. Dynamic light scattering confirmed the silane condensation and particle aggregation processes reported by the turbidity scanning. Employing macroscopic phase separation of the starting reactants from the solvent further allows for control over the reaction kinetics, as the interfacial area can be readily controlled by reaction vessel geometry, namely by controlling the surface area to volume. In-situ turbidity scanning and dynamic light scattering revealed distinct reaction kinetics for nPM and 3F, attributable to the electron withdrawing and donating nature of the fluoro- and organo-side chains of 3F and nPM, respectively.
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Difusão Dinâmica da Luz , Géis/química , Transição de Fase , Silanos/química , Soluções/química , Fenômenos Químicos , Difusão Dinâmica da Luz/métodos , Concentração de Íons de Hidrogênio , Hidrólise , Interações Hidrofóbicas e Hidrofílicas , Cinética , Nanopartículas/químicaRESUMO
Next generation electrochemical energy storage materials that enable a combination of high specific energy, specific power, and cycling stability can be obtained by a hybridization approach. This involves electrode materials that contain carbon and metal oxide phases linked on a nanoscopic level and combine characteristics of supercapacitors and batteries. The combination of the components requires careful design to create synergistic effects for an increased electrochemical performance. Improved understanding of the role of carbon as a substrate has advanced the power handling and cycling stability of hybrid materials significantly in recent years. This Concept outlines different design strategies for the design of hybrid electrode materials: (1)â the deposition of metal oxides on readily existing carbon substrates and (2)â co-synthesizing both carbon and metal oxide phase during the synthesis procedure. The implications of carbon properties on the hybrid material's structure and performance will be assessed and the impact of the hybrid electrode architecture will be analyzed. The advantages and disadvantages of all approaches are highlighted and strategies to overcome the latter will be proposed.
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Zinc- (Zn) doped hydroxyapatite (HAp) were prepared by sol-gel method. Zinc-doped hydroxyapatite (ZnHAp) and HAp were analyzed by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The Rietveld analysis revealed that the HAp and 7ZnHAp powders obtained by sol-gel method have a monophasic hydroxyapatite structure belonging to the P63/m spatial group. The results obtained from the ultrasound characterization of HAp and ZnHAp are also presented in this study. The effect of zinc concentration on properties that were deduced from ultrasonic measurements are studied in the case of a significant zinc concentration (xZn = 0.07). From the values of the ultrasonic waves velocities were determined by the pairs of elastic coefficients of the suspensions (Young modulus E, Poisson coefficient ν), which have proven to be similar to those determined by other authors.
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Durapatita/química , Zinco/química , Espectroscopia Fotoeletrônica , Difração de Raios XRESUMO
Two series of catalysts were prepared by sol-gel and microemulsion synthetic procedure (SG and ME, respectively). Each series includes both pure Mg and Zr solids as well as Mg-Zr mixed solids with 25%, 50% and 75% nominal Zr content. The whole set of catalysts was characterized from thermal, structural and surface chemical points of view and subsequently applied to the liquid-phase xylose dehydration to furfural. Reactions were carried out in either a high-pressure autoclave or in an atmospheric pressure multi-reactor under a biphasic (organic/water) reaction mixture. Butan-2-ol and toluene were essayed as organic solvents. Catalysts prepared by microemulsion retained part of the surfactant used in the synthetic procedure, mainly associated with the Zr part of the solid. The MgZr-SG solid presented the highest surface acidity while the Mg3Zr-SG one exhibited the highest surface basicity among mixed systems. Xylose dehydration in the high-pressure system and with toluene/water solvent mixture led to the highest furfural yield. Moreover, the yield of furfural increases with the Zr content of the catalyst. Therefore, the catalysts constituted of pure ZrO2 (especially Zr-SG) are the most suitable to carry out the process under study although MgZr mixed solids could be also suitable for overall processes with additional reaction steps.
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Furaldeído/química , Óxido de Magnésio/química , Xilose/química , Zircônio/química , Pressão Atmosférica , Catálise , Dessecação , Emulsões , Tolueno/química , Água/químicaRESUMO
We demonstrate the synthesis of a microporous covalent-network membrane derived from co-continuous blends of a porogenic urea network and a polyimide (PI). We show that the urea networks in the PI matrix may be thermally rearranged while selectively expelling small molecular fragments, thereby forming a new network bearing reticular microporous molecular pathways. The porous structures enable reverse-selective gas separation, efficiently blocking carbon dioxide to which most polymeric membranes exhibit selective permeability. The proposed method for fabricating microporous organic membranes with highly tunable porosities using a variety of chemical structures and processing parameters is facile and shows promise for the creation of new membrane-based molecular-separation techniques.