The invention provides a defluorination preparation method of
niobium pentoxide, which comprises the following steps: (1) mixing a
niobium hydroxide raw material with deionized water, and stirring until the
niobium hydroxide raw material and the deionized water are uniformly mixed to obtain a
slurry material; (2) uniformly smearing the
slurry-like material on the inner surface of a hollow cylindrical
crucible, and putting the hollow cylindrical
crucible into the middle section of a
glass tube of a
microwave tube furnace; (3) inserting a
thermocouple from one side of the
glass tube, enabling the end part of the
thermocouple to be in contact with the
slurry-like material in the hollow cylindrical
crucible, placing a
water vapor generating device on the other side of the
glass tube, and enabling a
water vapor tube of the
water vapor generating device to extend into the glass tube; and (4) starting the water vapor generating device and the
microwave tube furnace, raising the temperature of the slurry-like material in the hollow cylindrical crucible to a target temperature, preserving heat for 20-40 minutes, naturally cooling to
room temperature, and taking out to obtain
niobium pentoxide. According to the method, residual
fluorine can be efficiently removed while the purity of
niobium pentoxide is guaranteed, the
water consumption for washing is reduced, and the process period is shortened.