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Genesis of alumina supported hydrotreating (HDT) catalysts prepared with the use of decamolybdodicobaltate heteropolyanion and cobalt citrate during their sulfidation processes and deactivation in diesel HDT has been investigated. The sulfidation stage was studied for two procedures: gas phase sulfidation by H2S/H2 and liquid phase treatment by a mixture of dimethyldisulfide in diesel at various temperatures and durations. Mechanisms of the active phase formation in the course of gas and liquid phase sulfidation processes have been established. It was found that gas phase sulfidation led to formation of the CoMoS active phase with higher cobalt content comparing to liquid sulfidation of the catalyst and initial activity of the gas phase treated catalysts in diesel HDT was also higher than catalysts subjected to liquid sulfidation. Catalytic examination after accelerated deactivation conditions showed that the liquid phase sulfided sample was more resistant to the deactivation.