ZnO-Al2O3 mixed oxides were synthesized using a freeze drying modified cation-anion double hydrolysis method Freeze dried adsorbents exhibited a superior performance in reactive adsorption desulfurization A large amount of small sized ZnO gives rise to a large sulfur capacity The absence of the inactive NiAl2O4 phase in the adsorbents allows the fast cleavage of C-S bond in thiophene High surface area and large pore volume facilitate the mass transfer of reactants and accommodate more sulfur