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Zinc oxide/ and iron oxide/SBA-15 composites were synthesized using the innovative Two-Solvents procedure and tested as sorbents for the mid-temperature (300 C) removal of hydrogen sulphide, and then compared with a commercial unsupported ZnO sorbent. The sulphur retention capacity results showed the superior performance of the iron oxide/SBA-15 composite (401 mg S g1 Fe2O3) in comparison with the zinc oxide/SBA-15 composite (53 mg S g1 ZnO), both these sorbents being much more efficient than the commercial sorbent (6 mg S g1 ZnO). The different sorption behaviour was discussed in terms of the nature of the nanocomposites where: (i) the mesostructure of the support was retained with a high surface area and pore volume; (ii) the zinc oxide phase was incorporated inside the SBA-15 channels as a thin amorphous homogeneous layer while the iron oxide was dispersed in form of small maghemite crystallites; and (iii) significant interactions occurred between the silica matrix and the zinc oxide phase. Remarkable differences in the regeneration behaviour of the exhaust sorbents were revealed by temperature-programmed experiments under an oxidizing atmosphere. After regeneration, the sorption properties of the zinc oxide/SBA-15 composite appeared to be enhanced compared to the commercial sorbent. Incomplete recovery of the sorption activity was observed for the regenerated iron oxide/SBA-15 sorbent, whose performance remained far better than that of the ZnO-based one, either fresh or regenerated. In view of its higher sulphur retention capacity and appropriate regeneration temperature (T # 350 C), the iron oxide/SBA-15 composite is a promising material for the design of advanced sorbents for a thermally efficient H2S removal process from hot gas streams

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