Estudo da decomposição térmica de propelente sólido compósito de baixa emissão de fumaça

The thermal decomposition of hydroxyl-terminated polybutadiene (HTPB)/ammonium nitrate (AN) based propellants, so called smokeless formulations, and raw materials were investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The thermoanalytical profile of different components and of propellant were evaluated and the Arrhenius parameters for the thermal decomposition of the propellant sample were determined by the Ozawa method. The kinetic parameters of the thermal decomposition of propellant samples were determined by DSC measurements. The values obtained for activation energy (Ea) and pre-exponential factor were 163 kJ mol-1 and 1.94x10(6) min-1.

Estudo cinético por TG e DSC da decomposição térmica de alguns adutos de haletos de cádmio

By DSC data, the kinetical parameters Ea , n and A were calculated for the thermal decomposition of the adducts CdCl2.2dmf, CdCl2.dmf and CdBr2.dmf (dmf= dimethylformamide) by using Rogers and Smith method. The found values were : Ea = 85, 176 and 101 kJ mol-1 , n= 0.23, 0.25, and 0.17, A= 2.40x10(9), 1.89x10(19) and 1.07x10(9) respectively. By TGA data, the kinetical patameters for the thermal decomposition of the adduct CdCl2.1,5 dmeu (dmeu=dimethylethyleneurea) were calculated by using five different methods.

Decomposição térmica do bicarbonato de sódio: do processo Solvay ao diagrama tipo Ellingham

A didactic experiment based on the thermal decomposition of sodium bicarbonate using a reagent found in the marketplace is proposed. The reaction products are identified by qualitative tests and stoichiometric calculations. The thermal stability of carbonates and the influence of lattice energies are discussed, emphasizing periodic trends in the alkali and alkaline earth families. The industrial importance of the reaction is also explored.

O efeito da granulometria na decrepitação durante a decomposição térmica de calcários e carvão

The use of fluidized bed combustors to burn coal is largely studied to permit the addition of limestone to capture SO2. The particle size for coal and limestone is an important parameter in this process. Thermogravimetry (TG) is used to elucidate the combustion and sulfation processes, but the experimental parameters must be evaluated to be representative in fluidized bed combustors. In the present study the effect of particle size is analyzed in the calcination of limestones and the combustion of coal through the thermogravimetric curve for limestone and derivative thermogravimetric curve for coal. Small peaks representing mass losses between 400 and 500 ºC are observed due to the jumping of particles out of the crucible. This effect, recognized as decrepitation is observed for mid-sized particles provoked by the release of water vapor trapped within their lattice.

Estudo de efeito dos sais precursores sobre as propriedades eletrocatalíticas de eletrodos de Ti-SnO2/Sb preparados por decomposição térmica

The physical and electrochemical properties of Ti-SnO2/Sb electrodes obtained by the thermal decomposition of solutions of the precursor salts SnCl2×2H2O/SbCl3 and SnSO4/Sb2(SO4)3 were investigated. The reversibility of the cyclic voltammetric response of the Fe(CN)6(4-)/Fe(CN)6(3-) redox couple was assessed using the obtained electrodes. Their catalytic activity for the oxygen-evolving reaction and maximum capacity for electronic transfer were also evaluated by potential and current linear scans in 0.5 mol L-1 H2SO4. Additionally, scanning electron microscopy analyses allowed the visualization of the morphology of the oxide films obtained. The best results were presented by the electrodes obtained from the chloride salt precursors.

Decomposição térmica de complexos de Zn e Cd com isomaleonitriladitiolato (imnt)

Thermal decomposition of [Bu4N]2[Zn(imnt)2] and [M(NH3)2(imnt)] complexes with M = Zn and Cd, and imnt = (bis 1,1-dicyanoethylene-2,2 dithiolate) in inert atmosphere was investigated by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). Pyrolysis studies at different temperatures, 300, 400, 500, and 600 ºC, in N2 atmosphere were performed and the products were characterized by X-ray diffraction (XRD), infrared and Raman spectroscopy, and scanning electron microscopy (SEM). The products were identified as sulfide sub-micron particles, along with amorphous carbon. Particle sizes estimated by SEM were ca. 50 nm for the cationic complexes and 500 nm for the neutral complexes.

Decomposição térmica de espumas de poliuretano para fabricação de vitrocerâmica celular de Li2O-ZrO2-SiO2-Al2O3 (LZSA)

Characterization of the thermal decomposition of polyurethane (PUR) foams was performed by Fourier-transformed infrared (FT-IR) spectroscopy and thermogravimetric analysis (TGA). Three main weight loss paths were observed by TGA, the residue being lower than 3 wt.% for 3 different PUR foams analyzed. FT-IR spectra indicated CO2, CO, NH3 and isocyanides as main decomposition products. PUR foams of different cell sizes were immersed in a slurry of the parent glass ceramic of composition Li2O-ZrO2-SiO2-Al 2O3 (LZSA) and submitted to heat treatment. The LZSA cellular glass ceramics obtained after sintering and crystallization resembled the original morphology of the PUR foams.

Estudo da decomposição térmica de propelente sólido compósito de baixa emissão de fumaça

The thermal decomposition of hydroxyl-terminated polybutadiene (HTPB)/ammonium nitrate (AN) based propellants, so called smokeless formulations, and raw materials were investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The thermoanalytical profile of different components and of propellant were evaluated and the Arrhenius parameters for the thermal decomposition of the propellant sample were determined by the Ozawa method. The kinetic parameters of the thermal decomposition of propellant samples were determined by DSC measurements. The values obtained for activation energy (Ea) and pre-exponential factor were 163 kJ mol-1 and 1.94x10(6) min-1.

Estudo cinético da decomposição térmica do pentaeretritol-tetranitrado (PETN)

The pentaerythritol-tetranitrate (PETN) is a nitroether used in explosives and propellant formulations. Due to its suitable properties, PETN is used in booster manufacture. Knowing the thermal decomposition behavior of an energetic material is very important for storage and manipulation, and the purpose of this work is to study the kinetic parameters of the decomposition of PETN, compare the results with literature data and to study the decomposition activation energy differences between two crystalline forms of PETN (tetragonal and needle) by means of differential scanning calorimetry (DSC). Fourier transform infrared spectroscopy (FT-IR) is used to study the two crystalline forms.

Estudo da decomposição térmica de oxalato de estrôncio dopado com cério(III) como precursor de materiais luminescentes

Este trabalho trata da obtenção de SrC2O4, Ce2(C2O4)3, e SrC2O4 dopado com diferentes porcentagens de Ce3+ como precursores do luminóforo azul Sr2CeO4. Os precursores preparados foram estudados por TG e DTA. Uma mistura contendo SrC2O4 e Ce2(C2O4)3 na relação 4:1 respectivamente e SrC2O4 dopado com diferentes porcentagens de Ce3+, foram tratadas termicamente à 1100ºC, 12 horas. Os produtos foram analisados por XRD e espectroscopia de luminescência e apresentam mistura das fases SrCeO3, Sr2CeO4 e SrCO3. Os produtos contendo a fase Sr2CeO4 apresentam luminescência azul de banda larga, com exceção daquele obtido a partir de SrC2O4 dopado com 50% de Ce3+. Neste caso a fase predominante é SrCeO3. Pela curva DTA observa-se um pico endotérmico em torno de 1000ºC para todas as amostras, com exceção da amostra dopada em 50%, evidenciando a temperatura de formação da fase Sr2CeO4. A fase luminescente Sr2CeO4 é preferencialmente obtida partindo-se de SrC2O4:Ce3+ 25% e de misturas mecânicas na proporção de 4:1 de oxalatos de estrôncio e de oxalato de cério.

Determinação dos parâmetros cinéticos de decomposição térmica para propelentes BS e BD

O propósito deste trabalho foi determinar os parâmetros cinéticos de decomposição térmica para uma amostra de propelente base simples e base dupla. Os dados obtidos pela calorimetria exploratória diferencial foram ajustados para o modelo cinético de pseudo-primeira ordem de Flynn, Wall e Ozawa. Os respectivos parâmetros obtidos foram: BS REX 1200 (Ea) (2,3 ± 0,2) 10² kJ mol-1 e (A) 1,34 10(25) min-1; BD-111 (Ea) (1,6 ± 0,1) 10² kJ mol-1 e (A) 3,31 10(17) min-1. O espectro de infravermelho da amostra de propelente base dupla indicou a presença de salicilato, justificando o comportamento de decomposição observado na respectiva curva térmica.

Estudo da decomposição térmica da madeira de oito espécies da região do Seridó, Rio Grande do Norte

Este trabalho teve como objetivo avaliar o perfil de decomposição térmica da madeira de oito espécies utilizando as técnicas de termogravimetria (TGA) e calorimetria diferencial exploratória (DSC), bem como a consistência desses métodos para decidir quais espécies devem ser indicadas para produção de energia e carvão vegetal, comparando-os com os rendimentos gravimétricos da carbonização obtidos a partir de carbonizações em mufla de laboratório. Para as análises por TGA e DSC, amostras de serragem foram aquecidas à taxa de 10 °C min-1, sob atmosfera de nitrogênio, em vazão de 50 ml min-1 até a temperatura final de 600 °C. Foram determinados os valores de densidade básica e poder calorífico superior da madeira. As carbonizações foram realizadas em mufla de laboratório à taxa de 50 °C h-1 até a temperatura máxima de 450 °C, obtendo-se os rendimentos em carvão vegetal. Também foram determinados os valores de densidade aparente do carvão das oito espécies após a carbonização. Os resultados das análises térmicas indicaram perfis de decomposição pirolítica das madeiras e evidenciaram aquelas mais estáveis à ação térmica. O comportamento da estabilidade térmica das madeiras das oito espécies foi confirmado pela análise dos rendimentos da carbonização em mufla, em comparação com a análise por TGA e DSC. As madeiras de Aspidosperma pyrifolium e Mimosa tenuiflora apresentaram maior estabilidade térmica e, portanto, maiores rendimentos em carvão vegetal, bem como maiores densidades aparentes. As técnicas de termogravimetria e calorimetria diferencial exploratória são satisfatórias para avaliação da decomposição térmica das madeiras e garantem consistência na escolha de madeiras que resultam em maior rendimento e maior qualidade do carvão vegetal.

Síntese, caracterização e cinética da decomposição térmica dos materiais cerâmicos PrMO3 (M = Ni ou Co)

In this work have been studied the preparation, characterization and kinetic study of decomposition of the polymerizing agent used in the synthesis under non-isothermal condition ceramics PrMO3 of general formula (M = Co and Ni). These materials were obtained starting from the respective metal nitrates, as a cations source, and making use of gelatin as polymerizing agent. The powders were calcined at temperatures of 500°C, 700°C and 900°C and characterized by X-ray Diffraction (XRD), Thermogravimetric Analysis (TG / DTG/ DTA), Infrared Spectroscopy (FTIR), Temperature Programmed Reduction (TPR) and Scanning Electron Microscopy (SEM). The perovskite phase was detected in all the X-rays patterns. In the infrared spectroscopy observed the oxide formation as the calcination temperature increases with the appearance of the band metal - oxygen. The images of SEM revealed uniform distribution for the PrCoO3 and particles agglomerated as consequence of particle size for PrNiO3. From the data of thermal analysis, the kinetics of decomposition of organic matter was employed using the kinetics methods called Model Free Kinetics and Flynn and Wall, in the heating ratios 10, 20 and 30° C.min-1 between room temperature and 700°C. Finally, been obtained the values of activation energy for the region of greatest decomposition of organic matter in samples that were determined by the degree of conversion (α)

Síntese de nanopartículas de magnetita via decomposição térmica em meio não-aquoso

This work aims at obtaining nanoparticles of iron oxide, the magnetite one (Fe3O4), via synthesis by thermal decomposition through polyol. Thus, two routes were evaluated: a simple decomposition route assisted by reflux and a hydrothermal route both without synthetic air atmosphere using a synthesis temperature of 260ºC. In this work observed the influence of the observe of surfactants which are generally applied in the synthesis of iron oxide nanoparticles decreasing cluster areas. Further, was observed pure magnetite phase without secondary phases generally found in the iron oxide synthesis, a better control of crystallite size, morphology, crystal structure and magnetic behavior. Finally, the introduction of hydroxyl groups on the nanoparticles surface was analyzed besides its employment in the polymer production with OH radicals. The obtained materials were characterized by XRD, DLS, VSM, TEM, TG and DSC analyses. The results for the magnetite obtainment with a particle size greater than 5 nm and smaller than 11 nm, well defined morphology and good magnetic properties with superparamagnetic behavior. The reflux synthesis was more efficient in the deposition of the hydroxyl groups on the nanoparticles surface

Estudo da decomposição térmica de oxalato de estrôncio dopado com cério(III) como precursor de materiais luminescentes

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)