A stable and continuous leaching process for niobium and tantalum extraction from ferrocolumbium tantalum (FT) was developed. The effects of initial concentration of HF and H2SO4, grinding fineness, leaching time, and temperature on the leaching rate of Ta, Nb, Fe, and Si were studied. Experimental results show that the leaching rates of Ta, Nb, Fe, and Si were enhanced by the increase of acid concentrate, fineness, leaching time, and leaching temperature. The optimum process conditions are HF initial concentration of 5 mol/L, H2SO4 initial concentration of 2.5 mol/L, − 74 µm percentage of 65%, leaching time of 20 min, and leaching temperature of 25 °C. Continuous leaching of FT was carried out by feeding ore and acid every 20 min. By leaching with HF − H2SO4 for 4 h, then adding appropriate amount of HNO3 into the solution and keeping for another 1 h, a high Nb extraction rate of 99.8% was achieved. The established method provides a promising technique for the high-efficiency separation of niobium and tantalum from FT.Highlights: • The priority of metal extraction in HF−H2SO4 system is Si > Fe > Ta > Nb.• Ferrocolumbium tantalum can be stable leached by introducing raw material and acid every 20 min.• A high Nb extraction rate of 99.8% was achieved by the continuous leaching process.Graphical abstract: