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The temperature dependence on the reaction of desulfurization reagent CaCO_3 and SO_2 in O_2/CO_2 coal combustion was investigated by thermogravimetric analysis, X-ray diffraction measurement and pore structure analysis. The results show that the conversion of the reaction of CaCO_3 and SO_2 in air is higher at 500-1100 ℃ and lower at 1200℃ compared with that in O_2/CO_2 atmosphere. The conversion can be increased by increasing the concentration of SO_2, which causes the inhibition of CaSO_4decomposition and shifting of the reaction equilibrium toward the products. XRD analysis of the product shows that the reaction mechanism of CaCO_3 and SO_2 differs with temperature in O_2/CO_2 atmosphere, i.e. CaCO_3 directly reacts with SO_2 at 500℃ and CaO from CaCO_3 decomposition reacts with SO_2 at 1 000℃. The pore analysis of the products indicates that the maximum specific surface area of the products accounts for the highest conversion at 1 100 ℃ in O_2/CO_2 atmosphere. The results reveal that the effect of the atmosphere on the conversion is temperature dependence.