Cristalización de zeolita beta mediante conversión asistida por vapor: influencia de los parámetros de síntesis

In the present work, beta zeolites were prepared by an alternative route called steam-assisted conversion (SAC). Several zeolites were synthesized using amorphous dry gels with a low SDA concentration (0.09 mol, TEAOH). Temperature and crystallization time were the main parameters studied. X-ray diffraction (XRD), infrared spectroscopy (IR) and scanning electron microscopy (SEM) were the characterization techniques employed. The zeolites prepared showed mixed phases such as beta, MTW and ZSM-5 while only one sample treated at 150ºC with 24 h of crystallization time showed a pure ZSM-5 phase (SAC-5). These preliminary results serve as a starting point for optimizing the synthesis of a specific type of zeolite using the SAC method.

Nanoporous materials: pillared clays and regular silicas as an example of synthesis and their porosity characterization by X-ray diffraction

Because of their practical applications, porous materials attract the attention of undergraduate students in a way that can be used to teach techniques and concepts in various chemistry disciplines. Porous materials are studied in various chemistry disciplines, including inorganic, organic, and physical chemistry. In this work, the syntheses of a microporous material and a mesoporous material are presented. The porosity of the synthesized materials is characterized by X-ray diffraction analysis. We show that this technique can be used to determine the pore dimensions of the synthesized materials.

Celdas solares fotoelectroquímicas basadas en Bi2WO6

In this study, photoelectrochemical solar cells based on bismuth tungstate electrodes were evaluated. Bi2WO6 was synthesized by a hydrothermal method and characterized by scanning electron microscopy, UV-Vis reflectance spectroscopy, and X-ray powder diffraction. For comparison, solar cells based on TiO2 semiconductor electrodes were evaluated. Photoelectrochemical response of Grätzel-type solar cells based on these semiconductors and their corresponding sensitization with two inexpensive phthalocyanines dyes were determined. Bi2WO6-based solar cells presented higher values of photocurrent and efficiency than those obtained with TiO2 electrodes, even without sensitization. These results portray solar cells based on Bi2WO6 as promising devices for solar energy conversion owing to lower cost of production and ease of acquisition.

Nanocompósitos entre nanotubos de carbono e nanopartículas de platina: preparação, caracterização e aplicação em eletro-oxidação de álcoois

The synthesis and characterization of different platinum nanoparticle/carbon nanotube nanocomposite samples are described along with the application of these nanocomposites as electrocatalysts for alcohol oxidation. Samples were prepared by a biphasic system in which platinum nanoparticles (Pt-NPs) are synthesized in situ in contact with a carbon nanotube (CNT) dispersion. Variables including platinum precursor/CNT ratio, previous chemical treatment of carbon nanotubes, and presence or absence of a capping agent were evaluated and correlated with the characteristic of the synthesized materials. Samples were characterized by Raman spectroscopy, X-ray diffraction, thermogravimetric analysis and transmission electron microscopy. Glassy carbon electrodes were modified by the nanocomposite samples and evaluated as electrocatalysts for alcohol oxidation. Current densities of 56.1 and 79.8/104.7 mA cm-2 were determined for the oxidation of methanol and ethanol, respectively.

Influence of initial CaO/SiO2 ratio on the hydration of rice husk ash-Ca(OH)2 and sugar cane bagasse ash-Ca(OH)2 pastes

This work presents the results of a study on the hydration of pastes containing calcium hydroxide and either rice husk ash (RHA) or sugar cane bagasse ash (SCBA) in various initial CaO/SiO2 molar ratios. The products of the reactions were characterized by thermal analyses X-ray diffraction, and scanning electron microscopy. In the case of the RHA pastes, the product was composed of CaO-SiO2-H2O (type I C-S-H) or CaO-SiO2-H2O (type II C-S-H) according to the CaO/SiO2 ratio of the mixture. In contrast, in the case of the SBCA pastes, the product was composed primarily of CaO-SiO2-H2O that differed from both the previous types; the product also contained inclusions of calcium aluminate hydrates.

Estudo de catalisadores de níquel suportados em cinza de casca de arroz na reforma de metano com dióxido de carbono visando a produção de hidrogênio e gás de síntese

Rice husk ash (RHA) is used as a silica source for several purposes, among them to obtain metal catalysts, as was done in this work. The catalysts were characterized by chemisorption, physisorption, thermal analyses (TG, DSC), X-ray diffraction, X-ray fluorescence, temperature-programmed reduction and scanning electron microscopy. The catalysts synthesized with different Ni loadings supported on RHA were applied to the reaction of dry reforming of methane. The reaction was tested at three temperatures of catalytic reduction (500, 600 and 700 ºC). All synthesized catalysts were active for the studied reaction, with different H2/CO ratios achieved according to degree of metallic dispersion.

DESENVOLVIMENTO DE MATERIAIS HÍBRIDOS MICRO-MESOPOROSOS DO TIPO ZSM-12/MCM-41

Micro-mesoporous hybrid materials of ZSM-12/MCM-41 type with different micro- and mesoporosity contributions were prepared by a procedure that uses the desilication of the zeolite in an alkaline medium, followed by recrystallization onto the mesostructure, where the zeolite is used as the silica source in the formation of mesoporous phase. The materials were characterized by X-ray diffraction, nitrogen adsorption-desorption at 77 K, scanning electron microscopy and thermal analysis. The results showed that the methodology utilized is efficient for obtaining hybrid materials of ZSM-12/MCM-41 type with optimized micro-and mesoporosity.

ENCAPSULAÇÃO DO ÁCIDO L-ASCÓRBICO NO BIOPOLÍMERO NATURAL GALACTOMANANA POR SPRAY‑DRYING: PREPARAÇÃO, CARACTERIZAÇÃO E ATIVIDADE ANTIOXIDANTE

AbstractIn this study, the spray drying technique was used to prepare L-ascorbic acid (AA) microparticles encapsulated with galactomannan-an extract from the seeds of the Delonix regia species. The physico-chemical characteristics, antioxidant activity, and encapsulation efficiency of the AA microparticles were evaluated and characterized using thermogravimetric analysis, differential scanning calorimetry, infrared spectroscopy, X-ray diffraction, and scanning electron microscopy. The free-radical scavenging activity of the AA microparticles was determined at different environmental conditions using DPPH (1,1-diphenyl-2-picryl-hydrazyl). X-ray diffraction measurements demonstrated a loss of crystallinity in AA after the encapsulation process, and a DSC scan also showed the loss of the compound's melting peak. Thermogravimetric analysis showed small differences in the thermal stability of galactomannan before and after the incorporation of AA. The mean diameters of the obtained spherical microspheres were in the range of 1.39 ± 0.77 µm. The encapsulation efficiency of AA microparticles in different environmental conditions varied from 95.40 to 97.92, and the antioxidant activity showed values ranging from 0.487 to 0.550 mg mL-1.

UTILIZAÇÃO DO COMPÓSITO NANOESTRUTURADO SIO2/TIO2NA FOTODEGRADAÇÃO DE CORANTES TÊXTEIS COM LUZ SOLAR NATURAL

SiO2/TiO2 nanostructured composites with three different ratios of Si:Ti were prepared using the sol-gel method. These materials were characterized using energy dispersive X-ray fluorescence, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, photoluminescence, Raman with Fourier transform infrared spectroscopy, and the specific surface area. The band gaps of materials were determined by diffuse reflectance spectra, and the values of 3.20 ± 0.01, 2.92 ± 0.02, and 2.85 ± 0.01 eV were obtained as a result of the proportional increases in the amount of Ti within the composite. The materials exhibit only the anatase (TiO2) crystalline phase and have crystalline domains ranging from 4 to 5 nm. The photodegradation process of methylene blue, royal blue GRL, and golden yellow GL dyes were studied with respect to their contact times, pH variations within the solution, and the variations in the dye concentration of the solution in response to only sunlight. The maximum amount of time for the mineralization of dyes was 90 min. The kinetics of the process follows an apparently first order model, in which the obtained rate constant values were 5.72 × 10-2 min-1 for methylene blue, 6.44 × 10-2min-1 for royal blue GRL, and 1.07 × 10-1min-1 for golden yellow.

OBTENÇÃO E CARACTERIZAÇÃO DE MATERIAL HÍBRIDO ENTRE SÍLICA E CICLODEXTRINAS

The obtention of silica and cyclodextrin hybrid materials was accomplished by refluxing them in xylol using citric acid as a binding agent. The materials were characterized by infrared spectroscopy, X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, and elemental analysis. Evidence for the docking of cyclodextrins α and γ was substantiated based on the variation in band intensity for groups such as ≡Si-OH. Additional docking evidence includes the displacement of some of the bands that are related to cyclodextrin such as the deformation of the C-H axial bond. The α and γ-CDSi materials were characterized as amorphous compounds. The products obtained in the synthesis showed changes in the decomposition temperatures of their isolated constituents, in which the mass of α and γ-CD docked to the silica surface gave the estimated values of 41% and 47%, respectively. The elemental constituents were shown to be consistent and close to their relative theoretical values. ​Thermogravimetric analysis showed that a reduction in the percentage of the hybrids was proportional to the amount of lost mass. This new material is an improvement over synthesized organosilane materials because the operator and the environment benefit from a less toxic methodology. In addition, the material has several potential applications in complexation systems with cyclodextrin.

Ni(II), Cu(II), AND Zn(II) COMPLEXES DERIVED FROM A NEW SCHIFF BASE 2-((Z)-(3-METHYLPYRIDIN-2- YLEIMINO)METHYL)PHENOL AND SYNTHESIS OF NANO SIZED METAL OXIDE PARTICLES FROM THESE COMPOUNDS

Synthesis, spectral identification, and magnetic properties of three complexes of Ni(II), Cu(II), and Zn(II) are described. All three compounds have the general formula [M(L)2(H2O)2], where L = deprotonated phenol in the Schiff base 2-((z)-(3-methylpyridin-2-yleimino)methyl)phenol. The three complexes were synthesized in a one-step synthesis and characterized by elemental analysis, Fourier transform infrared spectroscopy, electronic spectra, X-ray diffraction (XRD), and room temperature magnetic moments. The Cu(II) and Ni(II) complexes exhibited room temperature magnetic moments of 1.85 B.M. per copper atom and 2.96 B.M. per nickel atom. The X-band electron spin resonance spectra of a Cu(II) sample in dimethylformamide frozen at 77 K (liquid nitrogen temperature) showed a typical ΔMS = ± 1 transition. The complexes ([M(L)2(H2O)2]) were investigated by the cyclic voltammetry technique, which provided information regarding the electrochemical mechanism of redox behavior of the compounds. Thermal decomposition of the complexes at 750 ºC resulted in the formation of metal oxide nanoparticles. XRD analyses indicated that the nanoparticles had a high degree of crystallinity. The average sizes of the nanoparticles were found to be approximately 54.3, 30.1, and 44.4 nm for NiO, CuO, and ZnO, respectively.

EFEITO DO DIOXIDO DE CARBONO SOBRE A ESTABILIDADE DA FASE Ca2Fe2O5 APLICADA NO PROCESSO DE DEGRADAÇÃO FOTOCATALITICO DO AZUL DE METILENO

Solid samples containing a Ca2Fe2O5 phase were synthesized using the Pechini method. The samples were characterized using X-ray diffraction, thermogravimetric analysis, differential thermal analysis, X-ray fluorescence, nitrogen adsorption/desorption isotherms, and scanning electron microscopy. The stability of the Ca2Fe2O5 phase was evaluated in the photocatalytic degradation of methylene blue (MB) in aqueous solution in the presence of bubbling gas (air, N2, or CO2). The presence of CO2 is known to suppress MB degradation. After the photocatalytic test, changes were observed in the crystalline phase of all systems. These results suggest the low stability of the Ca2Fe2O5 phase in aqueous systems and the significant effect of CO2 on the photocatalytic activity of the Ca2Fe2O5 phase.