Esterificação de ácidos graxos utilizando zircônia sulfatada e compósitos carvão ativado/zircônia sulfatada como catalisadores

In this work sulfated zirconia (SZr) and activated carbon/SZr composites produced by impregnation method with or without heating treatment step (CABC/SZr-I and CABC/SZr-I SC) and by the method of synthesis of SZr on the carbon (CABC/SZr-S) was used as catalysts in the esterification reactions of fatty acids. The SZr presented very active, conversions higher than 90% were obtained after 2 h of reaction. The activity of the composite CABC/SZr-I20%SC was up to 92%, however, this was directly related to time and temperature reactions. CABC/SZr-I and CABC/SZr-S were less active in esterification reactions, what could be attributed to its low acidity

Synthesis of indium tin oxide nanoparticles by a nonhydrolytic sol-gel method

Indium tin oxide nanoparticles were synthesized in two different sizes by a nonhydrolytic sol-gel method. These powders were then transformed into ITO via an intermediate metastable state at between 300 and 600 ºC. The presence of characteristic O-In-O and O-Sn-O bands at 480 and 670 cm-1 confirmed the formation of ITO. The X-ray diffraction patterns indicated the preferential formation of metastable hexagonal phase ITO (corundum type) as opposed to cubic phase ITO when the reflux time was less than 3 h and the heat treatment temperature was below 600 ºC. Particle morphology and crystal size were examined by scanning electron microscopy.

Avaliação da biocompatibilidade de vidro e vitrocerâmica do sistema SNCP (SiO2-Na2O-CaO-P2O5)

This article reports research results related to bioactivity and cytotoxicity tests using neutral red uptake method for glass powders and bulk glass ceramics belonging to the SNCP (SiO2-Na2O-CaO-P2O5) system. The obtained materials showed bioactivity when immersed in SBF promoting the surface deposition of HAp. When analyzed as powders, cytotoxicity was evidenced in the processed materials but not when bulk samples were tested.

Sinterabilidade de pós de precursor vitrocerâmico do sistema LZSA tratados por troca iônica

Ion exchange method was employed by means of surface modification of the glass powders of LZSA (Li2O-ZrO2-SiO2-Al2O3) system submitted to a 70wt% NaNO3/30wt% NaSO4 bath salt followed by a heat treatment. Chemical analysis by X-ray fluorescence was used to evaluate the efficiency of ion exchange, while optical dilatometry was employed to evaluate sintering of compacts. Evaluation of the structure of sintered bodies was made by scanning electron microscopy. Substitution of Li+ ions by Na+ ions on the surface of powders during heat treatments of 450 and 600 ºC for 2-10 h promoted an increase in densification of the sintered bodies.

Modification of the performance of WO3-ZrO2 catalysts by metal addition in hydrocarbon reactions

A study of the different hydrocarbon reactions over Ni doped WO3-ZrO2 catalysts was performed. Ni was found as NiO at low Ni concentration while at high Ni concentrations a small fraction was present as a metal. For both cases, Ni strongly modified total acidity and concentration of strong acid sites. In the cyclohexane dehydrogenation reaction, Ni addition promotes both benzene and methyl cyclopentane production. The hydroconversion activity (n-butane and n-octane) increases with the augment of total acidity produced by Ni. The selectivity to reaction products is modified according to the acid strength distribution changes produced by Ni addition.

A comparative study of hydroxyapatite nanoparticles synthesized by different routes

In this study, bioactive hydroxyapatite nanoparticles were prepared by two different methods: wet chemical precipitation and biomimetic precipitation. The aim was to evaluate the morphology, particle-size, crystallinity and phases of the powders obtained by traditional wet chemical precipitation and the novel biomimetic precipitation using a supersaturated calcium solution. The nanoparticles were investigated by transmission electron microscopy, Fourier transform infrared spectroscopy and X-ray diffraction. The results revealed that the nanoparticles were formed by hydroxyapatite with a high crystallinity and controlled morphology. Additionally, it was found that the shape and size of the nanoparticles can be modified with each preparation method.

Síntese e caracterização de CaZrO3 e BaZrO3 nanoestruturados

In this work, nanostructured samples of barium zirconate (BaZrO3) and calcium zirconate (CaZrO3) were synthesized by the gel-combustion method, using glycine as fuel. The ceramic powders were calcined at 550 °C for 2 h and subsequently heat treated at 1350 °C for 10 min (fast-firing). The X-ray diffraction technique was employed to identify and characterize the crystalline phases present in the synthesized powders, using the Rietveld method. Monophasic nanostructured samples of BaZrO3 and CaZrO3 presenting average crystallite sizes of around 8.5 and 10.3 nm, respectively, were found after fast-firing.

Diretrizes para a construção de um moinho de bolas para a moagem de sólidos em laboratórios

In this paper, we show the construction of a low-cost, high-quality ball mill for obtaining finely divided powders, with the goal of presenting guidelines for achieving the best results for the milling process. This equipment allows for the adjustment of the size of the mill in order to process different quantities of material. The construction of mechanical and electrical components that provide increased efficiency, the choice of milling medium, and frequent problems experienced with homemade ball mills are discussed.

SYNGAS PRODUCTION FROM CO2-REFORMING OF CH4 OVER SOL-GEL SYNTHESIZED Ni-Co/Al2O3-MgO-ZrO2 NANOCATALYST: EFFECT OF ZrO2 PRECURSOR ON CATALYST PROPERTIES AND PERFORMANCE

Ni-Co/Al2O3-MgO-ZrO2 nanocatalyst with utilization of two different zirconia precursors, namely, zirconyl nitrate hydrate (ZNH) and zirconyl nitrate solution (ZNS), was synthesized via the sol-gel method. The physiochemical properties of nanocatalysts were characterized by XRD, FESEM, EDX, BET and FTIR analyses and employed for syngas production from CO2-reforming of CH4. XRD patterns, exhibiting proper crystalline structure and homogeneous dispersion of active phase for the nanocatalyst ZNS precursor employed (NCAMZ-ZNS). FESEM and BET results of NCAMZ-ZNS presented more uniform morphology and smaller particle size and consequently higher surface areas. In addition, average particle size of NCAMZ-ZNS was 15.7 nm, which is close to the critical size for Ni-Co catalysts to avoid carbon formation. Moreover, FESEM analysis indicated both prepared samples were nanoscale. EDX analysis confirmed the existence of various elements used and also supported the statements made in the XRD and FESEM analyses regarding dispersion. Based on the excellent physiochemical properties, NCAMZ-ZNS exhibited the best reactant conversion across all of the evaluated temperatures, e.g. CH4 and CO2 conversions were 97.2 and 99% at 850 ºC, respectively. Furthermore, NCAMZ-ZNS demonstrated a stable yield with H2/CO close to unit value during the 1440 min stability test.

KINETIC STUDY OF SELECTIVE GAS-PHASE OXIDATION OF ISOPROPANOL TO ACETONE USING MONOCLINIC ZRO2 AS A CATALYST

Zirconia was prepared by a precipitation method and calcined at 723 K, 1023 K, and 1253 K in order to obtain monoclinic zirconia. The prepared zirconia was characterized by XRD, SEM, EDX, surface area and pore size analyzer, and particle size analyzer. Monoclinic ZrO2 as a catalyst was used for the gas-phase oxidation of isopropanol to acetone in a Pyrex-glass-flow-type reactor with a temperature range of 443 K - 473 K. It was found that monoclinic ZrO2 shows remarkable catalytic activity (68%) and selectivity (100%) for the oxidation of isopropanol to acetone. This kinetic study reveals that the oxidation of isopropanol to acetone follows the L-H mechanism.

Effect of organic amendments on sclerotial germination, mycelial growth, and Sclerotium rolfsii-induced diseases

The addition of organic residues to soil is an option to control some soil-borne diseases. Benzaldehyde and powders of kudzu (Pueraria lobata), velvetbean (Mucuna deeringiana), and pine-bark (Pinus elliottii and P. taeda) added to soil could reduce certain soil-borne diseases. This study evaluated the effects of benzaldehyde and the dried powders of kudzu, velvetbean, and pine-bark as soil amendments on germination and formation of sclerotia, on mycelial growth of Sclerotium rolfsii, on plant survival, and disease incidence. The data showed that high amounts of benzaldehyde (0.4 ml kg-1 of soil) and velvetbean (100 g kg-1) inhibited S. rolfsii mycelial growth and sclerotium germination. However, low amounts of benzaldehyde (0.1 ml kg-1), kudzu (25 g kg-1), and pine-bark (25 g kg-1) stimulated mycelial growth and sclerotium germination. Kudzu (25-100 g kg-1) and velvetbean (25-100 g kg-1) inhibited the formation of sclerotia. Nevertheless, benzaldehyde at 0.2 and 0.4 ml kg-1 stimulated the formation of sclerotia. Kudzu (50 and 100 g kg-1) and pine-bark (50 g kg-1) favored the colonization of sclerotia by Trichoderma sp. The numbers of soybean (Glycine max) plants were higher and diseased plants were lower than the non-amend soil in the following treatments: kudzu (50 and 100 g kg-1), velvetbean (50 and 100 g kg-1), and pine-bark (50 g kg-1). Disease severity on tomato (Lycopersicon esculentum) plants was low in soil treated with kudzu or velvetbean (30 and 35 g kg-1) and pine-bark (35 g kg-1). Dried powders of kudzu, velvetbean, or pine-bark added to soil can reduce disease by reducing pathogen inoculum.

Synthesis, structural and morphological characterization of CeO2-ZnO nanosized powder systems from Pechini's method

This work reports on the investigation of nanosized CeO2-ZnO systems prepared by Pechini's method. The structural and morphological characterization of CeO2-ZnO systems as well as the characterization of CeO2 and ZnO separately, showed that the employed method result in powders with spheroidal particles whose size are in the range 30 - 200 nm, which is appropriate to provide homogeneous suspensions. The ZnO present in the prepared mixed oxides seems to increase particle size distribution and to influence the arrangement of the particles after powder dispersion.

Influence of the synthesis conditions on the characteristics and metal adsorption properties of the 3-(1,4-phenylenediamine)propylsilica xerogel

The hybrid 3-(1,4-phenylenediamine)propylsilica xerogel was obtained starting from two different organic precursor quantity (5 and 8 mmol) to 22 mmol of TEOS, in the synthesis. The xerogel samples were characterized by using CHN elemental analysis, N2 adsorption-desorption isotherms, infrared thermal analysis. The xerogel was used as metal sorbent for Cu2+, Cd2+ and Pb2+ in aqueous solution with concentration range of 10-3 to 10-5 mmol l-1. The quantity of organic precursor added in the synthesis influences the characteristics of the xerogel as morphology and thermal stability, as well as the metal adsorption capacity.

Microencapsulation of pequi pulp by spray drying: use of modified starches as encapsulating agent

The aim of this study was to evaluate the microencapsulation of pequi pulp by spray drying. A central composite rotational design was used in order to evaluate the effect of the independent variables: inlet air temperature, surfactant concentration and modified starch concentration. The dependent variables were assumed as yield of the process and the product features microencapsulated. A selection of the best process condition was performed to obtain the best condition of a product with the highest vitamin C and carotenoids content. Powders showed moisture content below 2%. The experimental values of hygroscopicity, yield, water activity, total carotenoids and vitamin C powders ranged from 7.96 to 10.67 g of adsorbed water/100g of solids, 24.34 to 49.80%, 0.13 to 0.30, 145.78 to 292.11 mg of ascorbic acid/g of pequi solids and 15.51 to 123.42 mg of carotenoids/g of pequi solids, respectively. The inlet air temperature 140°C, the surfactant concentration of 2.5% and the modified starch concentration of 22.5% was recommended as the selected condition. By the scanning electron microscopy, it was observed that most of the particles had spherical shape and smooth surface.

Fractionation of Hen Egg and Oat Lipids with supercritical Fluids Chemical and functional Properties of Fractions

Hen eggs and oats (Avena Sativa) are important materials for the food industry. Today, instead of merely satisfying the feeling of hunger, consumers are asking for healthier, biologically active and environmentally friendly products. The growing awareness of consumers’ increasing demands presents a great challenge to the food industry to develop more sustainable products and utilise modern and effective techniques. The modification of yolk fatty acid composition by means of feed supplements is well understood. Egg yolk phospholipids are polar lipids and are used in several applications including food, cosmetics, pharmaceuticals, and special nutrients. Egg yolk phospholipids are excellent emulsifiers, typically sold as mixtures of phospholipids, triacylglycerols, and cholesterol. However, highly purified and characterised phospholipids are needed in several sophisticated applications. Industrial fractionation of phospholipids is usually based on organic solvents. With these fractionation techniques, some harmful residues of organic solvents may cause problems in further processing. The objective of the present study was to investigate the methods to improve the functional properties of eggs, to develop techniques to isolate the fractions responsible for the specific functional properties of egg yolk lipids, and to apply the developed techniques to plant-based materials, too. Fractionation techniques based on supercritical fluids were utilised for the separation of the lipid fractions of eggs and oats. The chemical and functional characterisation of the fractions were performed, and the produced oat polar lipid fractions were tested as protective barrier in encapsulation processes. Modifying the fatty acid compositions of egg yolks with different types of oil supplements in feed had no affect on their functional or sensory properties. Based on the results of functional and sensory analysis, it is evident that eggs with modified fatty acid compositions are usable in several industrial applications. These applications include liquid egg yolk products used in mayonnaise and salad dressings. Egg yolk powders were utilised in different kinds of fractionation processes. The precipitation method developed in this study resembles the supercritical anti-solvent method, which is typically used in the pharmaceutical industry. With pilot scale supercritical fluid processes, non-polar lipids and polar lipids were successfully separated from commercially produced egg yolk powder and oat flakes. The egg and oat-based polar lipid fractions showed high purities, and the corresponding delipidated fractions produced using supercritical techniques offer interesting starting materials for the further production of bioactive compounds. The oat polar lipid fraction contained especially digalactosyadiacylglycerol, which was shown to have valuable functional properties in the encapsulation of probiotics.