Aiming at different tantalum-containing niobium raw materials, the high purity niobium pentoxide was prepared by single extraction method, and the large-scale stable production of high purity niobium pentoxide with different physical and chemical properties was realized directly from raw materials. The separation and concentration technology of nanofiltration and reverse osmosis has been developed for fluoride alkaline wastewater from the tantalum-niobium industry, to realize the resource recovery and nearly zero discharge of alkaline wastewater in the production process.