CN-122012953-A - Method for utilizing iron, rare earth and niobium elements in stone-like niobium concentrate

Abstract

The invention relates to a method for utilizing iron, rare earth and niobium elements in easily-resolvable stone type niobium concentrate, belongs to the field of mineral processing and hydrometallurgy, and solves at least one of the problems that multi-element recovery of niobium, iron and rare earth is difficult to cooperatively utilize, the process flow is complex, the energy consumption and the cost are high, the reaction condition is harsh, the environmental pollution risk is high and the like in the prior art. The method comprises the steps of uniformly mixing niobium concentrate with a reducing agent, pelletizing, reducing and roasting to obtain roasted ore, crushing the roasted ore, carrying out magnetic separation to obtain iron concentrate and tailings, acidizing and roasting to obtain reburning ore, leaching the reburning ore in boiling water to obtain water leaching solution and water leaching slag, adjusting the pH value of the water leaching solution to 1.5-2.0, adding an oxalic acid precipitator to obtain rare earth compounds, and mixing the water leaching slag with an acid solution for acid leaching. The invention realizes the efficient synergistic recovery of niobium, iron and rare earth, reduces the energy consumption and the production cost, does not need harsh conditions, and is environment-friendly.

Inventors

• GUO CHUNLEI
• WANG WEIWEI
• CHEN BIAO
• JIN HAILONG
• DING YANRONG
• LI ERDOU

Assignees

• 包头稀土研究院

Dates

Publication Date

20260512

Application Date

20260130

Claims (10)

1. 1. The method for utilizing iron, rare earth and niobium elements in the easily resolvable stone type niobium concentrate is characterized by comprising the following steps of: (1) Uniformly mixing niobium concentrate with a reducing agent, pelletizing, and carrying out reduction roasting at 450-600 ℃ to obtain roasted ores; (2) Crushing the roasted ore, and then carrying out magnetic separation to obtain iron ore concentrate and tailings; (3) Uniformly mixing the tailings with sulfuric acid and an auxiliary leaching agent, and then conducting acidification roasting to obtain a reburning ore, wherein the acidification roasting temperature is 300-400 ℃; (4) Leaching the re-roasted ore in boiling water, and carrying out solid-liquid separation to obtain leaching liquid and leaching slag; (5) Adjusting the pH value of the water immersion liquid to 1.5-2.0 by adopting an adjusting agent, adding an oxalic acid precipitating agent, and carrying out solid-liquid separation to obtain a rare earth compound, wherein the adjusting agent is at least one of magnesium oxide or magnesium carbonate; And mixing the water leaching slag with an acid solution for acid leaching, and carrying out solid-liquid separation to obtain a niobium-containing acid leaching solution and acid leaching slag.
2. 2. The method of claim 1, wherein in the step (5), the amount of the oxalic acid precipitant is 1.5 to 3.5 times the amount of the rare earth oxide in the niobium concentrate, and/or, The rare earth oxide content in the rare earth compound obtained in step (5) is more than 45wt.%.
3. 3. The method of claim 1, wherein in step (5), the acid solution is a mixed acid of hydrofluoric acid and sulfuric acid, wherein the mass concentration of hydrofluoric acid in the mixed acid is 5-40 wt.% and the mass concentration of sulfuric acid in the mixed acid is 20-40 wt.%, or The acid solution is at least one of oxalic acid, tartaric acid and malic acid with the mass concentration of 20-80 wt.%.
4. 4. The method according to claim 1, wherein in the step (5), the acid leaching is performed at a temperature of 50-90 ℃ for 120-240 min.
5. 5. The method according to claim 1, wherein in the step (4), the solid-liquid mass ratio of the water immersion is 1 (2.0-8.0), and/or, The leaching time of the water leaching is 60-180 min.
6. 6. The method according to claim 1, wherein in the step (1), the mass ratio of the niobium concentrate to the reducing agent is 10 (5.0-3.0), and/or, And the heat preservation time of the reduction roasting is 60-180 min.
7. 7. The method of claim 1, wherein the magnetic field strength of the magnetic separation in step (2) is 120-300 mt.
8. 8. The method of claim 1, wherein in step (3), the leaching aid is at least one of ammonium sulfate or ammonium bisulfate, and/or, The mass concentration of the sulfuric acid is 60-98wt%, and/or, And the heat preservation time of the acidification roasting is 60-180 min.
9. 9. The method according to claim 1, characterized in that the iron concentrate has a total iron TFe content of more than 60wt.%, the recovery of rare earth is more than 85%, and the leaching rate of niobium, calculated as Nb 2 O 5 , is more than 95%.
10. 10. The method of claim 1, wherein the niobium concentrate is a low-grade, easily resolvable-stone-type niobium concentrate, wherein the easily resolvable-stone content is 1.0-35 wt.%, the hematite content is 30-70 wt.%, the Nb 2 O 5 content is 1.0-10.0 wt.%, the total iron TFe content is 26-50 wt.%, the rare earth oxide REO content is 1-10 wt.%, and the Ti content is 1.0-10 wt.%.

Description

Method for utilizing iron, rare earth and niobium elements in stone-like niobium concentrate Technical Field The invention relates to the technical field of mineral processing and hydrometallurgy, in particular to a method for utilizing iron, rare earth and niobium elements in easily-resolvable stone type niobium concentrate. Background Niobium (Nb) is an essential strategic metal for the steel, aerospace, superconducting and information industries. The total amount of niobium resources in China is large, but the niobium resources are mainly reserved in polymetallic paragenetic ores in bayan obo and other places. The stone-resolvable niobium mineral has complex components, close floatability and fine embedding granularity, and the conventional dressing and smelting technology can only obtain low-grade niobium concentrate, so that niobium resources in China face the dilemma of resource availability and difficult utilization for a long time, and the external dependency is continuously high. The separation and purification of the stone-like niobium concentrate is still in a laboratory research stage, industrial application is not realized, and the main flow technical route has obvious limitations that although the hydrofluoric acid decomposition-solvent extraction method can separate niobium, the system is extremely toxic and has strong corrosiveness and prominent hidden environmental protection trouble, and the alkali fusion-water leaching method has high energy consumption, large equipment loss and insufficient comprehensive recovery capability of associated valuable elements. Meanwhile, the existing technology has insufficient attention to the separation and recovery of iron and rare earth in niobium concentrate, few de-ironing technologies depend on high-cost means such as high-temperature reduction, protective atmosphere and the like, and efficient selective separation of iron is difficult to realize. In the aspect of rare earth recovery, the traditional method is mainly designed aiming at single rare earth ore with simple components, and when the method is directly used for treating easily-decomposed stone, the rare earth in the ore is close to the elements such as niobium, titanium, thorium and the like in a symbiotic manner, so that the dissolution of all elements and the subsequent separation are difficult, and the radioactive pollution and the environmental cost are associated. In the prior art, when the complex symbiotic structure of the easily-resolvable stone is treated, the economic and efficient synergistic comprehensive recycling of multiple elements of niobium, iron and rare earth is difficult to realize. Disclosure of Invention In view of the above analysis, the present invention aims to provide a method for utilizing iron, rare earth and niobium elements in an easily-resolvable stone type niobium concentrate, which is used for solving at least one of the problems in the prior art that the recovery of multiple elements of niobium, iron and rare earth in a low-grade easily-resolvable stone type niobium concentrate is difficult to cooperatively utilize, the process flow is complex, the energy consumption and the cost are high, the reaction conditions are harsh, the environmental pollution risk is high, and the like. The invention aims at realizing the following technical scheme: the invention provides a method for utilizing iron, rare earth and niobium elements in easily resolvable stone type niobium concentrate, which comprises the following steps: (1) Uniformly mixing niobium concentrate with a reducing agent, pelletizing, and carrying out reduction roasting at 450-600 ℃ to obtain roasted ores; (2) Crushing the roasted ore, and then carrying out magnetic separation to obtain iron ore concentrate and tailings; (3) Uniformly mixing the tailings with sulfuric acid and an auxiliary leaching agent, and then conducting acidification roasting to obtain a reburning ore, wherein the acidification roasting temperature is 300-400 ℃; (4) Leaching the re-roasted ore in boiling water, and carrying out solid-liquid separation to obtain leaching liquid and leaching slag; (5) Adjusting the pH value of the water immersion liquid to 1.5-2.0 by adopting an adjusting agent, adding an oxalic acid precipitating agent, and carrying out solid-liquid separation to obtain a rare earth compound, wherein the adjusting agent is at least one of magnesium oxide or magnesium carbonate; And mixing the water leaching slag with an acid solution for acid leaching, and carrying out solid-liquid separation to obtain a niobium-containing acid leaching solution and acid leaching slag. Further, in the step (5), the dosage of the oxalic acid precipitant is 1.5-3.5 times of the weight content of the rare earth oxide in the niobium concentrate, and/or, The rare earth oxide content in the rare earth compound obtained in step (5) is more than 45wt.%. Further, in the step (5), the acid solution is a mixed acid of hydrofluoric acid and sulf