Zn–Ti–Co(Ni) sorbents for H2S removal from model hot coal were prepared and characterized. Effects of cobalt (Co) and nickel (Ni) on the sorbents texture, structure, H2S sorption capacity and regeneration properties were determined. TiO2 formed mixed metal oxides with CoO and NiO in the fresh sorbents, while TiO2 and nanocrystalline sulfides of Zn, Co, Ni were found in sulphided ones. The oxidative regeneration of sulphided sorbents re-formed mixed oxides. Sorption capacity of studied materials increased along with an increase of the amount of added Co (Ni) and also with the number of work cycles. Co-doped Zn–Ti materials adsorbed up to 244% more sulfur than these of Zn–Ti, while Ni-doped materials adsorbed ca. twice more H2S than the corresponding Co-doped sorbents. The addition of Co (Ni) decreased the temperature of ZnS oxidation. The catalytic effect of the Co (Ni) oxides on the oxidation of ZnS was suggested.