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The present work describes a quick, simple, and efficient method based on the use of layered double hydroxides (LDH) coupled to dispersive solid phase micro-extraction (DSPME) to remove α-naphthol (α-NAP) and ß-naphthol (ß-NAP) isomers from water samples. Three different LDHs (MgAl-LDH, NiAl-LDH, and CoAl-LDH) were used to study how the interlayer anion and molar ratio affected the removal performance. The critical factors in the DSPME procedure (pH, LDH amount, contact time) were optimized by the univariate method under the optimal conditions: pH, 4-8; LDH amount, 5 mg; and contact time, 2.5 min. The method can be successfully applied in real sample waters, removing NAP isomers even in ultra-trace concentrations. The large volume sample stacking (LVSS-CE) technique provides limits of detections (LODs) of 5.52 µg/L and 6.36 µg/L for α-naphthol and ß-naphthol, respectively. The methodology's precision was evaluated on intra- and inter-day repeatability, with %RSD less than 10% in all cases. The MgAl/Cl--LDH selectivity was tested in the presence of phenol and bisphenol A, with a removal rate of >92.80%. The elution tests suggest that the LDH MgAl/Cl--LDH could be suitable for pre-concentration of α-naphthol and ß-naphthol in future works.
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Eletroforese Capilar , Limite de Detecção , Naftóis , Microextração em Fase Sólida , Poluentes Químicos da Água , Naftóis/química , Naftóis/análise , Naftóis/isolamento & purificação , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/isolamento & purificação , Poluentes Químicos da Água/química , Eletroforese Capilar/métodos , Microextração em Fase Sólida/métodos , Hidróxidos/química , Isomerismo , Reprodutibilidade dos Testes , Concentração de Íons de HidrogênioRESUMO
Indomethacin (INDO) has a mechanism of action based on inhibiting fatty acids cyclooxygenase activity within the inflammation process. The action mechanism could be correlated with possible anticancer activity, but its high toxicity in normal tissues has made therapy difficult. By the coprecipitation method, the drug carried in a layered double hydroxides (LDH) hybrid matrix would reduce its undesired effects by promoting chemotherapeutic redirection. Therefore, different samples containing INDO intercalated in LDH were synthesized at temperatures of 50, 70, and 90 °C and synthesis times of 8, 16, 24, and 48 h, seeking the best structural organization. X-ray diffraction (XRD), vibrational Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), spectrophotometric analysis in UV-VIS, and differential thermogravimetric analysis (TGA/DTA) were used for characterization. Our results indicate that higher temperatures and longer synthesis time through coprecipitation reduce the possibility of INDO intercalation. However, it was possible to establish a time of 16 h and a temperature of 50 °C as the best conditions for intercalation. In vitro results confirmed the cell viability potential and anticancer activity in the LDH-INDO sample (16 h and 50 °C) for gastric cancer (AGP01, ACP02, and ACP03), breast cancer (MDA-MB-231 and MCF-7), melanoma (SK-MEL-19), lung fibroblast (MRC-5), and non-neoplastic gastric tissue (MN01) by MTT assay. Cell proliferation was inhibited, demonstrating higher and lower toxicity against MDA-MB-231 and SK-MEL-19. Thus, a clinical redirection of INDO is suggested as an integral and adjunctive anticancer medication in chemotherapy treatment.
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Antineoplásicos , Hidróxidos , Indometacina , Nanopartículas , Humanos , Nanopartículas/química , Indometacina/farmacologia , Indometacina/química , Antineoplásicos/farmacologia , Antineoplásicos/química , Antineoplásicos/síntese química , Hidróxidos/química , Linhagem Celular Tumoral , Sobrevivência Celular/efeitos dos fármacos , Espectroscopia de Infravermelho com Transformada de Fourier , Difração de Raios X , Neoplasias/tratamento farmacológico , Neoplasias/patologia , Proliferação de Células/efeitos dos fármacosRESUMO
This work presents the development, synthesis, and application of a layered double hydroxide (LDH) coupled to magnetic particles for the removal of antibiotics as tetracyclines (TC´s): tetracycline (TC), chlortetracycline (CT), oxytetracycline (OT), and doxycycline (DT) from milk samples. The LDH synthesis conditions, reaction time (30-90 min), molar ratios Mg2+/Al3+ (7:1-1:7), interlayer anion (NO3-, Cl-, CO32-, and dodecyl sulphate (DS-)) were evaluated. Under synthesis conditions (reaction time of 30 min, Mg2+/Al3+ molar ratio of 7:1, and DS- as interlayer anion), the LDH was coupled in a magnetic solid phase microextraction (MSPµE) methodology. At the optimal extraction conditions (pH 6, 5 min of contact time, 10 mg of adsorbent), a removal percentage of 99.0 % was obtained for each tetracycline. FTIR, TGA, SEM, and adsorption isotherms were employed to characterize the optimal adsorbent. Each experiment was corroborated by large-volume sample stacking capillary electrophoresis (LVSS-CE). The adsorbent was applied directly to positive milk samples (previously tested) for TC´s removal.
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Hidróxidos , Leite , Tetraciclinas , Leite/química , Animais , Tetraciclinas/isolamento & purificação , Tetraciclinas/análise , Tetraciclinas/química , Hidróxidos/química , Adsorção , Microextração em Fase Sólida/métodos , Antibacterianos/isolamento & purificação , Antibacterianos/química , Antibacterianos/análise , Dióxido de Silício/químicaRESUMO
N-acetyl-L-cysteine (NAC), a derivative of the L-cysteine amino acid, presents antioxidant and mucolytic properties of pharmaceutical interest. This work reports the preparation of organic-inorganic nanophases aiming for the development of drug delivery systems based on NAC intercalation into layered double hydroxides (LDH) of zinc-aluminum (Zn2Al-NAC) and magnesium-aluminum (Mg2Al-NAC) compositions. A detailed characterization of the synthesized hybrid materials was performed, including X-ray diffraction (XRD) and pair distribution function (PDF) analysis, infrared and Raman spectroscopies, solid-state 13carbon and 27aluminum nuclear magnetic resonance (NMR), simultaneous thermogravimetric and differential scanning calorimetry coupled to mass spectrometry (TG/DSC-MS), scanning electron microscopy (SEM), and elemental chemical analysis to assess both chemical composition and structure of the samples. The experimental conditions allowed to isolate Zn2Al-NAC nanomaterial with good crystallinity and a loading capacity of 27.3 (m/m)%. On the other hand, NAC intercalation was not successful into Mg2Al-LDH, being oxidized instead. In vitro drug delivery kinetic studies were performed using cylindrical tablets of Zn2Al-NAC in a simulated physiological solution (extracellular matrix) to investigate the release profile. After 96 h, the tablet was analyzed by micro-Raman spectroscopy. NAC was replaced by anions such as hydrogen phosphate by a slow diffusion-controlled ion exchange process. Zn2Al-NAC fulfil basic requirements to be employed as a drug delivery system with a defined microscopic structure, appreciable loading capacity, and allowing a controlled release of NAC.
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The development of biomaterials has a substantial role in pharmaceutical and medical strategies for the enhancement of life quality. This review work focused on versatile biomaterials based on nanocomposites comprising organic polymers and a class of layered inorganic nanoparticles, aiming for drug delivery (oral, transdermal, and ocular delivery) and tissue engineering (skin and bone therapies). Layered double hydroxides (LDHs) are 2D nanomaterials that can intercalate anionic bioactive species between the layers. The layers can hold metal cations that confer intrinsic biological activity to LDHs as well as biocompatibility. The intercalation of bioactive species between the layers allows the formation of drug delivery systems with elevated loading capacity and modified release profiles promoted by ion exchange and/or solubilization. The capacity of tissue integration, antigenicity, and stimulation of collagen formation, among other beneficial characteristics of LDH, have been observed by in vivo assays. The association between the properties of biocompatible polymers and LDH-drug nanohybrids produces multifunctional nanocomposites compatible with living matter. Such nanocomposites are stimuli-responsive, show appropriate mechanical properties, and can be prepared by creative methods that allow a fine-tuning of drug release. They are processed in the end form of films, beads, gels, monoliths etc., to reach orientated therapeutic applications. Several studies attest to the higher performance of polymer/LDH-drug nanocomposite compared to the LDH-drug hybrid or the free drug.
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This study reports nickel removing by electrocoagulation of Ni(II)-NH3-CO2-SO2-H2O system at laboratory scale. Experiments were done using Al/Al pair electrodes at initial nickel concentration between 293 and 1356 mg·L-1 and under operation parameters of pH 8.6, current density 9.8 mA·cm-2, electrolysis time 30 min, and temperature 60 ºC. The obtained results show removal efficiencies between 97.7 and 99.7 %. Kinetics modeling suggested combined effects of external diffusion and nucleation, and as controlling step the chemical reaction and a possible autocatalytic contribution. The process followed the Langmuir´s isotherm with a maximum adsorption capacity of 7519 mg·g-1. ICP-OES, XRD and FTIR characterization of the precipitates indicated a typical Ni-Al layered double hydroxide structures with 33.4-40.7 % nickel and 6.3-7.0 % aluminum depending on initial nickel concentration. The operation costs of energy and electrode consumption were 320 - 537 $·t-1 of removed nickel.
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Clay materials and nanoclays have gained recent popularity in the vaccinology field, with biocompatibility, simple functionalization, low toxicity, and low-cost as their main attributes. As elements of nanovaccines, halloysite nanotubes (natural), layered double hydroxides and hectorite (synthetic) are the nanoclays that have advanced into the vaccinology field. Until now, only physisorption has been used to modify the surface of nanoclays with antigens, adjuvants, and/or ligands to create nanovaccines. Protocols to covalently attach these molecules have not been developed with nanoclays, only procedures to develop adsorbents based on nanoclays that could be extended to develop nanovaccine conjugates. In this review, we describe the approaches evaluated on different nanovaccine candidates reported in articles, the immunological results obtained with them and the most advanced approaches in the preclinical field, while describing the nanomaterial itself. In addition, complex systems that use nanoclays were included and described. The safety of nanoclays as carriers is an important key fact to determine their true potential as nanovaccine candidates in humans. Here, we present the evaluations reported in this field. Finally, we point out the perspectives in the development of vaccine prototypes using nanoclays as antigen carriers.
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Within the frame of this article, briefly but comprehensively, we present the existing knowledge, perspectives, and challenges for the utilization of Layered Double Hydroxides (LDHs) as adsorbents against a plethora of pollutants in aquatic matrixes. The use of LDHs as adsorbents was established by considering their significant physicochemical features, including their textural, structural, morphological, and chemical composition, as well as their method of synthesis, followed by their advantages and disadvantages as remediation media. The utilization of LDHs towards the adsorptive removal of dyes, metals, oxyanions, and emerging pollutants is critically reviewed, while all the reported kinds of interactions that gather the removal are collectively presented. Finally, future perspectives on the topic are discussed. It is expected that this discussion will encourage researchers in the area to seek new ideas for the design, development, and applications of novel LDHs-based nanomaterials as selective adsorbents, and hence to further explore the potential of their utilization also for analytic approaches to detect and monitor various pollutants.
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Poluentes Químicos da Água , Purificação da Água , Adsorção , Hidróxidos/química , Poluentes Químicos da Água/químicaRESUMO
The bacterium Streptomyces sp. is a common genus of the actinomycetes class found in soils and rhizospheres. This bacterium can produce substances with bio-stimulant capacity through the fixation of nitrogen from the air. In this work, the Streptomyces sp. bacterium was immobilized on a ZnMgAl-hydrotalcite clay and embedded in calcium alginate beads to generate a novel bio-composite that functions as a bacterial reservoir and as a controlled release material for bacteria to be used as a bio-fertilizer.The results showed that the novel bacterium-hydrotalcite/alginate bio-composite was very efficient as a bio-fertilizer showing a plant length of 64 mm in only 14 days of growing, which corresponds to an increase of ca. 760% in the lettuce plant growth in comparison with the materials without bacteria. In short, the present results demonstrate that the hydrotalcite and alginate served as an excellent container to keep the bacteria alive, providing nutrients to them and controlling their delivery.
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Fertilizantes , Nitrogênio , Alginatos , Hidróxido de Alumínio , Bactérias , Fertilizantes/microbiologia , Hidróxido de MagnésioRESUMO
Microplastics and nanomaterials are applied in a myriad of commercial and industrial applications. When leaked to natural environments, such small particles might threaten living organisms' health, particularly when considering their potential combination that remains poorly investigated. This study investigated the physiological and biochemical effects of polyethylene (PE; 64-125 µm in size, 0.1, 1.0, and 10.0 mg·L-1) single and combined with an engineered nanomaterial applied in antifouling coatings, the copper-aluminium layered double hydroxides (Cu-Al LDH; 0.33, 1.0, and 3.33 mg·L-1) in the flatfish Solea senegalensis larvae (8 dph) after 3 h exposure, in a full factorial design. Particles ingestion, histopathology, and biochemical biomarkers were assessed. Fish larvae presented <1 PE particles in their gut, independently of their concentration in the medium. The histological health index showed minimal pathological alterations at PE combined exposure, with a higher value observed at 1 mg LDH·L-1 × 0.1 mg PE·L-1. Gut deformity and increased antioxidant defences (catalase), neurotransmission (acetylcholinesterase), and aerobic energy production (electron transport system) were observed at PE ≥ 1.0 mg·L-1. No oxidative damage (lipid peroxidation) or alterations in the detoxification capacity (glutathione-S-transferase) was observed on single and combined exposures. PE, combined or not with Cu-Al LDH, does not seem to compromise larvae's homeostasis considering levels reported so far in the marine and aquaculture environments. However, harsh effects are expected with MP contamination rise, as projections suggest.
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Linguados , Poluentes Químicos da Água , Acetilcolinesterase , Animais , Microplásticos , Plásticos , Polietileno/toxicidade , Poluentes Químicos da Água/análise , Poluentes Químicos da Água/toxicidadeRESUMO
In the present study, Mg-Al and Zn-Al layered double hydroxides (LDH) were synthesized by the co-precipitation method and employed to remove phosphate from synthetic aqueous solutions and industrial wastewaters. LDH were characterized by X-ray diffraction (XRD), N2 adsorption/desorption isotherms (BET method), thermal analyses (TG-DTA) and Fourier transform infrared spectroscopy (FTIR). XRD and TG-DTA analysis showed that Mg-Al and Zn-Al formed the LDH structure. Experimental adsorption data indicated that pseudo-second order model best described phosphate adsorption kinetics. Data of equilibrium experiments fitted well to Sips and Freundlich models for Mg-Al and Zn-Al, respectively. The effect of co-existing anions on the phosphate adsorption capacity was analyzed by utilizing industrial wastewater. The results showed that the phosphate removal decreases in the presence of other anions. Mg-Al adsorbent exhibited 74% removal of phosphate with a dosage of 5â g/L in industrial wastewater.
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Fosfatos , Poluentes Químicos da Água , Adsorção , Alumínio , Hidróxidos , Cinética , Águas Residuárias , Poluentes Químicos da Água/análiseRESUMO
This work presents the development of multifunctional therapeutic membranes based on a high-performance block copolymer scaffold formed by polyether (PE) and polyamide (PA) units (known as PEBA) and layered double hydroxide (LDH) biomaterials, with the aim to study their uses as wound dressings. Two LDH layer compositions were employed containing Mg2+ or Zn2+, Fe3+ and Al3+ cations, intercalated with chloride anions, abbreviated as Mg-Cl or Zn-Cl, or intercalated with naproxenate (NAP) anions, abbreviated as Mg-NAP or Zn-NAP. Membranes were structurally and physically characterized, and the in vitro drug release kinetics and cytotoxicity assessed. PEBA-loading NaNAP salt particles were also prepared for comparison. Intercalated NAP anions improved LDH-polymer interaction, resulting in membranes with greater mechanical performance compared to the polymer only or to the membranes containing the Cl-LDHs. Drug release (in saline solution) was sustained for at least 8 h for all samples and release kinetics could be modulated: a slower, an intermediate and a faster NAP release were observed from membranes containing Zn-NAP, NaNAP and Mg-NAP particles, respectively. In general, cell viability was higher in the presence of Mg-LDH and the membranes presented improved performance in comparison with the powdered samples. PEBA containing Mg-NAP sample stood out among all membranes in all the evaluated aspects, thus being considered a great candidate for application as multifunctional therapeutic dressings.
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Auxins are a class of organic substances known as plant-growth regulators, which act on plant physiology, promoting its full development. However, due to the great instability of these substances among the diversity of crops and cultivation environments, it is necessary to seek more efficient modes of application, which lead to a homogeneous distribution and promote a sustained release according to the plants demand. Seed coating, using films containing a biodegradable polymer and auxins intercalated into layered compounds, emerges as a very promising approach to a new form of growth regulator application. Thus, the presented work had three aims: (i) the synthesis and characterization of an organic-inorganic hybrid material containing a layered double hydroxide (LDH) of zinc and aluminum and the synthetic auxin 1-naphthalenoacetic acid (ZnAl-NAA-LDH), (ii) the coating of bean seeds (Phaseolus vulgaris L.) with composite films produced from mixtures of alginate polymer and ZnAl-NAA-LDH, and (iii) the evaluation of the plant response by bioassays. The hybrid ZnAl-NAA-LDH was characterized by a set of analytical techniques, including powder X-ray diffraction, thermogravimetric analysis coupled to differential scanning calorimetry and mass spectrometry, specific surface area measurement, and scanning electron microscopy. Bioassays were performed with the seeds coated with the composite film to assess the germination rate and germination speed index of the seeds, as well as biometric analyses including measurements of root area, root fresh matter, and shoot length of the plants. The bioassay performed in soil pots showed that the alginate film containing ZnAl-NAA-LDH yields an enhancement regarding root area, fresh root matter and shoot length of plants. Thus, films produced from a mixture of alginate and the hybrid material containing the growth regulator intercalated into LDH can be a viable alternative to enhance plant development, which can be included in seed management.
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The magnetic adsorbent prepared with hydrocalumite-iron oxide (HC/Fe) modified with dodecyl sulfate (DS) was examined for the removal of the agrichemicals atrazine (ATZ) and chlorpyrifos (CPF) from aqueous solution. The adsorbent HC-DS/Fe was characterized by infrared spectroscopy (IR), Raman spectroscopy, X-ray diffractometry (XRD) and atomic absorption spectrometry. The effects of adsorbent dosage, contact time, pH and initial concentration of ATZ and CPF were evaluated. HC-DS/Fe presented a maximum adsorption capacity for ATZ of 4.5 mg g-1 (30 min) and for CPF of 72.9 mg g-1 (210 min) at 25 °C. HC-DS/Fe can be readily removed from the aqueous solution by magnetization because of its magnetic properties. The free energy variation for HC-DS/Fe during the adsorption of the ATZ was -48.78 to -53.91 kJ mol-1 and for the CPF of -55.79 to -59.28 kJ mol-1, suggesting the spontaneity of the adsorption process. The positive value of â³H suggests an endothermic process for the interaction of ATZ and CPF by HC-DS/Fe. This adsorbent showed satisfactory results when used in the treatment of a sample of river water, fortified with the agrichemicals chlorpyrifos, atrazine, thiamethoxam and acetamiprid.
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Poluentes Químicos da Água , Purificação da Água , Adsorção , Agroquímicos , Óxido de Alumínio , Cloreto de Cálcio , Compostos Férricos , Concentração de Íons de Hidrogênio , Cinética , Fenômenos Magnéticos , Dodecilsulfato de SódioRESUMO
[Co-Al-Cl] layered double hydroxide (LDH) obtained by co-precipitation at constant pH 8 presented a single phase in a hexagonal unit cell parameters similar to the hydrotalcite (JCPDS 14-191) belonging to the rhombohedral crystal system and space group R (-3)m . The adsorption kinetics of 2,4-D onto [Co-Al-Cl] LDH was better described by the Pseudo Second-Order (best adjust R2 = 0.9998 for 60 mg L-1 2,4-D adsorption). Intra-particle diffusion model was not the sole rate-controlling factor, indicating the adsorption of 2,4-D by the [Co-Al-Cl] LDH is a complex process for the experimental conditions performed, involving both boundary layer and intra-particle diffusion. The adsorption isotherm adjusted better to the Freundlich model (R2 = 0.9845) and the ΔH° value of - 51.18 kJ mol-1 indicated the predominance of the physical adsorption. The FT-IR spectrum of LDH after adsorption presented 2,4-D bands together with those of LDH and XRD showed an increase in the interlamellar distance (d 003) due to the intercalation of 2,4-D in the interlayer structure of the [Co-Al-Cl] LDH, corroborating inter and intra-particle adsorption data. Thus, [Co-Al-Cl] LDH, commonly used as electrodes in supercapacitors, can be effectively used as an adsorbent for the removal of 2,4-D from contaminated waters.
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The XRD profiles and FTIR analysis of sludge aggregates, Mg-Al layered double hydroxides, produced during electrocoagulation processes are presented. The data describes the composition of materials (LDH) produced at different operations conditions (atmospheric conditions and Mg2+/Al3+ ratio). The data show the diffraction peaks of (003), (006), (018) and (110) crystal planes for hydrotalcite structure.
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A series of samples of Mg/Zn/Al LDHs (layered double hydroxides) materials was prepared by the co-precipitation and urea hydrolysis methods. They were modified with organic surfactants (acrylate and oleate anions) and characterized by X-ray diffraction, which corroborated the intercalation of anionic species into the interlayer space. The hydrophobized materials were incorporated at low contents (10 and 15 wt.%) to polystyrene, which was synthesized by emulsion polymerization techniques. The polymeric composites were analyzed by thermogravimetry to determine the decomposition temperature. The results demonstrated that the materials with Zn presented the greatest increment in the degradation temperature (7 °C < T < 54 °C). Moreover, the Friedman, Flynn-Wall-Ozawa, and Coats-Redfern models were compared to obtain the kinetic parameters of degradation process. The obtained order of decomposition of the Coats-Redfern model showed that the decomposition process occurs in at least two stages. Finally, the addition of environmentally friendly modified Layered Double Hydroxides (LDH) nanomaterials to the polystyrene (PS) matrix allowed for obtaining polymeric composites with higher thermal stability, retarding the decomposition process of PS.
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In the present work, the composite MgAl-LDH/biochar using activated carbon from bovine bone as support for the layered double hydroxide particles was successfully synthesised and used as an alternative adsorbent for caffeine removal from water. Kinetic studies showed that the equilibrium was achieved in only 20 min of contact between the adsorbent and the adsorbate. The pseudo-first-order model represented the experimental data more satisfactorily (R2 = 0.95), suggesting a physical adsorption process. The isotherms were performed at three temperatures, in which it was observed the decrease in the adsorption in higher temperatures. It was obtained a maximum adsorption capacity of 26.219 mg/g at 40 °C, and the experimental data were better adjusted by Redlich-Peterson, R2 > 0.9942. In short, the study demonstrated that the composite was satisfactorily synthesised and its use in the caffeine removal was quite attractive, being a potential adsorbent for water treatment applications.
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Cafeína/análise , Carvão Vegetal/análise , Hidróxidos/química , Adsorção , Animais , Bovinos , Cinética , Temperatura , Purificação da ÁguaRESUMO
Layered double hydroxides (LDHs) are cheap materials suitable for immobilization of enzymes. In this study, we prepared Zn/Al-Cl LDHs with different Zn:Al molar ratios for immobilization of the lipase from Pseudomonas cepacia. The best values for activity retention (188%), immobilization efficiency (96%) and hydrolytic activity in organic medium (279 U g-1) were obtained with a molar ratio of Zn:Al of 4:1, a protein loading of 162â¯mgâ¯g-1 and Tris-HCl buffer (10â¯mmol L-1, pH 7.5) as the solvent for preparing the lipase solution. The immobilized lipase keeps its activity when stored at 4⯰C during 30 days. The immobilized lipase gave a conversion of 50% in 1â¯h for the kinetic resolution of the alcohol rac-1-phenylethanol, with both ees and eep higher than 99% and E higher than 200. In the reutilization study, 30 successive 1-h kinetic resolutions were done with the same batch of immobilized enzyme. For all 30 resolutions, 50% conversion was maintained, with ees and eep higher than 99% and E higher than 200. These are promising results that lay the basis for further studies of immobilization of lipases onto LDHs for applications in organic media.
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Alumínio/química , Compostos de Anilina/química , Burkholderia cepacia/enzimologia , Enzimas Imobilizadas/metabolismo , Lipase/metabolismo , Fenol/química , Álcool Feniletílico/química , Zinco/química , Hidrólise , Hidróxidos/química , CinéticaRESUMO
Epoxide ring opening driven alkalinization process was explored with the aim of preparing layered double hydroxide (LDH) phases on demand, at room temperature. Employing iodide as nucleophilic agent, the precipitation reaction can be driven under much lower halide concentrations. This scenario favors the selective intercalation of concomitant bulky oxo anions as nitrate or perchlorate in the LDH products, allowing for the one-pot synthesis of an LDH able to delaminate in formamide. Even large dicarboxylic acids, - O2 C-(CH2 )n -CO2 - , with n up to 8, can be quantitively intercalated within the growing LDH phase, providing a versatile one-pot route for hybrid LDHs as well. Under the mild conditions employed, governed by a continuous pH rise from a starting acid condition, a MII to M*III ratio of 2 prevails, independently from the overall cationic composition. However, after moderate hydrothermal aging LDH phases bearing a cationic ratio higher than 2 could result. The solubility of a given chloride-containing MII 2 M*III LDH can be approximated as a linear combination of the solubility of the pure hydroxylated phases of the constitutive cations, M(OH)2 and M* (OH)3 .