Síntese e Caracterização de Titanatos de Cobalto e Níquel, dopados com Praseodímio, obtidos a partir da decomposição de Nitrilotriacetatos

In recent years, studies about the physicochemical properties of mixed oxides, call attention of the scientific community, properties like as piezoelectricity, photoluminescence, or applications as catalysts, arise in these compounds, when their chemical compositions are modified, in this context some routes are employed in the synthesis of these materials, among which can be cited these methods: ceramic, combustion, co-precipitation, Pechini or polymeric precursor method, hydrothermal, sol-gel; these routes are divided into traditional routes or chemical routes. In this work were synthesized oxides with variable composition, from the thermal decomposition of titanium, cobalt, nickel and praseodymium nitrilotriacetates. The nitrilotriacetates were characterized by IR Spectroscopy (FTIR), Thermogravimetric (TG/ DTG) and Differential Scanning Calorimetry (DSC), while oxides have been characterized by X-ray diffraction (XRD), Spectrofluorimetry and IR Spectroscopy (FTIR). From FTIR data, it was demonstrated that the displacement of the band corresponding to the carboxylate group (νCOOH) at 1712 cm-1, present in nitrilotriacetic acid (H3NTA), for 1680-1545 cm-1, these stretches are characteristics of coordinated nitrilotriacetates, By thermal analysis (TG/DTG /DSC), it was suggested, that in an oxidizing atmosphere (air) oxides are obtained at lower temperatures than in an inert atmosphere N2(g). By results from X-ray Diffraction (XRD), it was determinated that the oxides are crystalline and the predominant phases obtained are summarized titanate phases rutile and ilmenite. By fluorimetry was observed that the intensity of emission bands are directly proportional to the concentration of ions Ni2+, Co2+ and Pr3+, and IR spectroscopy (FTIR) from oxides, demonstrated the disappearance of characteristic bands by nitrilotriacetates, determining the complete decomposition of the nitrilotriacetates in oxides

Síntese de carreadores de oxigênio à base de Ni e Co para estudo do processo de Chemical Looping usando CH4 como combustível

Increasing energy demand is being met largely by fossil fuel reserves, which emit CO2, SOx gases and various other pollutants. So does the search for fuels that emit fewer pollutants and have the same energy efficiency. In this context, hydrogen (H2) has been increasingly recognized as a potential carrier of energy for the near future. This is because the H2 can be obtained by different routes and has a wide application area , in addition to having clean burning, generating only H2O as a product of combustion , and higher energy density per unit mass . The Chemical Looping Reforming process (CLR) has been extensively investigated in recent years, it is possible to regenerate the catalyst by applying cycles of reduction and oxidation. This work has as main objective to develop catalysts based on nickel and cobalt to study the reactivity of reform with chemical recycling process. The catalysts were prepared by three different methods: combustion assisted by microwave, wet impregnation and co-precipitation. All catalysts synthesized have the same amount by weight of the active phases (60% w / w). The other 40 % m/m consists in La2O3 (8% w / w), Al2O3 (30% w / w) and MgO (2%). Oxygen carriers have been named as follows: N or C, nickel or cobalt, followed by the number 3 or 6, meaning 30 to 60% of active phase in the oxide form and C, CI or CP, which means self-combustion assisted by microwave, self-combustion assisted by microwave followed by wet impregnation and co-precipitation. The oxygen carriers were then characterized by the techniques of X-ray diffraction (XRD), surface area (BET), temperature programmed reduction (TPR) and scanning electron microscopy (SEM). The characterization results showed that the different synthesis methods have led to obtaining different morphologies and structures. Redox tests using CH4 as reducing agent and sintetic air as oxidant agent was done with N6C and C6C, N6CI and C6CI and N6CP and C6CP oxygen carriers. The tests revealed different behaviors, depending on active phase and on synthesis procedure. N6C oxygen carrier produced high levels of H2. The C6CI oxygen carrier produced CO2 and H2O without carbon deposits.