Síntese e caracterização de materiais nanoporosos para pirólise catalítica de óleos pesados

The present work reports the study of nanoporous structures, aiming at their use in research directed to the current demand of the petroleum industry to value heavy oil. Initially, two ways were chosen for the synthesis of porous structures from the molecular sieves of type Si-MCM-41. In the first way, the structure MCM-41 is precursory for heteroatom substitutes of silicon, generating catalyst of the type Al-MCM-41 from two different methods of incorporation of the metal. This variation of the incorporation method of Aluminum in the structure of Si-MCM-41 was carried out through the conventional procedure, where the aluminum source was incorporated to the gel of synthesis, and the procedure post-synthesis, where the Aluminum source was incorporated in catalyst after the synthesis of Si-MCM-41. In the second way, the MCM-41 acts as a support for growth of nanocrystals of zeolite embedded in their mesoporous, resulting in hybrid MCM-41/ZSM-5 catalyst. A comparative analysis was carried through characterizations by XRD, FTIR, measures of acidity through n-butylamine adsorption for TGA, SEM-XRF and N2 adsorption. Also crystalline aluminosilicate with zeolitic structure MFI of type ZSM-5 was synthesized without using organic templates. Methodologies to the preparation of these materials are related by literature using conventionally reactants that supply oxides of necessary silicon and aluminum, as well as a template agent, and in some cases co-template. The search for new routes of preparation for the ZSM-5 aimed at, above all, the optimization of the same as for the time and the temperature of synthesis, and mainly the elimination of the use of organic templates, that are material of high cost and generally very toxic. The current study is based on the use of the H2O and Na+ cations playing the role of structural template and charge compensation in the structure. Characterizations by XRD, FTIR, SEM-XRF and N2 adsorption were also conducted for this material in order to compare the samples of ZSM-5 synthesized in the absence of template and those used industrially and synthesized using structuring

Síntese, caracterização e aplicação do MCM-41 e A1-MCM-41 na pirólise do resíduo atmosférico de petróleo

In present work, mesoporous materials of the M41S family were synthesized, which were discovered in the early 90s by researchers from Mobil Oil Corporation, thus allowing new perspectives in the field of catalysis. One of the most important members of this family is the MCM-41, which has a hexagonal array of mesopores with pore diameters ranging from 2 to 10 nm and a high surface area, enabling it to become very promising for the use as a catalyst in the refining of oil in the catalytic cracking process, since the mesopores facilitate the access of large hydrocarbon molecules, thereby increasing the production of light products, that are in high demand in the market. The addition of aluminum in the structure of MCM-41 increases the acidity of the material, making it more beneficial for application in the petrochemical industry. The mesoporous materials MCM-41 and Al-MCM-41 (ratio Si / Al = 50) were synthesized through the hydrothermal method, starting with silica gel, NaOH and distilled water. CTMABr was used as template, for structural guiding. In Al-MCM-41 the same reactants were used, with the adding of pseudoboehmite (as a source of aluminum) in the synthesis gel. The syntheses were carried out over a period of four days with a daily adjustment of pH. The optimum conditions of calcination for the removal of the organic template (CTMABr) were discovered through TG / DTG and also through analysis by XRD, FTIR and Nitrogen Adsorption. It was found that both the method of hydrothermal synthesis and calcination conditions of the studies based on TG were promising for the production of mesoporous materials with a high degree of hexagonal array. The acidic properties of the materials were determined by desorption of n-butylamine via thermogravimetry. One proved that the addition of aluminum in the structure of MCM-41 promoted an increase in the acidity of the catalyst. To check the catalytic activity of these materials, a sample of Atmospheric Residue (RAT) that is derived from atmospheric distillation of oil from the Pole of Guamaré- RN was used. This sample was previously characterized by various techniques such as Thermogravimetry, FTIR and XRF, where through thermal analysis of a comparative study between the thermal degradation of the RAT, the RAT pyrolysis + MCM-41 and RAT + Al- MCM-41. It was found that the Al-MCM-41 was most satisfactory in the promotion of a catalytic effect on the pyrolysis of the RAT, as the cracking of heavy products in the waste occurred at temperatures lower than those observed for the pyrolysis with MCM-41, and thereby also decreasing the energy of activation for the process and increasing the rates of conversion of residue into lighter products

Avaliação da síntese e caracterização de zeólita ZSM-5 ausente de direcionador orgânico estrutural

The catalytic processes play a vital role in the worldwide economy, a business that handles about US$ 13 billion per year because the value of products depends on the catalytic processes, including petroleum products, chemicals, pharmaceuticals, synthetic rubbers and plastics, among others. The zeolite ZSM-5 is used as catalyst for various reactions in the area petrochemical, petroleum refining and fine chemicals, especially the reactions of cracking, isomerization, alkylation, aromatization of olefins, among others. Many researchers have studied the hydrothermal synthesis of zeolite ZSM-5 free template and they obtained satisfactory results, so this study aims to evaluate the hydrothermal synthesis and the physicochemical properties of ZSM-5 with the presence and absence of template compared with commercial ZSM-5. The methods for hydrothermal synthesis of zeolite ZSM-5 are of scientific knowledge, providing the chemical composition required for the formation of zeolitic structure in the presence and absence of template. Samples of both zeolites ZSM-5 in protonic form were obtained by heat treatment and ion exchange, according to procedures reported in the literature. The sample of commercial ZSM-5 was acquired by the company Sentex Industrial Ltda. All samples were characterized by XRD, SEM, FTIR, TG / DTG / DSC, N2 adsorption and desorption and study of acidity by thermo-desorption of probe molecule (n-butylamine), in order to understand their physicochemical properties. The efficiency of the methods applied in this work and reported in the literature has been proved by well-defined structure of ZSM-5. According as the evaluation of physicochemical properties, zeolite ZSM-5 free template becomes promising for application in the refining processes or use as catalytic support, since its synthesis reduces environmental impacts and production costs

Obtenção de biodiesel através da transesterificação do óleo de farelo de arroz utilizando KI/Al2O3

This study proposes to find a biodiesel through transesterification of rice bran oil with KI/Al2O3 checking the influence of two types of alumina (Amorphous and Crystalline) for conversion into methyl esters. The catalyst was synthesized by the wet impregnation method. Adding 30 mL of 35% KI(aq.) in 10 g of alumina, under stirring at 80 °C for 3 hours. The reaction conditions used in this study were optimized, with a molar ratio methanol:oil of 15:1, 8 h of reaction time and reflux temperature. The catalyst amount was varied in the range of 1 to 5 % wt. The solid catalysts materials were analyzed by: x-ray diffraction (XRD), thermogravimetry (TG), N2 adsorption/desorption, scanning electron microscopy (SEM) and basicity, for the identification of its structure and composition, verifying the presence of basic sites. The results showed that Al2O3(A) presents an amorphous structure, high surface area and a better catalytic activity, in relation to the catalyst synthesized with Al2O3(C) support that proved to have a more crystalline structure, having as well, a lesser surface area, enabling difficulties for the incorporation of active sites. The obtained biodiesel with 5% wt. KI/Al2O3(A) presented physicochemical properties within the standards specified by the Resolution No 7/2008 ANP and obtained the best reaction yield with 95.2%, according to quantitative measurement from the TG, which showed 96.2% conversion into methyl esters. It was furthermore found that with the increasing amount of the quantity of the catalyst in the reaction, there was also an increase in the ester content obtained. The specific mass and the kinematic viscosity were reduced with the increase of the amount of quantity of the catalyst, indicating an increase in the conversion of triglycerides

Avaliação da remoção de hidrocarbonetos aromáticos (BTEX) em águas utilizando materiais nanoestruturados do tipo Ti-MCM-41

Volatile Organic Compounds are pollutants coming mainly from activities that use fossil fuels. Within this class are the BTEX (benzene, toluene, ethylbenzene and xylenes) compounds that are considered hazardous. Among the various existing techniques for degradation of pollutants, there is advanced oxidation using H2O2 generating hidoxil radical ( OH). In this work, the mesoporous material of MCM-41 was synthesized by hydrothermal method and then was used as support, the impregnation of titanium by the method of synthesis with excess solvent to obtain the catalyst Ti-MCM-41. The catalyst was used in the reaction catalyzed removal of BTEX in water using H2O2 as oxidant. The materials were characterized by: XRD, TG/DTG, FTIR, nitrogen adsorption-desorption and FRX-EDX, in order to verify the method of impregnation of the mesoporous titanium support was effective. Catalytic tests were carried out in reactors of 20 mL containing BTEX (100.0 μg/L), H2O2 (2.0 M) and Ti-MCM-41 (2.0 g/L) in acid medium. The reaction occurred for 5 h at 60 °C and analysis were performed by gas chromatography with photoionization detector and static headspace sampler. The characterizations have proven the effectiveness of the synthesis method used and the incorporation of titanium lt in the support. The catalytic tests showed satisfactory results with conversion of more than 95 % for the studied compounds, where the catalyst 48% Ti-MCM-41 showed a higher removal efficiency of the compounds under study

Síntese, caracterização e estudo cinético da degradação de quitosana impregnada em SBA-15

O recente interesse em se obter materiais nanoporosos funcionalizados para aplicações como calisadores heterogêneos e adsorção de CO2, tem aumentado no meio industrial e cientifico. Nesta última aplicação, a introdução de grupos aminas, como os presentes em quitosana, em materiais nanoporosos do tipo SBA-15 para gerar interações específicas com o CO2 tem ganhado importância. Assim, neste trabalho foram realizadas a síntese do SBA-15 e posterior impregnação da CS no suporte mesoporoso através do método de impregnação por via úmida. Os materiais obtidos foram caracterizados por meio DRX, TG, DSC, MEV, FTIR e adsorção/dessorção de N2. Os resultados de DRX indicaram que a estrutura ordenada do suporte SBA-15 foi preservada após a impregnação e os cálculos mostraram que o diâmetro médio do poro e/ou a espessura média da parede (wt) foram alterados devido a introdução da quitosana nas amostras funcionalizadas. As curvas de TG e de DSC,corroboraram com os dados de DRX, indicando a presença da quitosana na estrutura mesoporosa do SBA-15, assim como as micrografias das amostras funcionalizadas, que possibilitou visualizar o estado de agregação do material obtido. As bandas características de absorção da CS na região IV foram identificadas e interpretadas nas amostras funcionalizadas confirmando as outras caracterizações. Foi visto também que a área superficial diminuiu nas amostras funcionalizadas, indicando a sucessiva incorporação do polímero no suporte mesoporoso. A energia de ativação do processo de degradação térmica da quitosana impregnada no suporte foi determinada por meio do método de cinética livre de Viazovkin e pelo método de Ozawa-Flay-Wall com os resultados indicando que o aumento da quitosana diminui em aproximadamente 10% a energia de ativação para sua degradação.

Remediação de solos contaminados com diesel por lavagem com solução de tensoativos

Combating pollution of soils is a challenge that has concerned researchers from different areas and motivated the search for technologies that aim the recovery of degraded soils. Literature shows numerous processes that have been proposed with the intent of remediating soils contaminated by oils and other by-products of the oil industry, considering that the processes available have, generally, high operating costs, this work proposes a costeffective alternative to the treatment of Diesel-contaminated soils. The washing solutions were prepared using water as aqueous phase, the saponified coconut oil (OCS) as surfactant and n-butanol as co-surfactant. In this study, the soil was characterized by physical and chemical analyses. The study of diesel desorption from the soil was held in bath, using hexane and washing solutions, which had 10 and 20 wt.% active matter (AM - co-surfactant/surfactants) respectively. The study of the influence of active matter concentration and temperature in bath agitated used an experimental planning. The experiment also developed a system of percolation in bed to wash the soil and studied the influence of the concentration of active substance and volume of washing solution using an experimental planning. The optimal times to achieve hexane extraction were 30 and 180 min, while the best results using a 10% AM was 60 min and using a 20% AM was 120 min. The results of the experimental planning on bath showed that the maximum diesel removal was obtained when at a 20 wt.% of AM and under 50 °C, removing 99.92% of the oil. As for experiments in the system of percolation soil bed, the maximum diesel removal was high when the volume of the washing solution was of 5 L and the concentration of 20% AM. This experiment concluded that the concentration of AM and the temperature were vital to bath experiments for diesel removal, while in the system of percolation soil bed only concentration of AM influenced the soil remediation

Síntese, caracterização e estudo cinético da degradação de quitosana impregnada em SBA-15

The recent interest in obtaining functionalized nanoporous materials for applications such as heterogeneous catalysts and adsorption of CO2 has increased today. In the latter application, the introduction of amino groups such as present in the chitosan (CS), in the nanoporous materials like SBA-15 to generate specific interactions with CO2 has gained importance. In this work were performed to hydrothermal synthesis of SBA-15 and subsequent impregnation of the CS in the support mesoporous by the method of the wet impregnation. The materials were characterized by TG/DTG, DSC, XRD, SEM, FTIR and adsorption / desorption of N2. The XRD showed that the ordered structure of the support SBA-15 was preserved after the impregnation and calculations have shown that the average pore diameter (Dp) and / or the average wall thickness (wt) have been changed due to introduction of the CS in the samples functionalized. The curves of TG and DSC data corroborates the XRD, indicating the presence of CS in the nanoporous structure of SBA-15, as well as micrographs of samples, which allowed the display state of aggregation of the material obtained. The characteristics of bands absorption in the region of the CS in the FTIR were identified and interpreted in the samples functionalized, confirming the further characterization. Measurements showed that the BET surface area decreases in the functionalized samples, indicating the successive incorporation of the polymer in the nanoporous support. The activation energy apparent (Ea) for the process of thermal degradation of CS in the impregnated support was determined by the methods of kinetic freedom Vyazovkin and Ozawa-Flynn-Wall with the results indicating that the sample functionalized CS/SBA-15 2,5 % was decrease of the Ea in their degradation of about 10% compared to 1,0 % CS/SBA-15 sample

Dessulfurização oxidativa em diesel utilizando catalisadores à base de vanádio ou manganês

The oxidative desulfurization process (ODS) of a commercial diesel fuel was performed under mild conditions in the presence of catalysts based on vanadium or manganese, supported on alumina, clays (commercial, natural and pillared) and zeolites (NaX, NaY, beta, mordenite and ZSM-5). The catalysts were synthesized by wet impregnation and characterized by X-ray diffraction, textural analysis by N2 adsorption and scanning electron microscopy. The dibenzothiophene (DBT) was used as sulfur compound in catalytic evaluation. The reactions were performed using acetonitrile as solvent and the hydrogen peroxide as oxidant at 55°C. The reaction products were analized by gas chromatography (GC-FID). In the studied conditions, the process was efficient due to the DBT was converted to its corresponding sulfone. Both DBT and corresponding sulfone were extracted by the solvent. Removals and oxidations up to 100% of sulfur compound were achieved. The catalysts supported on ZSM-5 zeolite showed are more effective for oxidation reaction of sulfur compound, presenting the best results. It was observed for oxidation reaction, that vanadium catalysts were more effective and manganese catalysts showed best results for removal of sulfur compounds

Degradação de compostos orgânicos voláteis usando o catalisador SBA-15 contendo titânio

The groundwater pollution arising due to fuel leaks gas stations has presented a problem aggravating. Increasingly studies related to environmental problems such accidents and seek to propose some solutions for the treatment of groundwater and soils that are contaminated by gasoline. This study evaluated the use of molecular sieve TiSBA-15 as a catalyst for the reaction of removing of volatile organic compounds, particularly benzene, toluene, ethylbenzene and xylenes, known as BTEX, one of the main pollutants found in groundwater. The catalyst was synthesized by the method post-synthesis techniques and characterized by XSD, TG/DTG, adsorption/desorption of N2, XRF-EDX, for checking the incorporation of titanium and formation of the structure of the catalyst. The reaction occurred with the presence of hydrogen peroxide, H2O2, in aqueous medium to form hydroxyl radicals, which are needed in the process of removal of BTEX compounds. The catalytic reaction was carried out for 5 hours at 60 °C, pH to 3.0, and analyzes of the compounds were made in a gas chromatograph with a flame detection means photoionization static headspace (HS-GC-PID). The catalytic tests have shown the efficacy of using this type of catalyst for the removal of these volatile organic compounds, having a removal rate of 90.60% in the range where the catalyst was studied TiSBA-15(5,0)

Hidróxidos duplos lamelares de magnésio e alumínio modificados com carbonato e p123 para adsorção de dióxido de carbono

Muitos mecanismos provocados pela ação humana vêm gerando um aumento na queima de combustíveis fósseis e processos químicos (produtos orgânicos, carvão, madeira, óleo diesel, gasolina e outros derivados de petróleo) e, consequentemente, há um aumento na emissão de CO2 na atmosfera. Uma das alternativas para a captura desse poluente é o processo de adsorção, o qual pode ajudar na redução do CO2. As hidrotalcitas ou hidróxidos duplos lamelares (HDL s) estão dentre esses materiais estudados, já que apresentam alta estabilidade e uma boa porosidade, tornando-se assim um promissor adsorvente de gases poluentes. Os HDL s formam um grupo de argilas do tipo aniônico que consiste em camadas positivamente carregadas de óxido de metal (ou hidróxido de metal) com intercamadas de ânions. Foi constatado que ânions que possuem duas cargas negativas, estabilizam muito mais que ânions monovalentes, sendo o carbonato o mais estável dos ânions divalentes. Neste trabalho, foi proposta uma modificação na síntese direta através da co-precipitação a pH constante utilizando sais de cátions divalentes (Mg2+) e trivalentes (Al3+) reportados na literatura. Durante a síntese dos HDL s retirou-se o carbonato, bem como, utilizou-se um copolímero como um template para o alargamento das lamelas. As amostras foram caracterizadas utilizando as técnicas de DRX, TG/DTG, FTIR, MEV/EDX, MET e adsorção e dessorção de N2. Os dados obtidos indicam que a estrutura, mesmo após a modificação, apresentou resultados condizentes com os encontrados na literatura. Dentre as várias aplicações dos HDL s foi realizado o estudo da adsorção do CO2. A capacidade de adsorção do material foi testada de acordo com o tempo de contato entre o adsorvente e o adsorbato, sendo esperado que os materiais tratados com template apresentassem um maior desempenho

Síntese e caracterização de membranas zeolíticas tipo mfi e aplicação em separação de aromáticos

The synthesis of MFI-type zeolite membranes was carried by the process in situ or hydrothermal crystallization. We studied the homogenization time of the room temperature and gel filtration just before the crystallization step performed out in an oven, thus obtaining a more uniform zeolite film. The powder synthesized zeolite (structure type MFI, Silicalite) was characterized by several complementary techniques such as Xray diffraction (XRD), scanning electron microscopy (SEM), thermal analysis, temperature programmed desorption (TPD), Fourier Transform infrared spectroscopy (FTIR) and textural analysis by nitrogen adsorption (specific surface area). For the purpose of evaluating the quality of the layer supported on the ceramic support, N2 permeation tests were carried starting from room temperature to 600 °C, where values were observed values more appropriate permeation from 200 °C. With the data obtained, it was made into a graph of temperature versus permeation function, the curve of surface diffusion was found. For scanning electron microscopy, we observed the formation of homogeneous crystals and the zeolite film showed no fissures or cracks, indicating that the process of synthesis and subsequent treatments not damaged the zeolite layer on the support. Carried permeation studies were found values ranging from 3.64x10-6 to 3.78x10-6, 4.71x10-6 to 5.02x10-6, to pressures 20 and 25 psi, respectively. And the mixture xylenes/N2 values were between 5.39x10-6 to 5.67x10-6 and 8.13x10-6 to 8.36x10-6, also for pressures of 20 and 25 psi. The values found for the separation factor were 15.22 at 400 °C in the first experiment and 1.64 for the second experiment at a temperature of 150 °C. It is concluded that the Silicalite membrane was successfully synthesized and that it is effective in the separation of binary mixtures of xylenes

Obtenção de diesel verde por craqueamento termocatalítico de óleo de buriti (Mauritia flexuosa L.) sobre materiais nanoestruturados do tipo LaSBA-15

In order to obtain a biofuel similar to mineral diesel, lanthanum-incorporated SBA- 15 nanostructured materials, LaSBA-15(pH), with different Si/La molar ratios (75, 50, 25), were synthesized in a two-steps hydrothermal procedure, with pH-adjusting of the synthesis gel at 6, and were used like catalytic solids in the buriti oil thermal catalytic cracking. These solids were characterized by X-ray fluorescence (XRF), powder X-ray diffraction (XRD), thermogravimetric analysis (TG/DTG), infrared spectroscopy (FTIR), nitrogen porosimetry and ethanol dehydration, aiming to active sites identify. Taken together, the analyses indicated that the synthesis method has employed to obtain materials highly ordered mesostructures with large average pore sizes and high surface area, besides suggested that the lanthanum was incorporated in the SBA-15 both into the framework as well as within the mesopores. Catalytic dehydration of ethanol over the LaSBA-15(pH) products has shown that they have weak Lewis acid and basic functionalities, indicative of the presence of lanthanum oxide in these samples, especially on the La75SBA-15(pH) sample, which has presented the highest selectivity to ethylene. The buriti oil thermal and thermal catalytic cracking, realized from the room temperature to 450 ºC in a simple distillation system, has allowed obtaining two liquid fractions, each consisting of two phases, one aqueous and another organic, organic liquid (OL). The OL obtained from first fractions has shown high acid index, even in the thermal catalytic process. One the other hand, OL coming from second ones, called green diesel (GD), have presented low acid index, particularly that one obtained from the thermal catalytic process realized over LaSBA-15(pH) samples. The acid sites presence in these samples, associated to their large average pore sizes and high surface areas, have allowed them, especially the La75SBA-15(pH), to present deoxygenating activity in the buriti oil thermal catalytic cracking, providing an oxygenates content reduction, particularly carboxylic acids, in the GD. Furthermore, the GD comes from the second liquid fraction obtained in the buriti oil thermal catalytic cracking over this latest solid sample has shown hydrocarbons composition and physic-chemical properties similar to that mineral diesel, beyond sulfur content low

Síntese, caracterizaçao e propriedades catalicas da peneira molecular nanoestruturada modificada com lantanio

The nanostructured molecular sieve SBA-15 was synthesized by the hydrothermal method, and modified with lanthanum with Si/La molar ratios of 25, 50, 75 and 100. The materials were evaluated as catalysts for the cracking of n-hexane model reaction. Type SBA- 15 and LaSBA-15 mesoporous materials were synthesized using tetraetilortosilicato as a source of silica, hydrochloric acid, heptahydrate lanthanum chloride and distilled water. Pluronic P123 triblock. polymer was used as structure template. The syntheses were carried out by 72 hours. The obtained SBA-15 samples were previously analyzed by thermogravimetry, in order to check the conditions of calcination for removal of organic template. Then, the calcined materials were characterized by X-ray diffraction, infrared spectroscopy, adsorption and desorption of nitrogen, scanning electron microscopy and X-ray microanalysis by dispersive energy. The acidity of the samples was determined using adsorption of n-bulinamina and desorption followed by thermogravimetry. It was found that the hydrothermal synthesis method was suitable for the synthesis of the SBA-15 mesoporous materials, with an excellent degree of hexagonal ordering. The reactions of catalytic cracking of n-hexane were carried out using a fixed bed continuous flow microreactor, coupled on-line to a gas chromatograph. From the catalytic evaluation, it was observed that the mesoporous materials containing lanthanum showed different results for the reaction of cracking of nhexane compared to the unmodified mesoporous material SBA-15. As a result of cracking was obtained as main products hydrocarbons in the range of C1 to C5. The catalyst that showed better properties in relation to the acidity and catalytic activity was LaSBA-15 with the ratio Si/La = 50

Carregadores de oxigênio a base de níquel suportado em materiais mesooros para aplicação na recirculação química com reforma (RQR)

Oxygen carriers are metal oxides which have the ability to oxidize and reduce easily by various cycles. Due to this property these materials are widely usedin Chemical-Looping Reforming processes to produce H2 and syngas. In this work supports based on MCM-41 and La-SiO2 were synthesized by hydrothermal method. After the synthesis step they were calcined at 550°C for 2 hours and characterized by TG, XRD, surface area using the BET method and FTIR spectroscopy. The deposition of active phase, in this case Nickel, took place in the proportions of 5, 10 and 20% by weight of metallic nickel, for use as oxygen carriers.The XRD showed that increasing in the content of Ni supported on MCM-41 resulted in a decrease in spatial structure and lattice parameter of the material. The adsorption and desorption curves of the MCM-41 samples exhibited variations with the increase of Ni deposited. Surface area, average pore diameter and wall density of silica showed significant changes , due to the increase of the active phase on the mesoporous material. By other hand, in the samples with La-SiO2 composition was not observed peaks characteristic of hexagonal structure, in the XRD diffractogram. The adsorption/desorption isotherms of nitrogen observed are type IV, characteristic of mesoporous materials. The catalytic test indicates that the supports have no influence in the process, but the nickel concentration is very important, because the results for minor concentration of nickel are not good. The ratio H2/O2 was close to 2, for all 15 cycles involving the test storage capacity of O2, indicating that the materials are effective for oxygen transport