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Baotou RE concentrate was decomposed with concentrated sulfuric acid by controlling the roasting temperature below 500℃. Thermogra-vimetry-differential thermal analysis (TG-DTA) and chemical analytical methods were used to study the thermal decomposition process and the thermal decomposition effect. The Freeman-Carroll method was applied to analyze the TG-DTA curves. The activation energy, reaction order, and reaction frequency factor at different stages were calculated. The Satava method was used to deduce the reaction mechanism and the relative reaction rate during the thermal decomposition process.