The invention provides a method for separating uranium and neptunium through a fluorinated volatilization technology. The method comprises the following steps that (1), air and water in a reactor are removed, the reactor is filled with a mixture A or a mixture B, the mixture A comprises a substance containing uranium elements and neptunium elements, the mixture B comprises a substance containing uranium elements, a substance containing neptunium elements and fused salt, the substance containing uranium elements comprises uranium elementary substance and/or uranium compound; and the substance containing neptunium elements is neptunium elementary substance and/or neptunium compound; (2), reaction products containing uranium elements are recycled; and (3) the residual product after the uranium elements are recycled is cooled to 350-600 DEG C, mixed gas of fluorine gas and inert gas is introduced, a reaction product containing neptunium elements is recycled; and the reaction temperature in the step 2 is higher than that in the step 3. The method has the advantages that the reaction speed is high, the conversion rate of uranium and neptunium is large, the separation efficiency of uranium and neptunium is high, side reactions are few, the separation selectivity is good, and serialization is easy.