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Perovskite-type oxides of the general formula ABO3 is a promising material as catalyst for the oxidative dehydrogenation of cyclohexane and oxidative coupling of methane to produce benzene and C2 (ethane and ethene) respectively. Perovskite LaNiO3, substituted La-perovskites (La1- xSrxNiO3 and La1-xLixNiO3) and doubled layered perovskite La2NiO4 samples were prepared by single and/or reverse microemulsions. Characterizations of the prepared perovskite samples have been studied by different teqnices; XRD, N2 adsorptiondesorption, DTA/ TGA, TEM and ICP-OES. The observed results indicated that all prepared samples are well crystalline, high surface area SB Et, nanaparticles of 9-38 nm in size and their particle sizes are almost uniform. The results of the catalytic activity showed that the prepared nano structured perovskite LaNiO3 and La0.6Sr0.4NiO3 samples are the most selective catalysts towards the oxidative dehydrogenation of cyclohexane (i.e. towards benzene formation) reachedto 91 , 95% respectively.