A method for separating niobium from niobium-containing ore

By mixing the crude niobium concentrate with a vulcanizer for reduction and smelting, the niobium in the furnace slag is transformed into niobium sulfide, which solves the problems of cumbersome sorting operations and low economicality in the existing niobium smelting process, and achieves efficient separation and enrichment of niobium and slag.

CN119372492BActive Publication Date: 2025-06-06CHANGSHA RES INST OF MINING & METALLURGY CO LTD

Patent Information

Application Number
CN202411907189.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-24
Publication Date
2025-06-06
Estimated Expiration
2044-12-24

AI Technical Summary

Technical Problem

The existing niobium smelting process has problems such as easy formation of niobium carbide, complicated sorting operations, high power consumption, long production cycle and low economy.

Method used

The reduction and smelting are mixed with a niobium concentrate and a vulcanizing agent to convert the niobium in the furnace slag into a niobium sulfide, and the separation and enrichment of niobium and slag are achieved through separation from the iron sulfide.

Benefits of technology

While separating slag and iron, it can efficiently separate and enrich niobium, obtain high-grade niobium-rich products. It has simple process and strong operability, and is suitable for industrial promotion.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses a method for separating niobium from niobium-containing ore, wherein the niobium coarse concentrate is mixed with a sulfiding agent to obtain a mixture, and the mixture is subjected to reduction smelting to obtain a reduced ore, and a niobium-rich product is directly obtained from the reduced ore, or the niobium-rich product is obtained after post-processing the reduced ore. Compared with the traditional reduction smelting process, the method for separating niobium from niobium-containing ore of the present invention can achieve separation of niobium from slag while achieving separation of slag and iron, and enrich niobium to obtain a high-grade niobium-rich product, which can be purified through further metallurgical processes. The process method of the present invention has strong operability, simple process, low requirements on load-bearing smelting equipment, and is easy to promote and apply industrially.
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Description

Technical Field

[0001] The invention relates to the field of utilization of iron-associated mineral resources, and in particular to a method for separating niobium from niobium-containing ores, which can realize separation of slag iron and slag niobium. Background Art

[0002] Niobium concentrate contains many kinds of valuable metals, including Fe, Nb, REE, Mg, Ca, Na, Al and other elements, and contains more than ten kinds of niobium minerals. The composition is complex and the size of niobium ore is relatively fine. At present, the recovery and enrichment methods for niobium crude concentrate mainly include selective reduction roasting smelting process and carbon thermal chlorination roasting process. Reduction roasting smelting is the process of converting metal oxides in ore into corresponding low-valent metal oxides or metals under conditions below the melting point of the charge and reducing atmosphere. The selective reduction-smelting process is to mix niobium concentrate and reducing agent, etc., and then make balls and selectively reduce roast in the roasting furnace to obtain reduced niobium concentrate, and then smelt the reduced niobium concentrate in an electric furnace to obtain niobium phosphorus semi-steel and niobium-rich slag. The niobium-rich slag is subjected to the second step of reduction smelting to obtain niobium iron alloy. This method can obtain low-grade niobium iron containing 12~41% niobium, and the total recovery rate of niobium is greater than 80%. Chlorination roasting is a process in which a chlorinating agent is used to convert the target components in the mineral raw materials into chlorides in the gas phase or condensed phase under certain temperature and atmosphere conditions. The generated chlorides such as niobium and titanium have low boiling points and can be carried away by the gas during the chlorination process and condensed in the condensation device; while high-melting-point chlorides, such as chlorides of rare earth elements, sodium, potassium, calcium and magnesium, remain in the chlorinator to form chloride molten salts to achieve the separation of impurities.

[0003] The existing niobium smelting process has technical problems such as easy formation of niobium carbide, complicated subsequent sorting operation of the product after reduction roasting, high power consumption, long production cycle and low economy. Summary of the invention

[0004] The present invention provides a method for separating niobium from niobium-containing ore, so as to solve the technical problems mentioned in the background technology.

[0005] In order to solve the above technical problems, the technical solution proposed by the present invention is:

[0006] A method for separating niobium from a niobium-containing ore comprises mixing the niobium rough concentrate with a sulfiding agent to obtain a mixture, then reducing and smelting the mixture to obtain a reduced ore, directly obtaining a niobium-rich product from the reduced ore, or obtaining a niobium-rich product after post-processing the reduced ore; the niobium-containing ore is a niobium rough concentrate.

[0007] Taking pyrite as a sulfiding agent as an example, under reducing conditions, the sulfiding agent is added to convert the niobium in the slag into niobium-containing sulfides. The converted niobium-containing sulfides are distributed in or around the iron sulfides to achieve the separation of niobium and slag.

[0008] As a further preferred embodiment of the above technical solution, the niobium rough concentrate is a rough concentrate obtained by preselecting niobium-containing ore, wherein niobium pentoxide (Nb 2 O 5 ) content ≥1%.

[0009] As a further preferred embodiment of the above technical solution, the vulcanizing agent includes at least one of calcium sulfide, sulfur, gypsum, sulfur-containing gas and sulfur-containing minerals, and the sulfur-containing minerals include at least one of pyrrhotite and pyrite.

[0010] As a further preferred embodiment of the above technical solution, the niobium crude concentrate is first mixed with a tempering agent and a sulfiding agent to obtain a mixture, and then the mixture is reduced and smelted under the action of a reducing agent to obtain a reduced ore; the reduced ore is melted to obtain iron and niobium-rich products.

[0011] As a further preferred embodiment of the above technical solution, the reducing agent includes at least one of a solid reducing agent and a reducing gas; the reducing agent is added to the mixture, and / or the reducing agent is introduced during the reduction smelting process.

[0012] As a further preferred embodiment of the above technical solution, the mass ratio of the niobium crude concentrate, the conditioning agent and the sulfiding agent is 100: (0.1-40): (5-35); the mass ratio of the mixture to the reducing agent is 100: (2-26).

[0013] As a further preferred embodiment of the above technical solution, the temperature of the reduction smelting is 700-1250° C., and the time of the reduction smelting is greater than 20 minutes.

[0014] As a further preferred embodiment of the above technical solution, the melting temperature is 1250-1600° C., and the melting time is greater than 15 minutes.

[0015] As a further preferred embodiment of the above technical solution, the niobium crude concentrate is first mixed with a tempering agent, a sulfiding agent and a reducing agent to obtain a mixture, and then the mixture is reduced and smelted under the action of the reducing agent to obtain a reduced ore, wherein the reduced ore includes iron, niobium sulphide and iron sulfide; and the reduced ore is beneficiated to obtain a niobium-rich product.

[0016] As a further preferred embodiment of the above technical solution, the reducing agent includes at least one of a solid reducing agent and a reducing gas; the reducing agent is added to the mixture, and / or the reducing agent is introduced during the reduction smelting process.

[0017] As a further preferred embodiment of the above technical solution, the mass ratio of the niobium crude concentrate, the tempering agent, the sulfiding agent and the reducing agent in the mixture is 100: (0.1~40): (5~35): (0.1~25); the mass ratio of the mixture to the reducing agent is 100: (0.1~30).

[0018] As a further preferred embodiment of the above technical solution, the reduced ore is crushed, screened, magnetically separated and sorted to obtain a niobium-rich product.

[0019] As a further preferred embodiment of the above technical solution, the reduced ore is crushed, screened, magnetically separated, desulfurized and separated to obtain a niobium-rich product.

[0020] As a further preferred embodiment of the above technical solution, the temperature of the reduction smelting is 1250-1600° C., and the time of the reduction smelting is 10-210 min.

[0021] As a further preferred embodiment of the above technical solution, the niobium rough concentrate is a niobium-containing rare earth rough concentrate, and the niobium-containing rare earth rough concentrate is a niobium rough concentrate containing rare earth elements, wherein the niobium pentoxide content is ≥1%, and the rare earth element oxide content is ≥4%; the niobium-containing rare earth rough concentrate is first mixed with a tempering agent, a sulfiding agent, and a reducing agent to obtain a mixture, and then the mixture is reduced and smelted to obtain a reduced ore, and the reduced ore includes iron and an iron-niobium-rare earth mixture; the iron-niobium-rare earth mixture is directly obtained as a niobium-rich product, or the iron-niobium-rare earth mixture is post-processed to obtain a niobium-rich product.

[0022] As a further preferred embodiment of the above technical solution, the mass ratio of the niobium rare earth crude concentrate, the conditioning agent, the sulfiding agent and the reducing agent in the mixture is 100: (0.1-40): (6-28): (10-26).

[0023] As a further preferred embodiment of the above technical solution, the temperature of the reduction smelting is 1240-1600° C., and the time of the reduction smelting is 20-180 min.

[0024] As a further preferred embodiment of the above technical solution, the post-treatment of the iron-niobium-rare earth mixture includes the following operations: crushing, screening and magnetically separating the iron-niobium-rare earth mixture to obtain niobium-rare earth slag and iron; and then sorting the niobium-rare earth slag to obtain niobium-rich concentrate and tailings, and the niobium-rich concentrate is recovered as a niobium-rich product.

[0025] The present invention has the following beneficial effects:

[0026] Compared with the traditional reduction smelting process, the method of separating niobium from niobium-containing ore of the present invention can achieve separation of niobium from slag while achieving separation of slag and iron, and enrich niobium to obtain a high-grade niobium-rich product, which can be purified through further metallurgical procedures. The process method of the present invention has strong operability, simple process, low requirements on bearing smelting equipment, and is easy to promote and apply industrially.

[0027] The present invention will be further described in detail below with reference to specific implementation modes. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a process flow chart of Examples 1-3;

[0029] Figure 2 is a process flow chart of Examples 4-6;

[0030] Figure 3 is a SEM image of the niobium sulfide-iron sulfide-iron pearl mixture of Example 4;

[0031] Figure 4 This is a SEM image of the niobium matte-iron sulfide-iron pearl mixture of Example 5;

[0032] Figure 5 This is an EDS image of the niobium matte-iron sulfide-iron pearl mixture of Example 5;

[0033] Figure 6 This is a SEM image of the niobium matte-iron sulfide-iron pearl mixture of Example 6;

[0034] Figure 7 is a process flow chart of Example 7-8;

[0035] Figure 8 is a SEM image of the iron-sulfide mixture of Example 7;

[0036] Fig. 9 is an EDS graph of the niobium sulfide-containing material of Example 7;

[0037] Fig.10 is the XRD pattern of the niobium sulfide in Example 7;

[0038] Fig.11 is a process flow chart of Examples 9-10;

[0039] Fig.12 is a SEM image of the iron sulfide mixture of Example 9;

[0040] Fig.13 is an EDS graph of niobium sulfide of Example 9;

[0041] Fig.14 is a SEM image of the niobium-rich product 1 of Example 9;

[0042] Fig.15 This is an EDS graph of niobium oxide of niobium-rich product 1 of Example 9;

[0043] Fig.16 is a process flow chart of Examples 11-13;

[0044] Fig.17 is a process flow chart of Examples 14-16;

[0045] Fig.18 is a SEM image of the mixture containing iron, niobium and rare earth in Example 14;

[0046] Fig.19 is an EDS graph of the niobium-containing rare earth sulfide of Example 14;

[0047] Fig. 20 is the EDS graph of the rare earth sulfide-containing material of Example 14;

[0048] Fig.21 is a process flow chart of Examples 17-18;

[0049] Fig. 22 is the SEM image of iron and slag of Comparative Example 1;

[0050] Fig.23 The SEM-EDS image of iron and slag of Comparative Example 1;

[0051] Fig.24 This is a SEM image of the niobium matte-iron sulfide-iron bead mixture of Example 19. DETAILED DESCRIPTION

[0052] The embodiments of the present invention are described in detail below with reference to the accompanying drawings, but the present invention can be implemented in many different ways as defined and covered by the claims.

[0053] Embodiment 1:

[0054] like Figure 1 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium crude concentrate as raw material, recovers niobium and iron in two stages through reduction sulfidation-smelting, and includes the following steps:

[0055] (1) First, the niobium concentrate was mixed with the conditioning agent (silicon oxide and calcium oxide) and pyrite in a mass ratio of 100:12:15 to adjust the CaO / SiO 2 The mass ratio is 0.4, and the mixture is mixed evenly to obtain a mixture (which is used in the next step in the form of powder);

[0056] (2) placing the mixed material from step (1) and coke in a mass ratio of 100:12 into a furnace, performing reduction smelting under an argon atmosphere at a temperature of 1100° C. for 30 minutes to obtain a reduced ore;

[0057] (3) discharging the reduced ore into a smelting furnace and smelting the ore under an argon atmosphere, heating the ore to 1500° C. and maintaining the temperature for 30 minutes to separate the slag from the iron and niobium-rich products, thereby obtaining iron, the first niobium-rich product and slag;

[0058] (4) The first niobium-rich product of step (3) is ground and then sent to a magnetic separation process. After magnetic separation, niobium sulfide is separated from iron and ferrous sulfide to obtain a second niobium-rich product. According to conventional methods, the recovery rate of niobium in the first niobium-rich product is 78.23%, and the mass proportion of niobium in niobium sulfide is 45.55%.

[0059] Embodiment 2:

[0060] like Figure 1 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium crude concentrate as raw material, recovers niobium and iron in two stages through reduction sulfidation-smelting, and includes the following steps:

[0061] (1) First, the niobium concentrate was mixed with the conditioning agent (silicon oxide and calcium oxide) and pyrite in a mass ratio of 100:10:15 to adjust the CaO / SiO 2 The mass ratio is 0.35, and the mixture is uniformly mixed to obtain a mixture (which is used in the next step in the form of powder);

[0062] (2) placing the mixed material from step (1) and coke in a mass ratio of 100:16 into a furnace, performing reduction smelting under an argon atmosphere at a temperature of 1100° C. for 30 minutes to obtain a reduced ore;

[0063] (3) discharging the reduced ore into a smelting furnace and smelting the ore under an argon atmosphere, heating the ore to 1550° C. and maintaining the temperature for 30 minutes to separate the slag from the iron and niobium-rich products, thereby obtaining iron, the first niobium-rich product and slag;

[0064] (4) The first niobium-rich product of step (3) is ground and then sent to a magnetic separation process. After magnetic separation, niobium sulfide is separated from iron and ferrous sulfide to obtain a second niobium-rich product. According to conventional methods, the recovery rate of niobium in the first niobium-rich product is 83.61%, and the mass proportion of niobium in niobium sulfide is 46.18%.

[0065] Embodiment 3:

[0066] like Figure 1 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium crude concentrate as raw material, recovers niobium and iron in two stages through reduction sulfidation-smelting, and includes the following steps:

[0067] (1) First, the niobium concentrate was mixed with the conditioning agent (silicon oxide and calcium oxide) and pyrite in a mass ratio of 100:10:23 to adjust the CaO / SiO 2 The mass ratio is 0.35, and the mixture is uniformly mixed to obtain a mixture (which is used in the next step in the form of powder);

[0068] (2) placing the mixed material from step (1) and coke in a mass ratio of 100:20 into a furnace, and performing reduction smelting under an argon atmosphere at a temperature of 1200° C. for 30 minutes to obtain a reduced ore;

[0069] (3) discharging the reduced ore into a smelting furnace and smelting the ore under an argon atmosphere, heating the ore to 1500° C. and maintaining the temperature for 30 minutes to separate the slag from the iron and niobium-rich products, thereby obtaining iron, the first niobium-rich product and slag;

[0070] (4) The first niobium-rich product of step (3) is ground and then sent to a magnetic separation process. After magnetic separation, niobium sulfide is separated from iron and ferrous sulfide to obtain a second niobium-rich product. According to conventional methods, the recovery rate of niobium in the first niobium-rich product is 93.3%, and the mass proportion of niobium in niobium sulfide is 46.38%.

[0071] Embodiment 4:

[0072] like Figure 2 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0073] (1) Niobium concentrate (Nb 2 O 5 The mass ratio is 1.2%, TiO 2 The mass proportion is 3.2%, the mass proportion of rare earth oxide (REO) is 1.9%, the mass proportion of CaO is 7.82%, and the mass proportion of SiO 2 The mass proportion is 32.82%, the mass proportion of MgO is 4.8%, and the mass proportion of Al 2 O 3 The mass percentage is 1.9%) for screening and drying;

[0074] (2) The niobium concentrate obtained in step (1) is mixed evenly with a conditioning agent (silicon oxide, calcium oxide), pyrite, and coke in a mass ratio of 100:10:15:8, and the CaO / SiO 2 The mass ratio is controlled to be 0.4, and the mixture is mixed evenly to obtain a mixture;

[0075] (3) placing reducing agent coke at the bottom of the smelting furnace, and then placing the mixture in step (2) (the mass ratio of the mixture to coke is 100:10) for heating and reduction smelting, the reduction smelting temperature is 1500° C., the smelting time is 20 minutes, and iron and niobium matte-iron sulfide-pellet iron mixture and slag are obtained;

[0076] (4) After the niobium matte-iron sulfide-iron pearl mixture in step (3) is cooled to room temperature, it is used for testing and analysis. The SEM results are as follows: Figure 3As shown. EDS-SEM determined that the elements contained in the niobium sulfide include niobium, sulfur and iron. The phosphorus content in the pearl iron obtained in this embodiment was detected by conventional methods to be 2.65%, the direct recovery rate of niobium content in the niobium matte-iron sulfide-pearl iron mixture reached 55.2%, and the direct recovery rate of iron reached 83%.

[0077] Embodiment 5:

[0078] like Figure 2 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0079] (1) Niobium concentrate (Nb 2 O 5 The mass ratio is 5.28%, TiO 2 The mass proportion is 9.687%, the mass proportion of rare earth oxide (REO) is 3.77%, the mass proportion of CaO is 6.74%, and the mass proportion of SiO 2 The mass proportion is 22.51%, the mass proportion of MgO is 8.68%, and the mass proportion of Al 2 O 3 The mass percentage is 1.36%) for screening and drying;

[0080] (2) The niobium concentrate obtained in step (1) is mixed evenly with a conditioning agent (silicon oxide, calcium oxide), pyrite, and coke in a mass ratio of 100:3:20:8, and the CaO / SiO 2 The mass ratio is controlled to be 0.4, and the mixture is mixed evenly to obtain a mixture;

[0081] (3) placing coke as a reducing agent at the bottom of a smelting furnace, and then placing the mixture in step (2) (the mass ratio of the mixture to coke is 100:12) for heating and reduction smelting, the reduction smelting temperature is 1460° C., the smelting time is 60 minutes, and iron and a niobium matte-iron sulfide-pellet iron mixture and slag are obtained;

[0082] (4) After the niobium matte-iron sulfide-iron pearl mixture in step (3) is cooled to room temperature, it is used for testing and analysis. The SEM results are as follows: Figure 4 As shown. Figure 5 As shown, the elements contained in the niobium sulfide include niobium, sulfur and iron as determined by EDS-SEM. The phosphorus content in the pearl iron obtained in this embodiment is 2.06% by conventional methods, the direct recovery rate of niobium content in the niobium matte-iron sulfide-pearl iron mixture reaches 73.6%, and the direct recovery rate of iron reaches 85.5%.

[0083] Embodiment 6:

[0084] like Figure 2 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0085] (1) Niobium concentrate (Nb 2 O 5 The mass ratio is 5.28%, TiO 2 The mass proportion is 9.687%, the mass proportion of rare earth oxide (REO) is 3.77%, the mass proportion of CaO is 6.74%, and the mass proportion of SiO 2 The mass proportion is 22.51%, the mass proportion of MgO is 8.68%, and the mass proportion of Al 2 O 3 The mass percentage is 1.36%) for screening and drying;

[0086] (2) The niobium concentrate obtained in step (1) is mixed evenly with a conditioning agent (silicon oxide, calcium oxide), pyrite, and coke in a mass ratio of 100:3:20:8, and the CaO / SiO 2 The mass ratio is controlled to be 0.3, and the mixture is mixed evenly to obtain a mixture;

[0087] (3) placing coke as a reducing agent at the bottom of a smelting furnace, and then placing the mixture in step (2) (the mass ratio of the mixture to coke is 100:14) for temperature-raising reduction smelting, the reduction smelting temperature is 1450° C., the smelting time is 90 minutes, and iron and a niobium matte-iron sulfide-pellet iron mixture and slag are obtained;

[0088] (4) After the niobium matte-iron sulfide-iron pearl mixture in step (3) is cooled to room temperature, it is used for testing and analysis. The SEM results are as follows: Figure 6 The phosphorus content of the pearl iron obtained in this embodiment is 8.8% by conventional method, the direct recovery rate of niobium content in the mixture of niobium matte-iron sulfide-pearl iron is 89.4%, and the direct recovery rate of iron is 92.2%.

[0089] Comparative Example 1:

[0090] The method for separating niobium from niobium-containing ore in this comparative example uses niobium crude concentrate as raw material, and comprises the following steps:

[0091] (1) Niobium concentrate (Nb 2 O 5 The mass ratio is 5.28%, TiO 2 The mass proportion is 9.687%, the mass proportion of rare earth oxide (REO) is 3.77%, the mass proportion of CaO is 6.74%, and the mass proportion of SiO 2 The mass proportion is 22.51%, the mass proportion of MgO is 8.68%, and the mass proportion of Al 2 O 3 The mass percentage is 1.36%) for screening and drying;

[0092] (2) The niobium concentrate obtained in step (1) is mixed evenly with coke in a mass ratio of 100:8, CaO / SiO 2 The mass ratio is controlled to be 0.3, and the mixture is mixed evenly to obtain a mixture;

[0093] (3) placing coke as a reducing agent at the bottom of a smelting furnace, and then placing the mixture in step (2) (the mass ratio of the mixture to coke is 100:14) for heating and reduction smelting, the reduction smelting temperature is 1450° C., the smelting time is 90 minutes, and iron and slag are obtained;

[0094] (4) After the iron and slag in step (3) are cooled to room temperature, they are used for testing and analysis. The SEM and SEM-EDS results are as follows: Fig. 22 and Fig.23 The analysis shows that the niobium-containing phase is mixed with the iron phase. According to the SEM-EDS spectrum, it is confirmed that there is no sulfur element in the niobium-containing phase, and the main elements are niobium, titanium and carbon.

[0095] Embodiment 7:

[0096] like Figure 7 The method for separating niobium from niobium-containing ore of this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0097] (1) First, in the niobium rough concentrate (Nb 2 O 5 Calcium oxide, silicon dioxide, pyrite and coke are added to niobium ore (grade is 6.7%), the total mass of calcium oxide and silicon dioxide is 5% of the mass of niobium rough concentrate, the mass ratio of calcium oxide / silicon dioxide is controlled to be 0.45, the amount of coke added is 15% of the mass of niobium rough concentrate, and the amount of pyrite added is 20% of the mass of niobium rough concentrate: heating reduction smelting is carried out in argon atmosphere, and the temperature is raised to 1450°C and then kept for 80 minutes; an iron-sulfide mixture and slag are obtained;

[0098] (2) crushing and screening the iron-sulfide mixture obtained in step (1) to obtain fine particles of 18-75 μm;

[0099] (3) subjecting the fine particles of step (2) to magnetic separation to separate iron and sulfide to obtain niobium-containing sulfide;

[0100] (4) Finally, the niobium sulfide is subjected to magnetic separation to obtain niobium-rich products and iron-rich products with higher niobium grades.

[0101] After testing, the SEM results of the iron-sulfide mixture obtained in step (2) are as follows: Figure 8 As shown, the EDS of niobium sulfide obtained in step (3) is as follows Fig. 9 As shown, the XRD pattern of niobium sulfide obtained in step (4) is Fig.10As shown; the mass proportion of iron in iron sulfide is 57.94%, the mass proportion of niobium in niobium sulfide is 45.31%, and the mass proportion of iron in niobium sulfide is 16.27%.

[0102] Embodiment 8:

[0103] like Figure 7 The method for separating niobium from niobium-containing ore of this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0104] (1) First, in the niobium rough concentrate (Nb 2 O 5 Calcium oxide, silicon dioxide, pyrite and coke are added to niobium crude concentrate (with a grade of 3.5%), the total mass of calcium oxide and silicon dioxide is 0.5% of the mass of the niobium crude concentrate, the mass ratio of calcium oxide to silicon dioxide is controlled to be 0.45, the amount of coke added is 15% of the mass of the niobium crude concentrate, the amount of pyrite added is 20% of the mass of the niobium crude concentrate, and the temperature is increased under an argon atmosphere for reduction smelting, and the temperature is increased to 1550°C and then kept for 60 minutes; an iron-sulfide mixture and slag are obtained;

[0105] (2) crushing and screening the iron-sulfide mixture obtained in step (1) to obtain fine particles of 18-75 μm;

[0106] (3) subjecting the fine particles of step (2) to magnetic separation to separate iron and sulfide to obtain niobium-containing sulfide;

[0107] (4) Finally, the niobium sulfide is subjected to magnetic separation to obtain niobium-rich products and iron-rich products with higher niobium grades.

[0108] After testing, it was found that the iron content of iron sulfide was 58.90% by weight, the niobium content of niobium sulfide was 45.45% by weight, and the iron content of niobium sulfide was 14.22% by weight.

[0109] Embodiment 9:

[0110] like Fig.11 The method for separating niobium from niobium-containing ore of this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0111] (1) Nb 2 O 5 Calcium oxide, silicon oxide, pyrite and coke were added to the 3.1% niobium concentrate, the total mass of calcium oxide and silicon dioxide was 7% of the mass of the niobium concentrate, the mass ratio of calcium oxide to silicon dioxide was controlled to be 0.38, the amount of coke added was 18% of the mass of the niobium concentrate, the amount of pyrite added was 22.5% of the mass of the niobium concentrate, and reduction sulfidation smelting was carried out in an argon atmosphere at a smelting temperature of 1450°C and a smelting time of 60 minutes to obtain an iron-sulfide mixture and slag, wherein the SEM results of the iron-sulfide mixture are as follows: Fig.12As shown;

[0112] (2) crushing and screening the iron-sulfide mixture obtained in step (1) to obtain fine particles with a particle size of less than 150 μm;

[0113] (3) The fine particles obtained in step (2) are subjected to magnetic separation at an intensity of 0.05T to separate iron and sulfide to obtain niobium sulfide and iron sulfide. The EDS results of niobium sulfide are as follows: Fig.13 As shown; Electron probe microanalysis (EPMA) showed that the mass proportion of iron in iron sulfide is 49.89%, and the mass proportion of niobium in niobium sulfide is 45.6%;

[0114] (4) The niobium-containing sulfide obtained in step (3) is roasted and desulfurized in an oxygen-containing environment. After desulfurization, the niobium-rich product 1 is obtained by magnetic separation at a magnetic field strength of 0.08 T. The SEM result of the niobium-rich product 1 is as follows: Fig.14 As shown in Figure 1, the main components are niobium oxide and a small amount of iron oxide. The EDS results of niobium oxide are shown in Figure 1. Fig.15 As shown, the main components are iron, oxygen and niobium. Electron probe microanalysis (EPMA) shows that the mass proportion of niobium pentoxide in niobium oxide is 72.2%.

[0115] This embodiment can obtain Nb 2 O 5 The recovery rate of the original ore is 40.56%, and the mixed product mainly composed of niobium oxide is 57.2%, which means that the niobium resources have been well recovered.

[0116] Embodiment 10:

[0117] like Fig.11 The method for separating niobium from niobium-containing ore of this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0118] (1) Nb 2 O 5 Calcium oxide, silicon oxide, pyrite and coke are added to the niobium rough concentrate with a grade of 3.1%, the total mass of calcium oxide and silicon dioxide is 7% of the mass of the niobium rough concentrate, the mass ratio of calcium oxide to silicon dioxide is controlled to be 0.38, the amount of coke added is 18% of the mass of the niobium rough concentrate, the amount of pyrite added is 22.5% of the mass of the niobium rough concentrate, reduction sulfidation smelting is carried out in an argon atmosphere, the smelting temperature is 1500°C, the smelting time is 90 minutes, and an iron-sulfide mixture and slag are obtained;

[0119] (2) crushing and screening the iron-sulfide mixture obtained in step (1) to obtain fine particles with a particle size of less than 150 μm;

[0120] (3) The fine particles obtained in step (2) are subjected to magnetic separation at an intensity of 0.25 T to separate iron and sulfide to obtain niobium-containing sulfide and iron sulfide; electron probe microanalysis (EPMA) shows that the mass proportion of iron in the iron sulfide is 48.1%, and the mass proportion of niobium in the niobium sulfide is 46.26%;

[0121] (4) The niobium-containing sulfide obtained in step (3) is roasted and desulfurized in an oxygen-containing environment. After desulfurization, it is subjected to magnetic separation at a magnetic field strength of 0.05 T to obtain a niobium-rich product 1, which is mainly composed of niobium oxide and a small amount of iron oxide. The main components of niobium oxide are iron, oxygen and niobium. Electron probe microanalysis (EPMA) shows that the mass proportion of niobium pentoxide in niobium oxide is 73.66%.

[0122] This embodiment can obtain Nb 2 O 5 The recovery rate of the original ore is 44.1%, and the mixed product mainly composed of niobium oxide is 50.78%, which means that the niobium resources have been well recovered.

[0123] Embodiment 11:

[0124] like Fig.16 The method for separating niobium from niobium-containing ore of this embodiment uses niobium-containing rare earth crude concentrate as raw material, and comprises the following steps:

[0125] (1) First, the niobium-containing rare earth concentrate is mixed with calcium oxide, silicon oxide, pyrite and coke to obtain a mixture. The total mass of calcium oxide and silicon dioxide is 4% of the mass of the niobium concentrate. The CaO / SiO ratio is adjusted. 2 The mass ratio is 0.4, the mass proportion of pyrite in the mixture is 18%, and the mass proportion of coke is 18%;

[0126] (2) heating the mixed material in step (1) to 1400° C. in an argon atmosphere for reduction smelting (i.e., mineral phase reconstruction) in the form of powder, and keeping the temperature for 90 minutes to obtain a reduced ore;

[0127] (3) crushing the reduced ore in step (2), and magnetically separating the fine particles obtained after crushing to obtain niobium-containing rare earth slag and iron. The niobium-containing rare earth slag contains iron sulfide, niobium sulfide, and rare earth-niobium sulfide. The total weight ratio of iron and sulfur in the iron sulfide is 88.4%, the weight ratio of niobium and sulfur in the niobium sulfide is 82.5%, and the weight ratio of niobium, rare earth and sulfur in the rare earth-niobium sulfide is 91.5%;

[0128] (4) flotating the sulfide-containing slag in step (3) to obtain niobium-rich concentrate and tailings.

[0129] After being processed by the method of this embodiment, for Nb 2 O5 The niobium-containing rare earth crude concentrate with a grade of 4.8% and a rare earth element (including lanthanum, cerium, and neodymium) content of 4.09% can produce a niobium-rich concentrate with a Nb grade of 11.5% and a rare earth element grade of 9.5%. The niobium recovery rate is 58.8% and the rare earth element recovery rate is 52%.

[0130] Embodiment 12:

[0131] like Fig.16 The method for separating niobium from niobium-containing ore of this embodiment uses niobium-containing rare earth crude concentrate as raw material, and comprises the following steps:

[0132] (1) First, the niobium-containing rare earth concentrate is mixed with calcium oxide, silicon oxide, pyrite and coke to obtain a mixture. The total mass of calcium oxide and silicon dioxide is 4% of the mass of the niobium concentrate. The CaO / SiO ratio is adjusted. 2 The mass ratio is 0.4, the mass proportion of pyrite in the mixture is 22%, and the mass proportion of coke is 20%;

[0133] (2) heating the mixed material in step (1) to 1450° C. in an argon atmosphere in the form of powder for reduction smelting (i.e., mineral phase reconstruction), and keeping the temperature for 120 minutes to obtain a reduced ore;

[0134] (3) crushing the reduced ore in step (2), and magnetically separating the fine particles obtained after crushing to obtain niobium-containing rare earth slag and iron. The niobium-containing rare earth slag is tested to contain iron sulfide, niobium sulfide, and rare earth-niobium sulfide. The total weight ratio of iron and sulfur in the iron sulfide is 85.5%, the weight ratio of niobium and sulfur in the niobium sulfide is 84.4%, and the weight ratio of niobium, rare earth and sulfur in the rare earth-niobium sulfide is 92.8%;

[0135] (4) flotating the sulfide-containing slag in step (3) to obtain niobium-rich concentrate and tailings.

[0136] After being processed by the method of this embodiment, Nb 2 O 5 The niobium-containing rare earth crude concentrate with a grade of 4.8% and a rare earth element (including lanthanum, cerium, and neodymium) content of 4.09% can obtain niobium-rich concentrate with a Nb grade of 16% and a rare earth element grade of 11.2%. The niobium recovery rate is 43.5% and the rare earth element recovery rate is 47.1%.

[0137] Embodiment 13:

[0138] like Fig.16 As shown, the method for separating niobium from niobium-containing ore in this embodiment uses niobium-containing rare earth crude concentrate as raw material, and comprises the following steps:

[0139] (1) First, the niobium-containing rare earth concentrate is mixed with calcium oxide, silicon oxide, pyrite and coke to obtain a mixture. The total mass of calcium oxide and silicon dioxide is 4% of the mass of the niobium concentrate. The CaO / SiO ratio is adjusted. 2 The mass ratio is 0.4, the mass proportion of pyrite in the mixture is 24%, and the mass proportion of coke is 21%;

[0140] (2) heating the mixed material in step (1) to 1350° C. in an argon atmosphere in the form of powder for reduction smelting (i.e., mineral phase reconstruction), and keeping the temperature for 60 minutes to obtain a reduced ore;

[0141] (3) crushing the reduced ore in step (2), and magnetically separating the fine particles obtained after crushing to obtain niobium-containing rare earth slag and iron. The niobium-containing rare earth slag is tested to contain iron sulfide, niobium sulfide, and rare earth-niobium sulfide. The total weight ratio of iron and sulfur in the iron sulfide is 85.5%, the weight ratio of niobium and sulfur in the niobium sulfide is 86.3%, and the weight ratio of niobium, rare earth and sulfur in the rare earth-niobium sulfide is 90.3%;

[0142] (4) flotating the sulfide-containing slag in step (3) to obtain niobium-rich concentrate and tailings.

[0143] After being processed by the method of this embodiment, Nb 2 O 5 The niobium-containing rare earth crude concentrate raw material with a grade of 4.8% and a rare earth element (including lanthanum, cerium, and neodymium) content of 4.09% can obtain niobium-rich concentrate with a Nb grade of 13.3% and a rare earth element grade of 10.7%. The niobium recovery rate is 47.8% and the rare earth element recovery rate is 49.4%.

[0144] Embodiment 14:

[0145] like Fig.17 The method for separating niobium from niobium-containing ore of this embodiment uses niobium-containing rare earth crude concentrate as raw material, and comprises the following steps:

[0146] (1) Dry niobium rare earth concentrate (Nb 2 O 5 The content accounts for 3.9%, TiO 2 The content accounts for 5.15%, CeO 2 The content accounts for 2.74%, La 2 O 3 The content accounts for 1.14%, Nd 2 O 3 The content accounts for 0.88%, Pr 6 O 11 The content accounts for 0.16%, Fe 2 O 3The content accounts for 27.13%, CaO content accounts for 14.14%, SiO 2 The content accounts for 20.27%, MgO content accounts for 11.28%, Al 2 O 3 Silicon dioxide, pyrite and coke are added to the niobium concentrate (the content accounts for 2.34%), the total mass of silicon dioxide is 1.5% of the mass of niobium rough concentrate, and the mass ratio of niobium rare earth rough concentrate to pyrite and coke is 100:9:20; the mixed material is directly used in the next step as a powder after being evenly mixed;

[0147] (2) The mixed material obtained in step (1) is subjected to reduction sulfidation smelting in an argon atmosphere at a reduction smelting temperature of 1480°C for 90 minutes. After cooling, the mixed material is crushed to obtain a mixture containing iron, niobium and rare earth and slag. The SEM results of the mixture containing iron, niobium and rare earth are as follows: Fig.18 As shown, the mixture includes iron, iron sulfide, niobium-containing rare earth sulfide, and rare earth sulfide; the EDS spectrum of niobium-containing rare earth sulfide is as shown Fig.19 As shown in Figure 1, the main components include niobium, lanthanum, cerium, praseodymium, neodymium, and sulfur. The conventional method detected that the mass proportion of niobium, lanthanum, cerium, praseodymium, neodymium, and sulfur is 85.1%; the EDS spectrum containing rare earth sulfides is shown in Figure 1. Fig. 20 As shown, the main component elements include lanthanum, cerium, praseodymium, neodymium and sulfur. The conventional method detects that the element mass proportion of niobium, lanthanum, cerium, praseodymium, neodymium and sulfur is 77.3%. The conventional method detects that the niobium enrichment rate in the mixture containing iron, niobium and rare earth is 53.5%, and the rare earth enrichment rate in the mixture containing iron, niobium and rare earth is 47.7%.

[0148] Embodiment 15:

[0149] like Fig.17 The method for separating niobium from niobium-containing ore of this embodiment uses niobium-containing rare earth crude concentrate as raw material, and comprises the following steps:

[0150] (1) Dry niobium rare earth concentrate (Nb 2 O 5 The content accounts for 3.9%, TiO 2 The content accounts for 5.15%, CeO 2 The content accounts for 2.74%, La 2 O 3 The content accounts for 1.14%, Nd 2 O 3 The content accounts for 0.88%, Pr 6 O 11 The content accounts for 0.16%, Fe 2 O 3 The content accounts for 27.13%, CaO content accounts for 14.14%, SiO2 The content accounts for 20.27%, MgO content accounts for 11.28%, Al 2 O 3 Silicon dioxide, pyrite and coke are added to the niobium concentrate (the content accounts for 2.34%), the total mass of silicon dioxide is 3.3% of the mass of niobium rough concentrate, and the mass ratio of niobium rare earth rough concentrate to pyrite and coke is 100:16:20; the mixed material is directly used in the next step as a powder after being evenly mixed;

[0151] (2) The mixture obtained in step (1) is subjected to reduction sulfidation smelting under an argon atmosphere, the reduction smelting temperature is 1550°C, the smelting time is 90 minutes, and the mixture is crushed after cooling to obtain a mixture containing iron, niobium and rare earth and slag. The mass proportion of niobium, lanthanum, cerium, praseodymium, neodymium and sulfur in the niobium-containing rare earth sulfide is 92.1% by conventional method, and the mass proportion of lanthanum, cerium, praseodymium, neodymium and sulfur in the rare earth sulfide is 88.3% by conventional method; the niobium enrichment rate in the iron, niobium and rare earth mixture is 71.4%, and the rare earth enrichment rate in the iron, niobium and rare earth mixture is 58.2%.

[0152] Embodiment 16:

[0153] like Fig.17 The method for separating niobium from niobium-containing ore of this embodiment uses niobium-containing rare earth crude concentrate as raw material, and comprises the following steps:

[0154] (1) Dry niobium rare earth concentrate (Nb 2 O 5 The content accounts for 7.7%, TiO 2 The content accounts for 10.21%, CeO 2 The content accounts for 3.56%, La 2 O 3 The content accounts for 1.5%, Nd 2 O 3 The content accounts for 1.33%, Pr 6 O 11 The content accounts for 0.45%, Fe 2 O 3 The content accounts for 25.68%, CaO content accounts for 9.45%, SiO 2 The content accounts for 24.28%, MgO content accounts for 5.79%, Al 2 O 3 Calcium oxide, silicon oxide, pyrite and coke are added to the niobium concentrate (1.55%), and the total mass of calcium oxide and silicon dioxide is 6.2% of the mass of the niobium concentrate. 2The mass ratio is controlled at 0.6, and the mass ratio of the niobium rare earth crude concentrate to pyrite and coke is 100:22:24; the mixed material is directly applied to the next step as a powder;

[0155] (2) The mixture obtained in step (1) is subjected to reduction sulfidation smelting in an argon atmosphere, the reduction smelting temperature is 1500°C, the smelting time is 60 minutes, and after cooling, it is crushed to obtain a mixture containing iron, niobium and rare earth and slag. The mass proportion of niobium, lanthanum, cerium, praseodymium, neodymium and sulfur in the niobium-containing rare earth sulfide is 89.9% by conventional method, and the mass proportion of lanthanum, cerium, praseodymium, neodymium and sulfur in the rare earth sulfide is 85.5% by conventional method; the niobium enrichment rate in the iron, niobium and rare earth mixture is 0.827, and the rare earth enrichment rate in the iron, niobium and rare earth mixture is 0.633.

[0156] Embodiment 17:

[0157] like Fig.21 The method for separating niobium from niobium-containing ore of this embodiment uses niobium rough concentrate as raw material, and its mineral composition is shown in Table 1, and comprises the following steps:

[0158] (1) Mix the niobium concentrate with calcium oxide, silicon oxide and pyrite. The total mass of calcium oxide and silicon dioxide is 7% of the mass of the niobium concentrate. Adjust the CaO / SiO ratio in the raw materials. 2 The mass ratio of niobium crude concentrate to pyrite is 0.4, the mass ratio of niobium crude concentrate to pyrite is 100:15, and the mixed material is used in the next smelting process as powder after being evenly mixed;

[0159] (2) The mixed material obtained in step (1) is introduced into carbon monoxide gas under an argon atmosphere for temperature reduction smelting. After the reaction is completed, the introduction of reducing gas is stopped. The smelting temperature is 1450° C. and the smelting time is 180 minutes. After the smelting is completed and cooled, iron, niobium-rich products and slag are obtained. Detection and analysis by conventional methods show that the niobium-rich product mainly contains iron, niobium, sulfur, phosphorus and manganese elements.

[0160] After being processed by the method for separating niobium in this embodiment, Nb 2 O 5 The niobium crude concentrate with a grade of 3.43% can produce a niobium-rich product with a separation rate of 77.2%, and the niobium resources are well separated and recovered.

[0161] Embodiment 18:

[0162] like Fig.21 The method for separating niobium from niobium-containing ore in this embodiment uses niobium rough concentrate as raw material (consistent with Example 17), and comprises the following steps:

[0163] (1) Mix the niobium concentrate with calcium oxide, silicon oxide and pyrite. The total mass of calcium oxide and silicon dioxide is 7% of the mass of the niobium concentrate. Adjust the CaO / SiO ratio in the raw materials. 2 The mass ratio of niobium crude concentrate to pyrite is 0.4, the mass ratio of niobium crude concentrate to pyrite is 100:24, and the mixed material is used in the next step of smelting in the form of powder after being evenly mixed;

[0164] (2) The mixture obtained in step (1) is introduced into carbon monoxide gas under an argon atmosphere for temperature reduction smelting. After the reaction is completed, the introduction of reducing gas is stopped. The smelting temperature is 1450° C. and the smelting time is 180 minutes. After the smelting is completed and cooled, iron, niobium-rich products and slag are obtained. According to conventional detection and analysis, the niobium-rich product mainly contains iron, niobium, sulfur, phosphorus and manganese elements.

[0165] After being processed by the method for separating niobium in this embodiment, Nb 2 O 5 The niobium crude concentrate with a grade of 3.43% can produce a niobium-rich product with a separation rate of 90.67%, and the niobium resources are well separated and recovered.

[0166] Table 1 Mineral composition of niobium rough concentrate

[0167]

[0168] Embodiment 19:

[0169] The method for separating niobium from niobium-containing ore in this embodiment uses niobium rough concentrate as raw material, and comprises the following steps:

[0170] (1) Niobium concentrate (Nb 2 O 5 The mass ratio is 2.31%, TiO 2 The mass proportion is 4.80%, CaO accounts for 10.36%, SiO 2 The mass proportion is 24.88%, the mass proportion of MgO is 8.27%, and the mass proportion of Al 2 O 3 The mass proportion is 3.02%, Fe 2 O 3 The mass ratio is 24.57%, Na 2 O accounts for 2.72% of the mass, K 2 O accounts for 1.71% by mass, and F accounts for 1.09% by mass) for sieving and drying;

[0171] (2) mixing the niobium concentrate obtained in step (1) with pyrite and coke in a mass ratio of 100:20:1 to obtain a mixture;

[0172] (3) placing coke as a reducing agent at the bottom of a smelting furnace, and then placing the mixture in step (2) (the mass ratio of the mixture to coke is 100:19) for heating and reduction smelting, the reduction smelting temperature is 1450° C., the smelting time is 90 minutes, and iron and a niobium matte-iron sulfide-pellet iron mixture and slag are obtained;

[0173] (4) After the niobium matte-iron sulfide-iron pearl mixture in step (3) is cooled to room temperature, it is used for testing and analysis. The SEM results are as follows: Fig.24 The conventional method was used to detect the niobium content in the niobium sulfide-iron sulfide-iron mixture obtained in this embodiment, and the direct recovery rate of niobium reached 77.5%, and the direct recovery rate of iron reached 89.9%.

[0174] The above are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited to the above embodiments. For those skilled in the art, improvements and changes obtained without departing from the technical concept of the present invention should also be regarded as the protection scope of the present invention.

[0175] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.

Claims

1. A method for separating niobium from a niobium-containing ore, characterized in that: Firstly, a niobium rough concentrate is mixed with a conditioning agent and a sulfiding agent to obtain a mixture, and then the mixture is subjected to reduction smelting under the action of a reducing agent to obtain a reduced ore. During the reduction smelting process, niobium in the slag is converted into niobium-containing sulfide, so that niobium and slag are separated and niobium is enriched, and a niobium-rich product is directly obtained from the reduced ore, or the niobium-rich product is obtained after post-processing the reduced ore; the niobium-containing ore is a niobium rough concentrate, which is a rough concentrate obtained by pre-selecting a niobium-containing ore, wherein the niobium pentoxide content is ≥1%; the sulfiding agent includes at least one of calcium sulfide, sulfur, gypsum, sulfur-containing gas and sulfur-containing minerals, and the sulfur-containing minerals include at least one of pyrrhotite and pyrite; the conditioning agent is calcium oxide and / or silicon dioxide.

2. The method for separating niobium from niobium-containing ore according to claim 1, characterized in that: The niobium crude concentrate is first mixed with a conditioning agent and a sulfiding agent to obtain a mixture, and then the mixture is reduced and smelted under the action of a reducing agent to obtain a reduced ore; the reduced ore is melted to obtain iron and niobium-rich products.

3. The method for separating niobium from niobium-containing ore according to claim 2, characterized in that: The reducing agent includes at least one of a solid reducing agent and a reducing gas; the reducing agent is added to the mixed material, and / or the reducing agent is introduced during the reduction smelting process.

4. The method for separating niobium from niobium-containing ore according to claim 2, characterized in that: The mass ratio of the niobium crude concentrate, the conditioning agent and the sulfiding agent is 100: (0.1-40): (5-35); the mass ratio of the mixture to the reducing agent is 100: (2-26).

5. The method for separating niobium from niobium-containing ore according to claim 2, characterized in that: The reduction smelting temperature is 700-1250° C., and the reduction smelting time is greater than 20 minutes.

6. The method for separating niobium from niobium-containing ore according to claim 2, characterized in that: The melting temperature is 1250-1600° C., and the melting time is greater than 15 minutes.

7. The method for separating niobium from niobium-containing ore according to claim 1, characterized in that: The niobium crude concentrate is first mixed with a conditioning agent, a sulfiding agent and a reducing agent to obtain a mixture, and then the mixture is subjected to reduction smelting under the action of the reducing agent to obtain a reduced ore, wherein the reduced ore includes iron, niobium sulphide and iron sulfide; and the reduced ore is subjected to ore dressing to obtain a niobium-rich product.

8. The method for separating niobium from niobium-containing ore according to claim 7, characterized in that: The mass ratio of the niobium crude concentrate, the conditioning agent, the sulfiding agent and the reducing agent in the mixture is 100: (0.1-40): (5-35): (0.1-25); the mass ratio of the mixture to the reducing agent is 100: (0.1-30).

9. The method for separating niobium from niobium-containing ore according to claim 7, characterized in that: The reduced ore is crushed, screened, magnetically separated and sorted to obtain a niobium-rich product.

10. The method for separating niobium from niobium-containing ore according to claim 9, characterized in that: The reduced ore is crushed, screened, magnetically separated, desulfurized and separated to obtain a niobium-rich product.

11. The method for separating niobium from niobium-containing ore according to claim 7, characterized in that: The reduction smelting temperature is 1250-1600° C., and the reduction smelting time is 10-210 min.

12. The method for separating niobium from niobium-containing ore according to claim 1, characterized in that: The niobium rough concentrate is a niobium-containing rare earth rough concentrate, and the niobium-containing rare earth rough concentrate is a niobium rough concentrate containing rare earth elements, wherein the niobium pentoxide content is ≥1%, and the rare earth element oxide content is ≥4%; the niobium-containing rare earth rough concentrate is first mixed with a tempering agent, a sulfiding agent, and a reducing agent to obtain a mixture, and then the mixture is reduced and smelted to obtain a reduced ore, and the reduced ore includes iron and an iron-niobium-rare earth mixture; the iron-niobium-rare earth mixture is directly obtained as a niobium-rich product, or the iron-niobium-rare earth mixture is post-processed to obtain a niobium-rich product.

13. The method for separating niobium from niobium-containing ore according to claim 12, characterized in that: The mass ratio of the niobium rare earth coarse concentrate, the conditioning agent, the sulfiding agent and the reducing agent in the mixture is 100: (0.1-40): (6-28): (10-26).

14. The method for separating niobium from niobium-containing ore according to claim 12, characterized in that: The reduction smelting temperature is 1240-1600° C., and the reduction smelting time is 20-180 min.

15. The method for separating niobium from niobium-containing ore according to claim 12, characterized in that: The post-treatment of the iron-niobium-rare earth mixture includes the following operations: crushing, screening and magnetically separating the iron-niobium-rare earth mixture to obtain niobium-rare earth slag and iron; and then sorting the niobium-rare earth slag to obtain niobium-rich concentrate and tailings, and the niobium-rich concentrate is recovered as a niobium-rich product.

Citation Information

Patent Citations

  • Method of producing ferrocolumbium

    CN105907990A

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