The invention discloses a preparation method of room-temperature ball-milling solid phase chemical reaction of rare earth mixing with nano stannic oxide, relates to a preparation technology of the rare earth mixing with the nano stannic oxide, which can be applied for antistatic coating, plastics, fibre and other fields. Inorganic salts containing stannum and rare earth are taken as reactants, oxalic acid, ammonium carbonate, ammonium bicarbonate, sodium oxalate or sodium carbonate is taken as a ligand, the processing steps are sequentially dosing, mixing and preparing precursors of the room-temperature ball-milling solid phase chemical reaction, and the targeted product can be obtained after impurity removing, drying and thermal decomposition. The preparation method is characterized in that the reaction process does not use water, the stannum ion can be prevented from hydrolysis, uniform mixing can be realized, a solid phase reaction system is broken by utilizing the shearing force and the impact force generated during the ball milling process, the specific surface area of the reactant is increased, the reaction rate is increased, micro-fine and uniform precursors can be prepared, then the processes of cleaning, drying and controlling the thermolysis temperature and time are carried out, and thereby the rare earth mixing with nano stannic oxide powder, the particle size distribution of which is 30 to 80nm and has controllable morphology, can be obtained.