Abstract: In this paper, the by-product (zinnwaldite) of tantalum-niobium ores in Jiangxi province was studied. Magnetic separation and flotation were tried to improve the quality of zinnwaldite. Finally, the high quality zinnwaldite concentrate with content Li₂O 2.45% and Rb₂O 0.81% was acquired by the flow sheet of grinding-floatation. This resource is comprehensive utilized, which, resulted in both social and economic effect.