A method for recovering slag from a horizontal electron beam smelting furnace

By performing crushing, grinding and thermal aluminum reduction reactions on the horizontal electron beam smelting furnace slag, the problem of failure to be effectively recycled and utilized is solved, efficient recycling and utilization of niobium is achieved, and production efficiency and product quality are improved.

CN118563128BActive Publication Date: 2025-02-18CHENGDE TIANDA VANADIUM IND
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Patent Information

Application Number
CN202410646616.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-05-23
Publication Date
2025-02-18
Estimated Expiration
2044-05-23

AI Technical Summary

Technical Problem

In the prior art, the slag produced by the horizontal electron beam smelting furnace during the preparation of the niobium smelting furnace cannot be effectively recycled, resulting in the waste of expensive metal niobium and affecting the economic benefits of the production process.

Method used

By crushing and grinding the slag, slag particles are obtained and mixed with niobium pentoxide and aluminum particles, placed in a vacuum reactor in a specific mass ratio and superposition manner to carry out aluminum thermal reduction reaction, and an aluminum-niobium alloy is prepared and passed The horizontal electron beam smelting furnace is smelted and purified to achieve the recycling of niobium.

Benefits of technology

The niobium elements in the slag are effectively recovered and utilized, which reduces production costs, improves the niobium smelting yield and the composition purity and uniformity of the aluminum-niobium alloy, and ensures the quality of subsequent niobium smelting.

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Abstract

The present invention belongs to the field of recycling of precious metal waste resources, and discloses a method for recycling slag from a horizontal electron beam melting furnace, specifically a method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelting niobium. The slag around the crucible and the smelting niobium ingot is used as a recycling raw material, the slag is crushed and ground to obtain slag particles, and the mixed material obtained by evenly mixing niobium pentoxide and aluminum particles and the slag particles are placed in a vacuum reactor in a certain superposition manner to carry out aluminothermic reduction reaction to prepare an aluminum-niobium alloy, and finally the aluminum-niobium alloy is processed through a horizontal electron beam melting furnace to prepare smelting niobium. The present invention uses the slag produced by the horizontal electron beam melting furnace in the process of preparing smelting niobium as a recycling raw material for the first time, realizes the recycling and reuse of the expensive metal niobium element, and practices the concept of circular economy.
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Description

Technical Field

[0001] The invention belongs to the field of recycling of precious metal waste resources, discloses a method for recovering slag from a horizontal electron beam smelting furnace, and specifically relates to a method for recovering and reusing slag from a horizontal electron beam smelting furnace in the process of preparing smelted niobium. Background Art

[0002] Niobium is a metal with high density, high melting point, good electrical conductivity and superconductivity, and has application needs in metallurgy, superconductivity, electronics, medical treatment, aerospace, atomic energy and other fields. Among them, niobium metal for smelting has the characteristics of high purity and low content of impurities such as oxygen and nitrogen, and has broad market prospects in the field of high-temperature alloys.

[0003] At present, the mainstream production process of niobium metal for smelting is divided into two steps: using niobium oxide and aluminum particles as raw materials, preparing aluminum-niobium alloys such as AlNb90 through aluminothermic reduction reaction, and then placing the aluminum-niobium alloy in a horizontal electron beam melting furnace for multiple smelting and purification to prepare smelting niobium. It is worth noting that during the production process, a lot of slag is often produced around the copper crucible of the horizontal electron beam melting furnace, which is what the industry calls crust slag, etc. These slags are mainly composed of aluminum and niobium. However, niobium oxide is expensive, and the waste of niobium in the slag will affect the economic benefits of the entire production process. How to recycle the slag and reuse the slag has become an important means for enterprises to achieve cost reduction and efficiency improvement and reflect the resource recycling economy.

[0004] Regarding the recovery of niobium, patent CN103415631B discloses a method for dissolving and recovering niobium from ores and concentrates; patent CN111621642A discloses a method for recovering niobium sawdust residues and purifying them. The above methods use ore and niobium sawdust as recovery raw materials, involving complex operations such as pickling, roasting, and magnetic separation, with many influencing factors and high recovery costs. However, the patent of the present invention uses the slag produced by the horizontal electron beam smelting furnace in the process of preparing smelting niobium as the recovery raw material, and there are currently no public reports on the recycling of such slag. Furthermore, taking the recycling of horizontal electron beam smelting furnace slag as the starting point, how to solve the problems involved in the recycling industry, such as complex operations and high recovery costs, has also become a focus of widespread attention. Summary of the invention

[0005] In view of this, the present invention provides a method for recovering slag from a horizontal electron beam smelting furnace, which is a method for recovering and reusing slag from a horizontal electron beam smelting furnace in the process of preparing smelted niobium, and focuses on solving the waste problem of existing slag.

[0006] In order to achieve the above technical objectives, the technical solution disclosed in the present invention is as follows:

[0007] A method for recovering slag from a horizontal electron beam smelting furnace comprises the following steps:

[0008] 1) Using a horizontal electron beam melting furnace to prepare the niobium melting process, after the furnace is taken out, the slag around the crucible and the smelted niobium ingot is collected;

[0009] 2) crushing and grinding the slag collected in step 1) to obtain slag particles;

[0010] 3) placing the slag particles obtained in step 2) and a mixture obtained by uniformly mixing niobium pentoxide and aluminum particles in a vacuum reactor in a certain stacking manner to perform aluminothermic reduction reaction to prepare an aluminum-niobium alloy;

[0011] 4) crushing the aluminum-niobium alloy obtained in step 3), placing it in a horizontal electron beam melting furnace for melting and purification to prepare smelted niobium.

[0012] Optionally, in step 1), the crucible is a cubic, grooved copper crucible with a size of (25-35) mm × (190-210) mm × (1400-1600) mm. The slag is the condensate of various shapes appearing on the crucible wall, the surface of the smelted niobium ingot and the surrounding area. The slag is tested and its main elements are aluminum and niobium, and the mass ratio of the two is Al:Nb=(50-70):(20-40). The purpose of collecting the slag is to avoid the waste of expensive metallic niobium elements in the slag, while ensuring that the crucible wall is removed of impurities to avoid pollution to the production of a new furnace of niobium smelting in the subsequent smelting process.

[0013] Optionally, in step 2), the crushing and grinding are first crushed by a sealed jaw crusher and then ground by a high-energy ball mill. The slag particles are particles with an edge size of less than 1 mm. The purpose of crushing and grinding the slag into particles is to ensure that the slag can be fully added to the subsequent aluminothermic reduction reaction process, to ensure that the aluminum, niobium and other elements in the slag are fully in contact and react with the molten pool, and to improve the recovery rate of the niobium element in the slag.

[0014] Optionally, in step 3), the purity of the niobium pentoxide and aluminum particles is greater than 99.7wt% and 99.8wt%, respectively. The purpose is to reduce the complexity of the subsequent smelting and purification process by reducing the impurity content in the raw materials. The particle sizes of the niobium pentoxide and aluminum particles are 60-100 and 80-120 meshes, respectively. The purpose is to ensure that the raw materials can fully react and improve the uniformity of smelting. The mass ratio of niobium pentoxide to aluminum particles is (11-13): (4-6). The purpose is to ensure that after mixing with the added slag particles, an aluminum-niobium alloy with a niobium content of 85-92wt% can be obtained through aluminothermic reduction reaction.

[0015] Furthermore, the mixing material, i.e., the mixing operation of niobium pentoxide and aluminum particles is performed by using a V-shaped mixer, the mixer speed is 20-50 r / min, and the mixing time is 30-60 minutes, in order to ensure that the raw materials are mixed evenly, which is conducive to the subsequent aluminothermic reduction reaction.

[0016] Furthermore, in step 3), the mass ratio of the mixed material and the slag particles is (93-97):(3-7). The purpose is to ensure that the three substances of niobium pentoxide, aluminum, and aluminum-niobium can participate in the aluminothermic reduction reaction in the best ratio, ultimately improving the smelting yield of niobium and improving the uniformity of composition and structure.

[0017] Furthermore, the superposition method in step 3) is as follows:

[0018] The first step is to use 30-50wt% of the mixture of niobium pentoxide and aluminum particles as the first layer of material and place it at the bottom of the crucible of the vacuum reactor; the second step is to use 40-60wt% of the slag particles as the second layer of material and place it above the first layer of material; the third step is to use 20-40wt% of the mixture of niobium pentoxide and aluminum particles as the third layer of material and place it above the second layer of material; the fourth step is to use 40-60wt% of the slag particles as the fourth layer of material and place it above the third layer of material; the fifth step is to use 20-40wt% of the mixture of niobium pentoxide and aluminum particles as the fifth layer of material and place it at the top. The purpose is to ensure that the raw materials fully undergo aluminothermic reduction reaction, the thermal effect in the furnace and the fluid velocity distribution are optimally configured, and the organization, composition uniformity and stability of the aluminum-niobium alloy product are fully improved.

[0019] Further, in step 3), the aluminothermic reduction reaction, that is, 30 to 50 g of potassium chlorate is placed at the center of the uppermost layer of the material prepared in a certain superposition manner, and then the two aluminum wires drawn from the furnace circuit system are connected using a nickel-chromium resistance wire, and the resistance wire is close to the potassium chlorate powder area. The purpose is that the subsequent start of the igniter will cause the resistance wire to heat up, stimulate the potassium chlorate to react with the material, and the system temperature rises sharply, prompting the aluminothermic reduction reaction to occur. Then, the vacuum reactor is evacuated to ≤20Pa, and the evacuation is stopped. When argon gas is passed to a vacuum degree of 200 to 300Pa, the igniter is started to discharge, and when the ignition current indicates a number of 0, the ignition is terminated, and the vacuum is continued. At the same time, the furnace is cooled for 8 to 12 hours and then taken out of the furnace. After surface cleaning and other treatments, an aluminum-niobium alloy is obtained. The purpose is to ensure that the aluminothermic reduction reaction is in the optimal vacuum range and to achieve effective separation of gas phase impurities such as oxygen and nitrogen in the alloy ingot.

[0020] Furthermore, in step 3), the aluminum-niobium alloy is an AlNb90 alloy having a niobium content of 85-92 wt%.

[0021] Optionally, in step 4), the crushing is performed by using a jaw crusher to crush the particles into particles with an edge size of 5 to 60 mm. The purpose is to ensure that the aluminum-niobium alloy particles can completely exchange energy with the electron beam during electron beam melting, improve the evaporation efficiency of impurity elements, and prevent the molten pool from splashing and affecting the final grade.

[0022] Furthermore, in step 4), the power of the smelting and purification is 200-450 kW, and the smelting speed is 30-120 kg / h. The purpose is to ensure that the metal molten pool is in the best state, which is conducive to the volatilization of impurity elements. The purity of niobium in the smelted niobium is ≥99.9wt%.

[0023] It can be seen from the above technical solution that, compared with the prior art, the present invention provides a method for recovering slag from a horizontal electron beam smelting furnace, which has the following excellent effects:

[0024] 1) The present invention is the first to use the slag produced in the process of preparing niobium by a horizontal electron beam melting furnace as a recycling object. By crushing and grinding the slag, it is used as a raw material for the aluminothermic reduction reaction, thereby realizing the recycling of expensive metal niobium. It is worth noting that this slag is produced when the aluminum-niobium alloy is subjected to horizontal electron beam melting treatment. The slag is hard and has various shapes. In the early stage, people often focused too much on how to control and optimize the entire production process of niobium melting. Even if recycling is considered, they often focus on how to recover the elemental niobium element through chemical methods such as pickling, ignoring the economic, quick and simple means of recycling the slag as a raw material for the aluminothermic reduction reaction without chemical treatment, only physical crushing and grinding, and using the characteristics of the high aluminum content in the slag in addition to niobium (the aluminum in the slag can serve as a reducing agent for niobium) without chemical treatment.

[0025] 2) The present invention arranges the raw materials participating in the aluminothermic reduction reaction, such as niobium pentoxide, aluminum particles, and recovered slag, in a special superimposed manner at a certain mass ratio, thereby ensuring that all raw materials fully participate in the reaction, optimizing the thermal cycle distribution of the molten pool, greatly improving the smelting yield of niobium, ensuring the purity and uniformity of the components of the aluminum-niobium alloy, and facilitating the quality of subsequent electron beam smelting of niobium.

[0026] It is worth noting that the above-mentioned effects can only be achieved through the mass ratio and superposition method of the present invention. Otherwise, the aluminum-niobium alloy prepared by the aluminothermic reduction reaction has a high impurity content and severe segregation, and the niobium grade is insufficient, and cannot be used as a raw material for producing niobium smelting in a horizontal electron beam furnace. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0028] Figure 1 (a) is a photo of a horizontal electron beam melting furnace just out of the furnace (including the grooved copper crucible, the molten niobium ingot in the middle of the crucible, and the surrounding slag), and (b) is a magnified observation of a suitable amount of slag.

[0029] Figure 2 It is a schematic diagram of the superposition method of the present invention.

[0030] Figure 3 This is the slag morphology taken from the furnace wall of the horizontal electron beam melting furnace in Comparative Example 1. DETAILED DESCRIPTION

[0031] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0032] The word "embodiment" used here as an "exemplary" does not necessarily mean that any embodiment described is superior to or better than other embodiments. Unless otherwise specified, the performance index tests in the embodiments of this application are performed using conventional test methods in the art. It should be understood that the terms described in this application are only used to describe specific implementation methods and are not used to limit the content disclosed in this application.

[0033] Unless otherwise specified, the technical and scientific terms used herein have the same meanings as those commonly understood by those skilled in the art to which this application belongs; other experimental methods and technical means not specifically noted in this application refer to experimental methods and technical means commonly used by those skilled in the art. Under the premise of no conflict, the technical features disclosed in the embodiments of this application can be combined arbitrarily, and the resulting technical solutions belong to the contents disclosed in the embodiments of this application.

[0034] In order to better understand the present invention, the present invention is further specifically described below through the following examples, but it should not be understood as a limitation of the present invention. Some non-essential improvements and adjustments made by technicians in this field based on the above invention content are also considered to fall within the protection scope of the present invention.

[0035] Example 1

[0036] The slag around the smelted niobium ingot is used as a recycled raw material, the slag is crushed and ground to obtain slag particles with an edge size of less than 1 mm, and a mixed material obtained by uniformly mixing niobium pentoxide and aluminum particles (the mass ratio of niobium pentoxide to aluminum particles is 12:5) and slag particles are stacked in a certain stacking manner according to a mass ratio of 95:5 (40wt% of the niobium pentoxide and aluminum particle mixture is used as the first layer material and placed at the bottom of the crucible of the vacuum reactor; 50wt% of the slag particles is used as the second layer material; 30wt% of the niobium pentoxide and aluminum particle mixture is used as the third layer material; 50wt% of the slag particles is used as the fourth layer material; 30wt% of the niobium pentoxide and aluminum particle mixture is used as the fifth layer material and placed at the top of the crucible) ) is placed in a vacuum reactor for aluminothermic reduction reaction to prepare aluminum-niobium alloy (that is, 35g of potassium chlorate is placed at the center of the uppermost layer of the material, and two aluminum wires led out of the furnace circuit system are connected using a nickel-chromium resistance wire, and the resistance wire is close to the potassium chlorate powder area. The vacuum reactor is evacuated to 10Pa, and the evacuation is stopped. When the vacuum degree is 230Pa, the igniter is started to discharge. When the ignition current indicates 0, the ignition is terminated, and the evacuation is continued. At the same time, the furnace is cooled for 10 hours before being taken out of the furnace. After surface cleaning and other treatments, the aluminum-niobium alloy is obtained), and finally the aluminum-niobium alloy is processed in a horizontal electron beam melting furnace to prepare smelted niobium (the smelting power of the horizontal electron beam melting furnace is 260kW, and the smelting speed is 60kg / h). After testing, the purity of the smelted niobium ingot is ≥99.9wt%.

[0037] Example 2

[0038] The preparation method of this embodiment is similar to that of embodiment 1, except that the mixture obtained by uniformly mixing niobium pentoxide and aluminum particles and the slag particles are subjected to aluminothermic reduction reaction at a mass ratio of 97:3. After testing, the purity of the smelted niobium ingot is ≥99.9wt%.

[0039] Example 3

[0040] The preparation method of this embodiment is similar to that of embodiment 1, except that: 30wt% of the mixture of niobium pentoxide and aluminum particles is used as the first layer material and placed at the bottom of the crucible of the vacuum reactor; 40wt% of the slag particles are used as the second layer material; 40wt% of the mixture of niobium pentoxide and aluminum particles is used as the third layer material; 60wt% of the slag particles is used as the fourth layer material; 30wt% of the mixture of niobium pentoxide and aluminum particles is used as the fifth layer material and placed at the top of the crucible. After testing, the purity of the smelted niobium ingot is ≥99.9wt%.

[0041] Example 4

[0042] The preparation method of this embodiment is similar to that of embodiment 1, except that the horizontal electron beam melting furnace is used to melt the aluminum-niobium alloy with a melting power of 400 kW and a melting speed of 90 kg / h. After testing, the purity of the melted niobium ingot is ≥99.9wt%.

[0043] In order to further demonstrate the beneficial effects of the present invention and to better understand the present invention, the following comparative examples are used to further illustrate the technical features disclosed in the present invention, but they should not be construed as limiting the present invention. Other improvements made by those skilled in the art based on the above invention content without inventive work are also considered to fall within the scope of protection of the present invention.

[0044] Comparative Example 1

[0045] The preparation method of this comparative example is similar to that of Example 1, except that the slag from the furnace wall of the horizontal electron beam melting furnace is used as the recycled raw material.

[0046] After testing, the purity of the smelted niobium was far below 99wt%, which was not in line with expectations. This was because the slag was taken from the furnace wall of the horizontal electron beam melting furnace (such as Figure 3 As shown). According to the test, the slag here has a low niobium content, and the main element content is: Nb 5-8wt%, Al 87-90wt%, O 1.4-1.8wt%, and there are also impurity elements such as N, C, Fe, Si, S and a small amount of insoluble matter. According to the mass ratio of Example 1, the slag with low Nb content will introduce more impurities; according to the smelting process and parameters of the present invention, it is difficult to obtain smelted niobium with purity that meets the requirements.

[0047] Comparative Example 2

[0048] The preparation method of this comparative example is similar to that of Example 1, except that the slag is only crushed without grinding, and the edge size of most slag particles is between 2 and 10 mm. In addition, the mixed material and slag particles obtained by uniformly mixing niobium pentoxide and aluminum particles are subjected to aluminothermic reduction reaction at a mass ratio of 9:1.

[0049] After testing, the purity of the smelted niobium is far below 99wt%, which is not in line with expectations. This is because when the aluminothermic reduction reaction occurs, the slag particles are large and account for a large proportion of the mass, the solubility and participation of the slag particles in the molten pool are insufficient, and the aluminothermic reduction reaction time is very short, it is difficult to ensure that the slag such as alumina and the aluminum-niobium alloy are completely separated, the purity of the aluminum-niobium alloy is insufficient, and finally it is difficult to obtain smelted niobium with purity that meets the requirements.

[0050] Comparative Example 3

[0051] The preparation method of this comparative example is similar to that of Example 1, except that: the stacking method of the materials in the vacuum reactor is different (the stacking order is the same, but the mass of each layer of materials is different), that is, 20wt% of the mixture of niobium pentoxide and aluminum particles is used as the first layer of material and placed at the bottom of the crucible of the vacuum reactor; 70wt% of the slag particles is used as the second layer of material; 10wt% of the mixture of niobium pentoxide and aluminum particles is used as the third layer of material; 30wt% of the slag particles is used as the fourth layer of material; and 70wt% of the mixture of niobium pentoxide and aluminum particles is used as the fifth layer of material and placed on the top.

[0052] After testing, the purity of the smelted niobium is far below 99wt%, which is not in line with expectations. This is because this superposition method does not allow the raw materials to fully undergo aluminothermic reduction reaction, the thermal effect in the furnace and the fluid velocity distribution cannot achieve the optimal configuration, the purity and composition uniformity of the aluminum-niobium alloy are insufficient, and finally it is difficult to obtain smelted niobium with purity that meets the requirements.

[0053] Comparative Example 4

[0054] The preparation method of this comparative example is similar to that of Example 1, except that: the stacking method of the materials in the vacuum reactor is different (the mass of each layer of materials is the same, but the stacking order is different). That is, 50wt% of the slag particles are used as the first layer of materials and placed at the bottom of the crucible of the vacuum reactor; 30wt% of the mixture of niobium pentoxide and aluminum particles are used as the second layer of materials; 30wt% of the mixture of niobium pentoxide and aluminum particles are used as the third layer of materials; 50wt% of the slag particles are used as the fourth layer of materials; and 40wt% of the mixture of niobium pentoxide and aluminum particles are used as the fifth layer of materials and placed at the top of the crucible.

[0055] After testing, the purity of the smelted niobium was far below 99wt%, which was not in line with expectations. This was because the stacking method did not achieve the optimal arrangement of the raw materials, the aluminothermic reduction reaction was not fully achieved at each position in the furnace, and the entire ingot showed obvious segregation, making it difficult to obtain smelted niobium with a purity that met the requirements.

[0056] Comparative Example 5

[0057] The preparation method of this comparative example is similar to that of Example 1, except that: the stacking method of the materials in the vacuum reactor is different (the stacking order and the mass of each layer of materials are different), that is, 30wt% of the slag particles are used as the first layer of materials and placed at the bottom of the crucible of the vacuum reactor; 50wt% of the mixture of niobium pentoxide and aluminum particles are used as the second layer of materials; 40wt% of the slag particles are used as the third layer of materials; 50wt% of the mixture of niobium pentoxide and aluminum particles are used as the fourth layer of materials; and 30wt% of the slag particles are used as the fifth layer of materials and placed at the top.

[0058] After testing, the purity of the smelted niobium was far below 99wt%, which was not in line with expectations. This was because the stacking method did not achieve the optimal arrangement of the raw materials, the aluminothermic reduction reaction was not fully achieved at each position in the furnace, and the entire ingot showed obvious segregation, making it difficult to obtain smelted niobium with a purity that met the requirements.

[0059] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium, characterized in that: The method specifically comprises the following steps: 1) Use a horizontal electron beam melting furnace to prepare the niobium melting process. After the furnace is taken out, collect the slag around the crucible and the smelted niobium ingot; 2) crushing and grinding the slag collected in step 1) to obtain slag particles; 3) placing the slag particles obtained in step 2) and a mixture obtained by uniformly mixing niobium pentoxide and aluminum particles in a vacuum reactor in a certain stacking manner to perform aluminothermic reduction reaction to prepare an aluminum-niobium alloy; 4) crushing the aluminum-niobium alloy obtained in step 3), placing it in a horizontal electron beam melting furnace for melting and purification to prepare smelting niobium; The slag is a condensate of various shapes appearing on the crucible wall, the surface of the smelted niobium ingot and the surroundings. The main elements of the slag are aluminum and niobium, and the mass ratio of aluminum to niobium is (50-70): (20-40); The superposition method is as follows: In the first step, 30-50 wt% of the mixed material is used as the first layer material and placed at the bottom of the crucible of the vacuum reactor; In the second step, 40-60wt% of the slag particles are used as the second layer material and placed on top of the first layer material; The third step is to use 20-40wt% of the mixed material as the third layer material and place it on the second layer material; The fourth step is to use 40-60wt% of the slag particles as the fourth layer material, which is placed on the third layer material; The fifth step is to use 20-40wt% of the mixed material as the fifth layer material and place it on the top.

2. The method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium according to claim 1, characterized in that: In step 2), the crushing and grinding are firstly crushed by a sealed jaw crusher and then ground by a high-energy ball mill; the slag particles are particles with an edge size of less than 1 mm.

3. The method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium according to claim 1, characterized in that: In step 3), the purity of the niobium pentoxide is greater than 99.7wt%, and the particle size is 60-100 mesh; the purity of the aluminum particles is greater than 99.8wt%, and the particle size is 80-120 mesh; and the mass ratio of niobium pentoxide to aluminum particles is (11-13):(4-6).

4. The method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium according to claim 1 or 3, characterized in that: The mixing material is to use a V-shaped mixer to mix niobium pentoxide and aluminum particles, the mixer speed is 20-50 r / min, and the mixing time is 30-60 minutes.

5. The method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium according to claim 4, characterized in that: The mass ratio of the mixed material to the slag particles is (93-97): (3-7).

6. The method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium according to claim 1, characterized in that: In step 4), the crushing, i.e., using a jaw crusher to crush the aluminum-niobium alloy into particles with an edge size of 5 to 60 mm; the power of the smelting and purification is 200 to 450 kW, and the smelting speed is 30 to 120 kg / h.

7. The method for recycling slag from a horizontal electron beam melting furnace in the process of preparing smelted niobium according to claim 1, characterized in that: The aluminum-niobium alloy is an AlNb90 alloy with a niobium content of 85-92wt%, and the purity of niobium in the smelted niobium is ≥99.9wt%.

Citation Information

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