Metal vapor collection condensing device, method for separating rare earth metals

Abstract

This invention provides a metal vapor collection and condensation device and a method for rare earth metal separation, belonging to the field of lithium batteries. The metal vapor collection and condensation device includes a crucible lid 1, a crucible bottom 2, and a plurality of graphite components 3 disposed between the crucible lid 1 and the crucible bottom 2. The graphite components 3 have through-hole structures in the direction from the crucible lid 1 to the crucible bottom 2. A first liner 4 is provided on the inner side of each graphite component 3. A condensation plate 7 is provided between the crucible lid 1 and adjacent graphite components 3. When the number of graphite components 3 is ≥2, a baffle 5 is also provided between adjacent graphite components. The baffle 5 has through-hole structures. A second liner 6 is provided on the inner side of the crucible bottom 2. This invention's metal vapor collection and condensation device can reduce the pollution risk during the high-temperature processing of volatile metals and improve the convenience of removing and recovering distillation condensation products.

Description

Technical Field

[0001] This invention relates to the field of rare earth metal purification and alloy separation, specifically to a metal vapor collection and condensation device and a method for rare earth metal separation. Background Technology

[0002] With the continuous development of rare earth material preparation, purification, and separation technologies, the material selection of high-temperature experimental equipment has a significant impact on the stability of the experimental process, product purity, and subsequent sampling operations. As a key component directly supporting raw materials and collecting products during high-temperature processing, the suitability of the crucible's material and structure directly affects reaction contamination, product recovery, and experimental repeatability.

[0003] Common crucibles made of materials such as graphite and corundum possess certain high-temperature resistance properties, meeting the needs of most routine experiments. However, when handling highly reactive or volatile metal materials, these materials still exhibit insufficient compatibility. For example, with samarium-containing materials (such as samarium-cobalt permanent magnet waste or other samarium-containing alloys), under high-temperature conditions, the highly reactive rare earth element samarium may react with graphite or corundum, causing contamination of raw materials or products, thus affecting subsequent purification and separation. For other volatile metals or alloys containing volatile metals, the condensation and collection efficiency may also be affected by the reaction, wetting, or adhesion of metal vapors to the vessel wall material.

[0004] Molybdenum exhibits good chemical compatibility in handling samarium-containing materials. Under high-temperature conditions, samarium and metallic molybdenum do not readily react, thus molybdenum is frequently used in high-temperature experimental environments for samarium-containing materials. However, different volatile metal systems exhibit variations in reactivity, melting point, and wetting behavior, meaning that a single molybdenum material may not be suitable for all experimental materials. Using a straight-sided compatibility crucible can also introduce new operational challenges: firstly, molten metal may penetrate or adhere to the crucible surface, making it difficult to remove residual material after the experiment; secondly, during vacuum distillation or condensation, condensate tends to uniformly coat the inner wall of the straight-sided crucible, and due to the crucible's structure, the removal and recovery of condensate is challenging.

[0005] Therefore, there is an urgent need to design a device structure that takes into account both the selectivity of contact materials and the convenience of separate sampling, so that the components in contact with raw materials, metal vapor or condensate products can be adjusted according to the properties of the experimental raw materials, thereby reducing the pollution risk during the high-temperature treatment of volatile metals and improving the product recovery operation after the experiment. Summary of the Invention

[0006] This invention provides a metal vapor collection and condensation device and a method for rare earth metal separation. The metal vapor collection and condensation device of this invention can take into account both the selectivity of contact materials and the convenience of separate sampling.

[0007] The present invention provides a metal vapor collection and condensation device, the components of which include a crucible lid 1, a crucible bottom 2, and a plurality of graphite parts 3 disposed between the crucible lid 1 and the crucible bottom 2; the graphite parts 3 have through-hole structures in the direction from the crucible lid 1 to the crucible bottom 2. The graphite component 3 has a first liner 4 on its inner side; A condenser plate 7 is provided between the crucible lid 1 and the adjacent graphite part 3; When the number of graphite parts 3 is ≥2, a baffle 5 is also provided between adjacent graphite parts; the baffle 5 has a through hole structure; A second lining layer 6 is provided on the inner side of the crucible bottom 2.

[0008] Preferably, the raw materials for preparing the liner 4, liner 6, baffle 5 and condenser plate 7 include one or more of metals, alloys and ceramics.

[0009] Preferably, the raw materials for preparing the liner 4, liner 6, baffle 5 and condenser plate 7 include one or more of molybdenum, tungsten, tantalum, niobium, titanium, nickel-based alloys, boron nitride, aluminum oxide and zirconium oxide.

[0010] Preferably, adjacent components are detachably connected.

[0011] Preferably, the detachable connection is a mutually compatible threaded connection, a fitting connection, or a stepped limiting connection.

[0012] Preferably, the graphite part has a groove on its upper surface for accommodating and limiting the baffle 5.

[0013] This invention also provides a method for separating rare earth metals, carried out in the metal vapor collection and condensation device described in the above technical solution, comprising the following steps: Raw materials containing rare earth metals are placed in a metal vapor collection and condensation device for vacuum distillation and condensation.

[0014] Preferably, when the raw material is a samarium-cobalt alloy, samarium-copper alloy or samarium-iron alloy, the raw material for preparing the first liner 4, the second liner 6, the baffle 5 and the condenser plate 7 is molybdenum.

[0015] Preferably, the vacuum distillation temperature is 1218~1673K, the time is 2~3h, and the vacuum degree is 0.005~0.02Pa.

[0016] Preferably, when the raw material is crude scandium, the raw material for preparing the first liner 4, the second liner 6, the baffle 5 and the condenser plate 7 is tungsten; The vacuum distillation was performed at a temperature of 1983 K for 3 hours, with a vacuum level of 0.0067 Pa.

[0017] The first liner 4, the second liner 6, the baffle 5, and the condenser plate 7 in the metal vapor collection and condensation device of the present invention can be selected according to the reactivity, wettability, melting point, and high-temperature chemical compatibility of the metal or alloy to be treated. This can reduce the pollution risk during the high-temperature treatment of volatile metals and improve the convenience of taking out and recovering the distillation condensation products.

[0018] In addition, the metal vapor collection and condensation device of the present invention also has the good support and thermal conductivity of graphite material. Attached Figure Description

[0019] Figure 1 This is a schematic diagram of the device used in the embodiment. Detailed Implementation

[0020] The present invention provides a metal vapor collection and condensation device, the components of which include a crucible lid 1, a crucible bottom 2, and a plurality of graphite parts 3 disposed between the crucible lid 1 and the crucible bottom 2; the graphite parts 3 have through-hole structures in the direction from the crucible lid 1 to the crucible bottom 2. The graphite component 3 has a first liner 4 on its inner side; A condenser plate 7 is provided between the crucible lid 1 and the adjacent graphite part 3; When the number of graphite parts 3 is ≥2, a baffle 5 is also provided between adjacent graphite parts; the baffle 5 has a through hole structure; A second lining layer 6 is provided on the inner side of the crucible bottom 2.

[0021] The components of the metal vapor collection and condensation device provided by the present invention include a crucible lid 1.

[0022] The metal vapor collection and condensation device provided by the present invention includes a crucible bottom 2. The crucible bottom 2 includes a bottom receiving cavity for holding the volatile metal material to be processed.

[0023] In this invention, a second liner 6 is provided on the inner side of the crucible bottom 2. That is, the second liner 6 covers the inner wall of the cavity of the crucible bottom 2.

[0024] In one specific embodiment of the present invention, the raw materials for preparing the second liner 6 include one or more of metals, alloys and ceramics.

[0025] In one specific embodiment of the present invention, the raw materials for preparing the second liner 6 include one or more of molybdenum, tungsten, tantalum, niobium, titanium, nickel-based alloys, boron nitride, aluminum oxide, and zirconium oxide.

[0026] The metal vapor collection and condensation device provided by the present invention includes a plurality of graphite parts 3 disposed between the crucible lid 1 and the crucible bottom 2; the graphite parts 3 have through-hole structures in the direction from the crucible lid 1 to the crucible bottom 2. The graphite parts 3 have through-hole structures in the direction from the crucible lid 1 to the crucible bottom 2, and a groove is provided above the graphite parts for accommodating and limiting the baffle 5.

[0027] In this invention, the number of graphite parts 3 is preferably 3.

[0028] When the number of graphite parts 3 is ≥2, a baffle 5 is also provided between adjacent graphite parts; the baffle 5 has a through hole structure; a first liner 4 is provided on the inner side of the graphite parts 3.

[0029] In one specific embodiment of the present invention, the raw materials for preparing the first liner 4 include one or more of metals, alloys and ceramics.

[0030] In one specific embodiment of the present invention, the raw materials for preparing the first liner 4 include one or more of molybdenum, tungsten, tantalum, niobium, titanium, nickel-based alloys, boron nitride, aluminum oxide, and zirconium oxide.

[0031] Graphite components are mainly used as outer shell support parts. The good thermal conductivity and easy processing properties of graphite material help to improve the overall heating uniformity of the crucible.

[0032] In one specific embodiment of the present invention, when the number of graphite elements 3 is ≥ n, and n=3, and the number of baffles is n-1 (i.e., multiple), the baffles 5 are stacked along the crucible axis. Axial stacking can increase the condensation path and condensation area, which is suitable for experimental situations requiring segmented condensation or improved collection efficiency. The number of baffle layers is adjustable, and the contact materials are replaceable, which can adapt to different experimental scales, condensation requirements, and volatile metal systems.

[0033] In one specific embodiment of the present invention, the raw materials for preparing the baffle 5 include one or more of metals, alloys and ceramics.

[0034] In one specific embodiment of the present invention, the raw materials for preparing the baffle 5 include one or more of molybdenum, tungsten, tantalum, niobium, titanium, nickel-based alloys, boron nitride, aluminum oxide, and zirconium oxide.

[0035] In one specific embodiment of the present invention, a condenser plate 7 is provided between the crucible lid 1 and the adjacent graphite part 3.

[0036] In one specific embodiment of the present invention, the raw materials for preparing the condenser plate 7 include one or more of metals, alloys and ceramics.

[0037] In one specific embodiment of the present invention, the raw materials for preparing the condenser plate 7 include one or more of molybdenum, tungsten, tantalum, niobium, titanium, nickel-based alloys, boron nitride, aluminum oxide, and zirconium oxide.

[0038] The condenser plate 7, as an additional condensing component near the top of the crucible, increases the condensing contact surface, is used to receive rising vapor and collect condensed products, and at the same time reduces the assembly redundancy that may be caused by setting a baffle at the top position.

[0039] The area inside the device that comes into contact with raw materials, metal vapor, or condensed products is composed of a first liner 4, a second liner 6, a baffle 5, and a condenser plate 7. That is, the raw materials, metal vapor, or condensed products do not come into direct contact with the graphite parts or the bottom of the crucible. Suitable materials can be selected according to different experimental raw materials to reduce the risk of high-temperature reactions or contamination.

[0040] In one specific embodiment of the present invention, adjacent components are detachably connected.

[0041] In one specific embodiment of the present invention, the detachable connection is a mutually compatible threaded connection, a fitting connection, or a stepped limiting connection.

[0042] Detachable connections facilitate assembly, disassembly, and cleaning.

[0043] In one specific embodiment of the present invention, the graphite component adjacent to the crucible lid 1 is provided with a groove for accommodating and limiting the baffle 5. The baffle 5 forms a blocking surface or condensation surface inside the crucible, facilitating the adhesion of condensed products and their removal along with the baffle after the experiment.

[0044] This invention also provides a method for separating rare earth metals, carried out in the metal vapor collection and condensation device described in the above technical solution, comprising the following steps: Raw materials containing rare earth metals are placed in a metal vapor collection and condensation device for vacuum distillation and condensation.

[0045] In this invention, when the raw material is preferably a samarium-cobalt alloy, samarium-copper alloy, or samarium-iron alloy, the raw material for preparing the first liner 4, the second liner 6, the baffle 5, and the condenser plate 7 is preferably molybdenum; the vacuum distillation temperature is preferably 1218~1673K, the time is preferably 2~3h, and the vacuum degree is preferably 0.005~0.02Pa.

[0046] In this invention, when the raw material is preferably crude scandium, the raw material for preparing the first liner 4, the second liner 6, the baffle 5 and the condenser plate 7 is preferably tungsten; The preferred temperature for vacuum distillation is 1983 K, the preferred time is 3 h, and the preferred vacuum level is 0.0067 Pa.

[0047] The method of the present invention selects a compatible material based on the properties of the volatile metal in the raw material to be treated; the compatible material is made into or set as a liner, baffle, and / or condenser; the raw material to be treated is placed on the compatible material liner on the inner side of the crucible bottom; one or more baffle layers are assembled and the crucible lid is installed according to experimental requirements; heating is carried out under vacuum or protective atmosphere conditions to evaporate the volatile metal and condense it on the compatible material baffle and / or compatible material condenser; after cooling, the crucible lid and baffle layers are removed and the condensed product is taken out, which improves the convenience of taking out and recovering the distillation condensate.

[0048] The following detailed description of the metal vapor collection and condensation device and rare earth metal separation method provided by the present invention, with reference to the embodiments, should not be construed as limiting the scope of protection of the present invention.

[0049] Figure 1 This is a schematic diagram of the device used in the embodiment.

[0050] Example 1 This embodiment takes vacuum distillation of samarium-cobalt permanent magnet waste as an example, and the corresponding compatible material is molybdenum.

[0051] A second molybdenum liner 6 is provided on the inner side of the crucible bottom 2. The second molybdenum liner 6 covers the inner wall of the bottom cavity of the crucible bottom 2, so that the samarium cobalt permanent magnet waste to be processed does not directly contact the graphite shell during the heating process.

[0052] Next, install three graphite components 3 in sequence according to experimental requirements. A molybdenum first liner 4 is provided on the inner side of each graphite component 3. A molybdenum baffle 5 is installed between adjacent graphite components 3. A molybdenum condenser plate 7 is placed above the uppermost graphite component 3. Finally, install the crucible lid 1. After the experiment is completed and cooled, the crucible lid 1 and graphite components 3 can be removed, and the molybdenum baffle 5, molybdenum condenser plate 7, and molybdenum first liner 4 can be taken out, thereby realizing the separation and recovery of the condensed products.

[0053] Under the process conditions of vacuum degree of 0.008 Pa, distillation temperature of 1673 K and holding time of 3 h, the recovery rate of samarium in the distillation product can reach 95.47%, and the purity of the collected samarium is 99.5502 wt% as detected by glow discharge mass spectrometry.

[0054] Example 2 This embodiment takes vacuum distilled samarium copper alloy as an example, and the corresponding compatible material is molybdenum.

[0055] A second molybdenum liner 6 is provided on the inner side of the crucible bottom 2. The second molybdenum liner 6 covers the inner wall of the bottom cavity of the crucible bottom 2, so that the samarium copper alloy to be processed does not directly contact the graphite shell during the heating process.

[0056] Next, install three graphite components 3 in sequence according to experimental requirements. A molybdenum first liner 4 is provided on the inner side of each graphite component 3. A molybdenum baffle 5 is installed between adjacent graphite components 3. A molybdenum condenser plate 7 is placed above the uppermost graphite component 3. Finally, install the crucible lid 1. After the experiment is completed and cooled, the crucible lid 1 and graphite components 3 can be removed, and the molybdenum baffle 5, molybdenum condenser plate 7, and molybdenum first liner 4 can be taken out, thereby realizing the separation and recovery of the condensed products.

[0057] Under the process conditions of vacuum degree of 0.0085 Pa, distillation temperature of 1218 K and holding time of 2 h, the recovery rate of samarium in the distillation product can reach 93.97%, and the purity of the collected samarium is 99.9973 wt% as detected by glow discharge mass spectrometry.

[0058] Example 3 This embodiment takes vacuum distilled samarium-iron alloy as an example, and the corresponding compatible material is molybdenum.

[0059] A second molybdenum liner 6 is provided on the inner side of the crucible bottom 2. The second molybdenum liner 6 covers the inner wall of the bottom cavity of the crucible bottom 2, so that the samarium iron alloy to be treated does not directly contact the graphite shell during the heating process.

[0060] Next, install three graphite components 3 in sequence according to experimental requirements. A molybdenum first liner 4 is provided on the inner side of each graphite component 3. A molybdenum baffle 5 is installed between adjacent graphite components 3. A molybdenum condenser plate 7 is placed above the uppermost graphite component 3. Finally, install the crucible lid 1. After the experiment is completed and cooled, the crucible lid 1 and graphite components 3 can be removed, and the molybdenum baffle 5, molybdenum condenser plate 7, and molybdenum first liner 4 can be taken out, thereby realizing the separation and recovery of the condensed products.

[0061] Under the process conditions of vacuum degree of 0.013 Pa, distillation temperature of 1673 K and holding time of 2 h, the recovery rate of samarium in the distillation product can reach 92.48%, and the purity of the collected samarium is 99.9944 wt% as detected by glow discharge mass spectrometry.

[0062] Example 4 This embodiment takes vacuum distilled samarium-cobalt alloy as an example, and the corresponding compatible material is molybdenum.

[0063] A second molybdenum liner 6 is provided on the inner side of the crucible bottom 2. The second molybdenum liner 6 covers the inner wall of the bottom cavity of the crucible bottom 2, so that the samarium cobalt alloy to be processed does not directly contact the graphite shell during the heating process.

[0064] Next, install three graphite components 3 in sequence according to experimental requirements. A molybdenum first liner 4 is provided on the inner side of each graphite component 3. A molybdenum baffle 5 is installed between adjacent graphite components 3. A molybdenum condenser plate 7 is placed above the uppermost graphite component 3. Finally, install the crucible lid 1. After the experiment is completed and cooled, the crucible lid 1 and graphite components 3 can be removed, and the molybdenum baffle 5, molybdenum condenser plate 7, and molybdenum first liner 4 can be taken out, thereby realizing the separation and recovery of the condensed products.

[0065] Under the process conditions of vacuum degree of 0.016 Pa, distillation temperature of 1673 K and holding time of 2 h, the recovery rate of samarium in the distillation product can reach 94.11%, and the purity of the collected samarium is 99.9913 wt% as detected by glow discharge mass spectrometry.

[0066] Example 5 This embodiment takes vacuum distillation of 3N grade metallic scandium as an example, and the corresponding compatible material is tungsten.

[0067] A second tungsten liner 6 is provided on the inner side of the crucible bottom 2. The second tungsten liner 6 covers the inner wall of the bottom cavity of the crucible bottom 2, so that the 3N grade scandium metal to be processed does not directly contact the graphite shell during the heating process.

[0068] Next, install four graphite components 3 in sequence according to experimental requirements. A tungsten first liner 4 is provided on the inner side of each graphite component 3. Tungsten baffles 5 are installed between adjacent graphite components 3. A tungsten condenser plate 7 is placed above the uppermost graphite component 3. Finally, the crucible lid 1 is installed. After the experiment is completed and cooled, the crucible lid 1 and graphite components 3 can be removed, and the tungsten baffles 5, tungsten condenser plate 7, and tungsten first liner 4 can be taken out, thereby realizing the separation and recovery of the condensation products.

[0069] Under the process conditions of vacuum degree of 0.0067 Pa, distillation temperature of 1983 K and holding time of 3 h, the recovery rate of scandium in the distillation product can reach 98.23%, and the purity of the collected scandium is 99.9937 wt% as detected by glow discharge mass spectrometry.

[0070] Comparative Example 1 This comparative example uses vacuum distillation of samarium-cobalt permanent magnet waste in a cylindrical graphite crucible as an example, with molybdenum as the corresponding compatible material.

[0071] A molybdenum liner is installed inside the crucible, covering the inner wall of the bottom cavity to prevent the samarium-cobalt permanent magnet waste from directly contacting the graphite shell during heating. A molybdenum condenser plate is installed under the crucible lid. After the experiment is completed and cooled, the molybdenum liner and condenser plate are removed, thereby achieving the separation and recovery of the condensation products.

[0072] Under the process conditions of vacuum degree of 0.0078 Pa, distillation temperature of 1673 K and holding time of 3 h, the recovery rate of samarium in the distillation product was only 32.55%. The purity of the collected samarium was 93.5411 wt% as determined by inductively coupled plasma atomic emission spectrometry.

[0073] Comparative Example 2 This comparative example uses vacuum distillation of samarium copper alloy in a cylindrical graphite crucible as an example, with molybdenum as the corresponding compatible material.

[0074] A molybdenum liner is placed inside the crucible, covering the inner wall of the bottom cavity to prevent the samarium copper alloy from directly contacting the graphite shell during heating. A molybdenum condenser is installed under the crucible lid. After the experiment is completed and cooled, the molybdenum liner and condenser are removed, thereby achieving the separation and recovery of the condensation products.

[0075] Under the process conditions of vacuum degree of 0.0086 Pa, distillation temperature of 1218 K and holding time of 2 h, the recovery rate of samarium in the distillation product was only 56.22%. The purity of the collected samarium was 99.9806 wt% as determined by inductively coupled plasma atomic emission spectrometry.

[0076] Comparative Example 3 This comparative example uses vacuum distillation of samarium-cobalt alloy in a cylindrical graphite crucible as an example, with molybdenum as the corresponding compatible material.

[0077] A molybdenum liner is placed inside the crucible, covering the inner wall of the bottom cavity to prevent the samarium-cobalt alloy from directly contacting the graphite shell during heating. A molybdenum condenser is installed under the crucible lid. After the experiment is completed and cooled, the molybdenum liner and condenser are removed, thereby achieving the separation and recovery of the condensation products.

[0078] Under the process conditions of vacuum degree of 0.014 Pa, distillation temperature of 1673 K and holding time of 2 h, the recovery rate of samarium in the distillation product was only 39.41%. The purity of the collected samarium was 99.9891 wt% as determined by inductively coupled plasma atomic emission spectrometry.

[0079] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A metal vapor collection and condensation device, characterized in that, The components of the metal vapor collection and condensation device include a crucible lid (1), a crucible bottom (2), and a plurality of graphite parts (3) disposed between the crucible lid (1) and the crucible bottom (2); the graphite parts (3) have through-hole structures in the direction from the crucible lid (1) to the crucible bottom (2); The graphite part (3) has a first liner (4) on its inner side. A condenser plate (7) is provided between the crucible lid (1) and the adjacent graphite part (3). When the number of graphite parts (3) is ≥2, a baffle (5) is also provided between adjacent graphite parts; the baffle (5) has a through hole structure; A second liner (6) is provided on the inner side of the crucible bottom (2).

2. The metal vapor collection and condensation device according to claim 1, characterized in that, The raw materials used to prepare the liner (4), liner (6), baffle (5) and condenser plate (7) include one or more of metals, alloys and ceramics.

3. The metal vapor collection and condensation device according to claim 1, characterized in that, The raw materials used to prepare the liner (4), liner (6), baffle (5) and condenser plate (7) include one or more of molybdenum, tungsten, tantalum, niobium, titanium, nickel-based alloys, boron nitride, aluminum oxide and zirconium oxide.

4. The metal vapor collection and condensation device according to claim 1, characterized in that, Adjacent components are detachably connected.

5. The metal vapor collection and condensation device according to claim 4, characterized in that, The detachable connection is a mutually compatible threaded connection, a fitting connection, or a stepped limiting connection.

6. The metal vapor collection and condensation device according to claim 1, characterized in that, The graphite piece has a groove on its upper part for accommodating and limiting the baffle (5).

7. A method for separating rare earth metals, characterized in that, The metal vapor collection and condensation apparatus according to any one of claims 1 to 6 is used, comprising the following steps: Raw materials containing rare earth metals are placed in a metal vapor collection and condensation device for vacuum distillation and condensation.

8. The method according to claim 7, characterized in that, When the raw material is samarium-cobalt alloy, samarium-copper alloy or samarium-iron alloy, the raw material for preparing the first liner (4), the second liner (6), the baffle (5) and the condenser plate (7) is molybdenum.

9. The method according to claim 8, characterized in that, The vacuum distillation temperature is 1218~1673K, the time is 2~3h, and the vacuum degree is 0.005~0.02Pa.

10. The method according to claim 7, characterized in that, When the raw material is crude scandium, the raw material for preparing the first liner (4), the second liner (6), the baffle (5) and the condenser plate (7) is tungsten; The vacuum distillation was performed at a temperature of 1983 K for 3 hours, with a vacuum level of 0.0067 Pa.

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