NANOCRISTAIS DE CELULOSE A PARTIR DE CELULOSE BACTERIANA

Bacterial cellulose produced from Gluconacetobacter xilinus was used to produce cellulose nanocrystals by sulfuric acid hydrolysis. Hydrolysis was performed with 64% sulfuric acid at 50 ºC with the hydrolysis time ranging between 5 and 90 min. The production of nanocrystals was observed to have size distributions that were dependent on hydrolysis times up to 10 min, after which time the suspensions showed distributions closer in size. Results from thermal analysis and X-ray diffraction showed that the amorphous cellulose was removed, leaving only the crystalline portion. Self-supported films were formed from the suspension of nanocrystals and had iridescence characteristics. The films were characterized by microscopy measures and specular reflectance.

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.

Thermoanalytical study of the complexes of 4-dimetilaminocinnamylidenepiruvate with manganese (II), cobalt (II), nickel (II), cupper (II), zinc (II) and lead (II), in the solid state

Solid state compounds M-4-DMCP, where 4-DMCP is 4-dimethylaminocinnamylidenepyruvate and M represents Mn (II), Co (II), Ni (II), Cu (II), Zn (II) and Pb (II) were prepared. These compounds were studied by thermoanalitycal techniques: thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC), X-ray diffraction powder patterns and complexometric titration with EDTA. From the results obtained by the complexometric titration with EDTA, TG, DTG and DSC curves, was possible to establish the hydration degree, stoichiometry and thermal stability of the prepared compounds.

Influence of the Al content on the phase transformations in Cu-Al-Ag alloys

The influence of the Al content on the phase transformations in Cu-Al-Ag alloys was studied by classical differential thermal analysis (DTA), optical microscopy (OM) and X-ray diffractometry (XRD). The results indicated that the increase in the Al content and the presence of Ag decrease the rate of the b1 phase decomposition reaction and contribute for the raise of this transition temperature, thus decreasing the stability range of the perlitic phase resulted from the b1 decomposition reaction.

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.

Self-assembly of supermolecular species directed by hydrogen bonding and aromatic π-π stacking interactions

A new Cu(II) trimers, [Cu3(dcp)2(H2O)8]. 4DMF, with the ligand 3,5-pyrazoledicarboxylic acid monohydrate (H3dcp) has been prepared by solvent method. Its solid-state structure has been characterized by elemental analysis, thermal analysis (TGA and DSC), and single crystal X-ray diffraction. X-ray crystallographic studies reveal that this complex has extended 1-D,2-D and 3-D supramolecular architectures directed by weak interactions (hydrogen bond and aromatic π-π stacking interaction) leading to a sandwich solid-state structure.

Thermoanalytical study and characterization of native starches of Paraná pine seeds (Araucaria angustiofolia, Bert O. Ktze) and European chestnut seeds (Castanea sativa, Mill)

Starch is the most important carbohydrate storage in plants. It is a raw material with diverse botanical origins, and is used by the food, paper, chemical, pharmaceutical, textile and other industries. In this work, native starches of Paraná pine seeds (pinhão) (Araucária angustiofolia, Bert O. Ktze) and european chestnut seeds (Castanea sativa, Mill) were studied by thermoanalytical techniques: thermo-gravimetry (TG), differential thermal analysis (DTA) and differential scanning calorimetry (DSC), as well as X-ray powder patterns diffractometry. Apparent and total amylose content was also determined.

Lanthanum based high surface area perovskite-type oxide and application in CO and propane combustion

The perovskite-type oxides using transition metals present a promising potential as catalysts in total oxidation reaction. The present work investigates the effect of synthesis by oxidant co-precipitation on the catalytic activity of perovskite-type oxides LaBO3 (B= Co, Ni, Mn) in total oxidation of propane and CO. The perovskite-type oxides were characterized by means of X-ray diffraction, nitrogen adsorption (BET method), thermo gravimetric and differential thermal analysis (ATG-DTA) and X-ray photoelectron spectroscopy (XPS). Through a method involving the oxidant co-precipitation it's possible to obtain catalysts with different BET surface areas, of 33-44 m²/g, according the salts of metal used. The characterization results proved that catalysts have a perovskite phase as well as lanthanum oxide, except LaMnO3, that presents a cationic vacancies and generation for known oxygen excess. The results of catalytic test showed that all oxides have a specific catalytic activity for total oxidation of CO and propane even though the temperatures for total conversion change for each transition metal and substance to be oxidized.

Synthesis and characterization of Fe(III)-doped ceramic membranes of titanium dioxide and its application in photoelectrocatalysis of a textile dye

Pure and Fe(III)-doped TiO2 suspensions were prepared by the sol gel method with the use of titanium isopropoxide (Ti(OPri)4) as precursor material. The properties of doped materials were compared to TiO2 properties based on the characterization by thermal analysis (TG-DTA and DSC), X-ray powder diffractometry and spectroscopy measurements (FTIR). Both undoped and doped TiO2 suspensions were used to coat metallic substrate as a mean to make thin-film electrodes. Thermal treatment of the precursors at 400ºC for 2 h in air resulted in the formation of nanocrystalline anatase TiO2. The thin-film electrodes were tested with respect to their photocatalytic performance for degradation of a textile dye in aqueous solution. The plain TiO2 remains as the best catalyst at the conditions used in this report.

Effect of particle morphology on the mechanical and thermo-mechanical behavior of polymer composites

Fiber reinforced polymer composites have been used in many applications, such as in automobile, aerospace and naval industries, due basically to their high strength-to-weight and modulus-to-weight, among other properties. Even though particles are usually not able to lead to the level of reinforcement of fibers, particle reinforced polymer composites have been proposed for many new applications due to their low cost, easy fabrication and isotropic properties. In this work, polymer composites were prepared by incorporating glass particles of different morphologies on poly(aryl sulfones) matrices. Particles with aspect ratios equal to 1, 2.5 and 10 were used. The prepared composites were characterized using electron microscopy and thermal analysis. Mechanical properties of the composites were evaluated using a four-point bending test. The thermo-mechanical behavior of the obtained composites was also investigated. The results showed that the morphology of the particles alter significantly the mechanical properties of composites. Particles with larger values of aspect ratio led to large elastic modulus but low levels of strain at failure. This result was explained by modeling the thermo-mechanical behavior of the composites using a viscoelastic model. Parameters of the model, obtained from a Cole-Cole type of plot, demonstrated that interactions at the polymer-reinforcing agent interface were higher for composites with large aspect ratio particles. Higher levels of interactions at interfaces can lead to higher degrees of stress transfer and, consequently, to composites with large elastic modulus, as experimentally observed.

Physicochemical study of CaCO3 from egg shells

Calcium carbonate, a pharmaceutical excipient, is widely used as diluent in solid dosage forms. It is also used as a base for medicinal and dental preparations, a buffering and dissolution aid for dispersible tablets, a food additive and a calcium supplement. Egg shells are a rich source of mineral salts, mainly calcium carbonate, which corresponds to about 94% of the shell. Layer farms produce large amounts of shells, whose final disposal poses a challenge from the environmental standpoint. This work was designed to evaluate the physicochemical and thermal properties of calcium carbonate obtained from egg shells. The findings indicated that calcium carbonate from egg shells can be used as an alternative pharmaceutical excipient.