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Manganese-based octahedral molecular sieves of the type K-OMS-2 (cryptomelane structure) were prepared via reflux method by synproportionation of KMnO 4 and Mn 2? in acidic aqueous suspension. For this method, different manganese anions (sulphate, chloride and acetate) were used, which exert a strong influence on the prepared materials. Several techniques such as X-ray diffraction, Fourier transformer infrared, Raman spectroscopy, transmission electron microscopy, differential and gravimetric thermal analysis and H 2 -temperature programmed reduction were used to characterize the prepared samples. The results revealed that the prepared samples were mainly pure mono-phase cryptomelane materials. The obtained K-OMS-2 material on using the sulphate anion has more available lattice oxygen as compared to that prepared by the other anions. The catalytic activity of the prepared samples was tested towards the oxidative dehydrogenation of cyclohexane. Over the K-OMS-2RS sample, cyclohexane conversion was significantly higher than the other prepared samples.

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