High-purity titanium and preparation process and system thereof

Abstract

The invention belongs to the technical field of metal material purification, and discloses high-purity titanium and a preparation process and system thereof. The high-purity titanium preparation equipment comprises an iodine evaporation tank, a low-temperature reactor, a high-temperature reactor, a material conveying pipeline and a communicating pipe, the iodine evaporation tank is communicated with the low-temperature reactor through the material conveying pipeline, the low-temperature reactor is arranged above the high-temperature reactor, and the communicating pipe is communicated with the high-temperature reactor. The low-temperature reactor and the high-temperature reactor are connected through the communicating pipe, the iodine evaporation tank is used for placing an iodine source, the low-temperature reactor is used for placing a crude titanium raw material, and the high-temperature reactor is used for depositing high-purity titanium. By arranging a low-temperature reactor and a high-temperature reactor, an intermediate product titanium iodide and a final product titanium are separately carried out in different spaces, iodination and decomposition reactions are independently controlled in different containers, and by monitoring temperature and pressure parameters in real time, the heat radiation loss of a high-temperature area to a low-temperature area is reduced, and the heating efficiency of the high-temperature area is improved; and the heat loss and the requirement on equipment power are reduced.

Description

Technical Field

[0001] This invention belongs to the field of metal material purification technology, and relates to a process for improving the purity of elemental titanium, specifically to a high-purity titanium and its preparation process and system. Background Technology

[0002] High-purity titanium, due to its excellent physical and chemical properties, has wide applications in high-end fields such as aerospace, electronics and information technology, and biomedicine. For example, in aerospace, high-purity titanium is used to manufacture key components for aircraft to reduce weight and improve structural strength; in electronics and information technology, it is an important material for manufacturing high-performance semiconductor devices; and in biomedicine, it can be used to manufacture medical implants, such as bone screws and joints with extremely high biocompatibility requirements. With the rapid development of these high-end fields, the requirements for the quality and purity of high-purity titanium are becoming increasingly stringent, and the market demand for high-purity titanium is growing daily.

[0003] The preparation methods of high-purity titanium can be divided into chemical refining and physical refining methods. Chemical refining mainly uses chemical reactions such as oxidation, reduction, and complexation to separate impurities, while physical refining utilizes the differences in physical properties between the main metal and impurities to achieve high purity of the main metal.

[0004] To obtain high-purity metallic titanium, chemical methods are typically used first to obtain a metal of a certain purity, followed by physical methods to achieve even higher purity. Currently, widely used processes for preparing high-purity titanium both domestically and internationally include the Kroll process (Mg thermal reduction method), titanium iodide thermal decomposition method, molten salt electrolysis method, and electron beam melting refining method. However, these methods suffer from drawbacks such as low product purity, complex process flows, and high production costs.

[0005] In cutting-edge fields such as semiconductors, the iodination method for producing high-purity titanium remains the dominant technology in the industry. The titanium iodide thermal decomposition method (commonly known as the iodination method) for producing high-purity titanium utilizes the reversible reaction of titanium with halogenating agents in low and high temperature regions, while impurity elements do not participate in the halogenation or decomposition reactions within these temperature ranges, thus achieving the separation of impurities. Currently, the main production systems in use are single-furnace systems. Patent CN100475990A discloses a method and apparatus for producing high-purity titanium, using the same reactor for both the iodination and deposition reactions. To reduce the heat radiation during the decomposition and deposition processes, additional heat exchange equipment is required, resulting in high heat loss and high equipment power requirements.

[0006] Patent CN104141058 A discloses a method and apparatus for producing high-purity titanium, in which two reactors are connected in parallel and the mass transfer process of intermediate products is completed by a gas pump. However, the reaction rates of iodization and deposition decomposition reactions are different at different stages and are not easy to monitor. The gas pump flow rate is difficult to control, resulting in an imbalance in the gas ratio between the synthesis reactor and the decomposition reactor. In addition, the intermediate transmission pipeline and pump body are long, and iodine and titanium iodide vapors are easy to condense and deposit in the pipeline, requiring regular cleaning and maintenance, which increases maintenance costs. Both of the above methods are intermittent production with low production efficiency. Summary of the Invention

[0007] In view of the defects and deficiencies of the existing technology, the present invention provides, firstly, an apparatus for preparing high-purity titanium; secondly, a method for preparing high-purity titanium; and thirdly, a high-purity titanium.

[0008] In a first aspect, the present invention provides a high-purity titanium preparation apparatus, comprising an iodine evaporator, a low-temperature reactor, a high-temperature reactor, a feed pipeline, and a connecting pipe. The iodine evaporator and the low-temperature reactor are connected through the feed pipeline. The low-temperature reactor is disposed above the high-temperature reactor. The low-temperature reactor and the high-temperature reactor are connected through the connecting pipe. The iodine evaporator is used to hold an iodine source. The low-temperature reactor is used to hold crude titanium raw materials. The high-temperature reactor is used to deposit high-purity titanium.

[0009] Preferably, the two ends of the connecting pipe are connected to the bottom of the low-temperature reactor and the top of the high-temperature reactor, respectively.

[0010] Preferably, the connecting pipe is provided with two vacuum valves, which are respectively located at the upper and lower parts of the connecting pipe.

[0011] Preferably, the low-temperature reactor and the high-temperature reactor are detachably connected.

[0012] Preferably, the equipment for preparing high-purity titanium further includes a condensation recovery tank and an iodine recovery connecting pipe, wherein the condensation recovery tank is detachably connected to the high-temperature reactor via the iodine recovery connecting pipe.

[0013] Preferably, the iodine evaporator, the low-temperature reactor, and the high-temperature reactor are provided with a shell, an insulation layer, and a heating wire layer in sequence from the outside to the inside, and the shell, the insulation layer, and the heating wire layer are arranged in sequence from the outer layer to the inner layer.

[0014] Preferably, the cryogenic reactor is provided with a mesh cover, which is disposed inside the heating wire layer, and a storage space is provided between the mesh cover and the heating wire layer.

[0015] Preferably, the mesh cover is arranged in a ring shape.

[0016] Preferably, the equipment for preparing high-purity titanium further includes a vacuum device and a vacuum tube, wherein the vacuum tube is disposed on the vacuum device, and the vacuum device can evacuate the iodine evaporator, the high-temperature reactor, and the low-temperature reactor.

[0017] Preferably, the reaction chamber of the high-temperature reactor is further provided with a heating wire, which is a high-purity titanium wire.

[0018] Preferably, the material conveying pipe is a heat tracing pipe.

[0019] Secondly, the present invention provides a method for preparing high-purity titanium, using the above-mentioned preparation equipment.

[0020] Preferably, the method for preparing the high-purity titanium includes: Solid iodine raw material is heated under vacuum, and the resulting iodine vapor enters a low-temperature reactor. At the same time, crude titanium in the low-temperature reactor is heated under vacuum, and titanium iodide vapor is generated in the low-temperature reactor. The titanium iodide vapor flows downward into a high-temperature reactor and is heated to generate iodine vapor and high-purity titanium. The iodine vapor flows upward into the low-temperature reactor to participate in the circulation, and the high-purity titanium is deposited on the heating wire layer of the high-temperature reactor.

[0021] Preferably, the iodine raw material is high-purity iodine; the crude titanium is sponge titanium.

[0022] Preferably, the heating temperature of solid iodine is 100~150℃, the heating temperature in the low-temperature reactor is 200~700℃, and the heating temperature in the high-temperature reactor is 1000~1400℃.

[0023] Preferably, the process also includes a recovery step, in which the high-temperature reactor and the low-temperature reactor are separated when a certain amount of high-purity titanium is deposited, and then the high-temperature reactor is connected to a condensation recovery tank to recover titanium iodide vapor and iodine vapor from the high-temperature reactor.

[0024] Thirdly, the present invention provides a high-purity titanium, which is prepared by the above-described method.

[0025] Compared with the prior art, the present invention has the following significant advantages: (1) This invention provides a novel, easy-to-operate preparation equipment and process that improves reaction continuity, optimizes iodine cycle efficiency, reduces equipment maintenance costs, and improves energy utilization. It effectively solves the key technical problems of low efficiency and serious iodine loss in the prior art. Furthermore, the preparation equipment provided by this invention can be recycled and replaced to achieve uninterrupted production and improve production efficiency. In addition, the combination of the equipment and process provided by this invention can improve product purity and has good engineering application prospects and industrialization potential.

[0026] (2) The preparation equipment provided by the present invention separates the intermediate product titanium iodide and the final product titanium in different spaces (low temperature reactor and high temperature reactor) by setting up a low temperature reactor and a high temperature reactor. The iodination and decomposition reactions are controlled independently in separate containers. By monitoring the temperature and pressure parameters in real time, the heat radiation loss of the high temperature zone to the low temperature zone is reduced, the heating efficiency of the high temperature zone is improved, and the heat loss and power requirements of the equipment are reduced.

[0027] (3) The low-temperature reactor and high-temperature reactor provided by the present invention are arranged vertically, with a short-distance heat tracing pipeline design in the middle: the synthesis reactor and the decomposition reactor are compactly integrated, the conveying distance is shortened to within 1m, and the risk of deposition is reduced. In addition, the gravity-driven + temperature difference circulation method eliminates the need for a gas pump and utilizes the height difference and temperature gradient between the reactors to achieve natural gas circulation.

[0028] (4) The production system provided by the present invention condenses and recovers intermediate products titanium iodide and iodine vapor during product recycling. In the later stage of the reaction, a condensation recovery tank is used to condense and recover iodine and titanium iodide in the high-temperature zone, thereby reducing raw material loss and production costs. It is expected that the implementation of this technology will bring significant economic benefits and improve the competitiveness of enterprises in the high-purity titanium market. Attached Figure Description

[0029] Figure 1 A schematic diagram of the overall structure of the high-purity titanium preparation equipment provided by the present invention; Figure 2 The schematic diagram of the cold energy recovery tank is included in the high-purity titanium preparation equipment provided by this invention.

[0030] Reference numerals: 1. Iodine evaporator; 2. Low-temperature reactor; 3. High-temperature reactor; 4. Feeding pipeline; 5. Connecting pipe; 501. Low-temperature section; 502. Vacuum tube three; 503. High-temperature section; 6. Vacuum pipeline one; 7. Vacuum valve one; 8. Iodine addition valve; 9. Pressure vacuum gauge; 10. Vacuum pipeline two; 11. Vacuum valve two; 12. Vacuum valve three; 13. Vacuum valve four; 14. Heating wire layer; 15. Insulation cotton layer; 16. Mesh cover; 17. Heating wire; 18. Condensation recovery tank; 19. Iodine recovery connecting pipe. Detailed Implementation

[0031] The present invention provides the following specific technical solutions.

[0032] In a first aspect, the present invention provides a high-purity titanium preparation apparatus, comprising an iodine evaporator, a low-temperature reactor, a high-temperature reactor, a feed pipeline, and a connecting pipe. The iodine evaporator and the low-temperature reactor are connected through the feed pipeline. The low-temperature reactor is disposed above the high-temperature reactor. The low-temperature reactor and the high-temperature reactor are connected through the connecting pipe. The iodine evaporator is used to hold an iodine source. The low-temperature reactor is used to hold crude titanium raw materials. The high-temperature reactor is used to deposit high-purity titanium.

[0033] To address the problems of high heat loss, high equipment requirements, intermittent production, and even greater heat loss in existing high-purity titanium preparation technologies, the inventors have proposed the preparation equipment provided by this invention. First, by setting up a low-temperature reactor and a high-temperature reactor, the intermediate product titanium iodide and the final product titanium are separated into different spaces (low-temperature reactor and high-temperature reactor). The iodination and decomposition reactions are independently controlled in separate containers. By monitoring temperature and pressure parameters in real time, the heat radiation loss from the high-temperature zone to the low-temperature zone is reduced, the heating efficiency of the high-temperature zone is improved, and the heat loss and power requirements of the equipment are reduced.

[0034] Furthermore, the layout of the cryogenic and high-temperature reactors is optimized. Titanium iodide vapor is synthesized in the cryogenic reactor, and then decomposes in the high-temperature reactor to obtain elemental titanium and iodine vapor. In other words, titanium iodide vapor is synthesized in the cryogenic reactor, and iodine vapor is generated in the high-temperature reactor. The cryogenic reactor is set above the high-temperature reactor. Utilizing the density difference between titanium iodide vapor and iodine vapor and the temperature gradient between the upper and lower reactors, titanium iodide vapor enters the high-temperature reactor from the cryogenic reactor from top to bottom, while iodine vapor in the high-temperature reactor enters the high-temperature reactor from bottom to top to participate in the cycle again.

[0035] Finally, the equipment provided by this invention combines multiple reactors in the iodization reaction stage, thermal decomposition stage, cooling and discharging stage, and charging stage to improve production efficiency.

[0036] Preferably, the two ends of the connecting pipe are connected to the bottom of the low-temperature reactor and the top of the high-temperature reactor, respectively.

[0037] Preferably, the connecting pipe is provided with two vacuum valves, which are respectively located at the upper and lower parts of the connecting pipe.

[0038] Preferably, the low-temperature reactor and the high-temperature reactor are detachably connected.

[0039] Preferably, the equipment for preparing high-purity titanium further includes a condensation recovery tank and an iodine recovery connecting pipe, wherein the condensation recovery tank is detachably connected to either the high-temperature reactor or the low-temperature reactor via the iodine recovery connecting pipe.

[0040] By setting up a condensation recovery tank, after the high-temperature reactor is split up and before the high-purity titanium is removed, the high-temperature reactor and the condensation recovery tank are connected through an iodine recovery connection pipe to recover the iodine vapor and titanium iodide vapor in the high-temperature reactor. The recovered material can be used as raw material to participate in the reaction again. Similarly, after the crude titanium raw material in the low-temperature reactor is consumed, the low-temperature reactor can be split up. First, the iodine vapor and titanium iodide vapor in the low-temperature reactor are recovered using the condensation recovery tank, and then the crude titanium raw material is added to the low-temperature reactor.

[0041] Preferably, the iodine evaporator, the low-temperature reactor, and the high-temperature reactor are provided with a shell, an insulation layer, and a heating wire layer in sequence from the outside to the inside, and the shell, the insulation layer, and the heating wire layer are arranged in sequence from the outer layer to the inner layer.

[0042] Preferably, the cryogenic reactor is provided with a mesh cover, which is disposed inside the heating wire layer, and a storage space is provided between the mesh cover and the heating wire layer.

[0043] Preferably, the mesh cover is arranged in a ring shape.

[0044] Preferably, the equipment for preparing high-purity titanium further includes a vacuum device and a vacuum tube, wherein the vacuum tube is disposed on the vacuum device, and the vacuum device can evacuate the iodine evaporator, the high-temperature reactor, and the low-temperature reactor.

[0045] Preferably, the reaction chamber of the high-temperature reactor is further provided with a heating wire, which is a high-purity titanium wire.

[0046] In existing technologies for producing high-purity titanium using the iodination method, high-purity titanium tubes are typically used as deposition tubes, requiring a separation process between the product and the deposition tube during product collection. The inventors discovered that using titanium wire as the deposition substrate allows for simple cleaning and drying of the resulting product. In contrast, titanium tubes have the potential for closed pores on their inner walls (which hinders the diffusion of iodine and titanium iodide), easily leaving residual iodine and titanium iodide that is difficult to remove during cleaning, affecting subsequent use. This invention uses high-purity titanium wire as both the heating element and the deposition substrate. The heating wire and product are collected and processed together, simplifying the process and improving product recovery rate and purity.

[0047] Preferably, the material conveying pipe is a heat tracing pipe.

[0048] In existing technologies, iodine vapor is typically transported via air pumps in conveying pipelines. Firstly, the high-temperature iodine vapor corrodes the pump's flow components, leading to mechanical and chemical corrosion on the surface, resulting in high manufacturing and maintenance costs for corrosion protection. Furthermore, there is a risk of iodine vapor leakage, polluting the surrounding environment. Secondly, the iodination and deposition / decomposition reactions occur at different stages, making the process complex and difficult to control accurately. This results in: an imbalance in the gas ratio between the synthesis and decomposition reactors; and fluctuations in the TiI4 decomposition rate, affecting the uniformity of titanium deposition. Thirdly, the long and complex conveying pipelines cause a drop in iodine vapor temperature, leading to iodine and iodide deposits on the pipelines and pumps, causing blockages. These deposits require weekly shutdowns for cleaning, reducing the equipment's continuous operation rate. Through research, the inventors discovered that by using a gravity-driven + temperature difference circulation method, the gas pump can be eliminated, and the natural circulation of gas can be achieved by utilizing the height difference and temperature gradient between reactors. Furthermore, a heat tracing pipe is used as a material conveying pipeline to ensure the temperature of iodine vapor. Driven by the gas pressure in the iodine evaporator, the iodine vapor moves into the low-temperature reactor, avoiding heat loss of iodine vapor and the introduction of external impurities, thus ensuring the purity of high-purity titanium.

[0049] Secondly, the present invention provides a method for preparing high-purity titanium, using the above-mentioned preparation equipment.

[0050] Preferably, the method for preparing the high-purity titanium includes: Solid iodine raw material is heated under vacuum, and the resulting iodine vapor enters a low-temperature reaction reactor. At the same time, crude titanium in the low-temperature reactor is heated under vacuum, and titanium iodide vapor is generated in the low-temperature reactor. The titanium iodide vapor flows downward into a high-temperature reactor and is heated to generate iodine vapor and high-purity titanium. The iodine vapor flows upward into the low-temperature reactor to participate in the circulation, and the high-purity titanium is deposited on the heating wire (high-purity titanium wire) of the high-temperature reactor.

[0051] Preferably, the iodine raw material is high-purity iodine; the crude titanium is sponge titanium.

[0052] Preferably, the heating temperature of solid iodine is 100~150℃, the heating temperature in the low-temperature reactor is 200~700℃, and the heating temperature in the high-temperature reactor is 1000~1400℃.

[0053] In actual production, the heating temperature of solid iodine can be 100℃, 110℃, 120℃, 130℃, 140℃, or 150℃. The heating temperature in the low-temperature reactor can be 200℃, 250℃, 300℃, 350℃, 400℃, 450℃, 500℃, 550℃, 600℃, 650℃, or 700℃. The heating temperature in the high-temperature reactor can be 1000℃, 1050℃, 1100℃, 1150℃, 1200℃, 1250℃, 1300℃, 1350℃, or 1400℃.

[0054] Preferably, the process also includes a recovery step, in which the high-temperature reactor and the low-temperature reactor are separated when a certain amount of high-purity titanium is deposited, and then the high-temperature reactor is connected to a condensation recovery tank to recover titanium iodide vapor and iodine vapor from the high-temperature reactor.

[0055] Thirdly, the present invention provides a high-purity titanium, which is prepared by the above-described preparation equipment or the above-described preparation method.

[0056] To make the technical problems, technical solutions and technical advantages of the present invention clearer, a detailed description will be given below with reference to specific examples. However, the scope of protection of the present invention is not limited to the following specific embodiments.

[0057] Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by those skilled in the art. The technical terms used herein are for the purpose of describing particular embodiments only and are not intended to limit the scope of the invention.

[0058] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.

[0059] Example 1: To address the problems of high heat loss, high equipment requirements, intermittent production, and even greater heat loss in existing high-purity titanium preparation technologies, the inventors have proposed a high-purity titanium preparation device, referencing... Figure 1 It includes an iodine evaporator 1, a low-temperature reactor 2, a high-temperature reactor 3, a conveying pipeline 4, a connecting pipe 5, a vacuum device and a vacuum extraction pipe, with the vacuum extraction pipe installed on the vacuum device.

[0060] The top of the iodine evaporator 1 is equipped with a vacuum pipe 6, which is used to connect to a vacuum pumping tube. After solid iodine raw material is added to the iodine evaporator 1, a vacuum device is used to extract the gas from the iodine evaporator 1 to provide a vacuum atmosphere. A vacuum valve 7 is installed on the vacuum pipe 6, which is used to open and close the vacuum pipe 6.

[0061] Iodine evaporator 1 and low-temperature reactor 2 are connected by a conveying pipe 4. An iodine valve 8 is installed on the conveying pipe 4 to open and close the conveying pipe 4.

[0062] The cryogenic reactor 2 is equipped with a vacuum pipe 2 10 and a vacuum valve 2 11. Both the cryogenic reactor 2 and the high-temperature reactor 3 are equipped with only a pressure-vacuum gauge 9, which is used to measure the vacuum level in the cryogenic reactor 2. The vacuum pipe 2 10 is connected to the cryogenic reactor 2, and the vacuum valve 2 11 is installed on the vacuum pipe 2 10. The vacuum valve 2 11 is used to open and close the vacuum pipe 2 10. After closing the iodine addition valve 8, the vacuum tube is connected to the vacuum valve 2 11, and then the vacuum equipment is started to extract the gas in the cryogenic reactor 2 and provide a vacuum atmosphere.

[0063] A cryogenic reactor 2 is positioned above a high-temperature reactor 3. The cryogenic reactor 2 and the high-temperature reactor 3 are connected by a connecting pipe 5, with both ends of the connecting pipe 5 connected to the bottom of the cryogenic reactor 2 and the top of the high-temperature reactor 3, respectively. The cryogenic reactor 2, the connecting pipe 5, and the high-temperature reactor 3 are arranged vertically from top to bottom. A vacuum valve 3 12 and a vacuum valve 4 13 are installed on the connecting pipe 5, with the vacuum valve 3 12 positioned above the vacuum valve 4 13. In a specific embodiment of the invention, the connecting pipe 5 includes a cryogenic section 501, a high-temperature section 503, and a vacuum valve 3 502, arranged sequentially from top to bottom. The cryogenic section 501, vacuum valve 3 502, and high-temperature section 503 are connected. The top of the cryogenic section 501 is fixedly connected to and communicates with the cryogenic reactor 2, and the bottom of the high-temperature section 503 is fixedly connected to and communicates with the high-temperature reactor 3. Vacuum valve 3 12 is installed on the cryogenic section 501, and vacuum valve 4 13 is installed on the high-temperature section 503. Vacuum valve 312 and vacuum valve 413 are vacuum butterfly valves.

[0064] The low-temperature section 501 and vacuum tube 3 502, and the high-temperature section 503 and vacuum tube 3 502 are connected by flange structures. Specifically, a flange is fixedly connected to the lower end of the low-temperature section 501, flanges are fixedly connected to both ends of the vacuum tube 3 502, and a flange is fixedly connected to the top end of the high-temperature section 503. The flanges of the low-temperature section 501 and the upper flange of the vacuum tube 3 502 are fixed with screws, and the flanges of the high-temperature section 503 and the lower flange of the vacuum tube 3 502 are fixed with screws. In order to improve the sealing performance, a sealing ring is provided between the two flanges that are in contact with each other. The structure of the connecting pipe 5 facilitates the disassembly and assembly of the high-temperature reactor 3 and the low-temperature reactor 2.

[0065] When evacuating the high-temperature reactor 3, close vacuum valve 312 and open vacuum valve 413 to connect vacuum tube 3502 with the high-temperature reactor 3. Then connect the vacuum tube and vacuum tube 3502, start the vacuum equipment, and extract the gas from the high-temperature reactor 3.

[0066] The iodine evaporator 1, the low-temperature reactor 2, and the high-temperature reactor 3 all contain a heating wire layer 14 and a heat insulation cotton layer 15. The heat insulation cotton layer 15 and the heating wire layer 14 are arranged sequentially from the outer layer to the inner layer. Taking the iodine evaporator 1 as an example, the heat insulation cotton layer 15 is arranged inside the shell of the iodine evaporator 1 and is attached to the shell of the iodine evaporator 1. The heating wire layer 14 is arranged inside the heat insulation cotton layer 15 and is attached to the heat insulation cotton layer 15.

[0067] In addition, a mesh cover 16 is installed inside the low-temperature reactor 2. The mesh cover 16 is located inside the heating wire layer 14 and is arranged in a ring shape. A storage space is provided between the mesh cover 16 and the heating wire layer 14 for placing crude titanium raw materials. A heating wire 17 is also installed in the reaction chamber of the high-temperature reactor 3. The heating wire 17 is used to deposit high-purity titanium. The heating wire 17 is a high-purity titanium wire and serves as both a heating element and a deposition substrate. The heating wire and the product (high-purity titanium) are collected and processed together without separation, simplifying the process and improving product recovery rate and purity.

[0068] It also includes a condensation recovery tank 18 and an iodine recovery connecting pipe 19. The condensation recovery tank 18 is detachably connected to either the high-temperature reactor 3 or the low-temperature reactor 2 via the iodine recovery connecting pipe 19. By setting up the condensation recovery tank 18, after the high-temperature reactor 3 is disassembled and before the high-purity titanium is removed, the high-temperature reactor 3 and the condensation recovery tank 18 are connected through the iodine recovery connecting pipe 19 to recover the iodine vapor and titanium iodide vapor in the high-temperature reactor 3. The recovered material can be used as raw material to participate in the reaction again. Similarly, after the crude titanium raw material in the low-temperature reactor 2 is consumed, the low-temperature reactor 2 can be disassembled. The iodine vapor and titanium iodide vapor in the low-temperature reactor 2 are first recovered using the condensation recovery tank 18, and then the crude titanium raw material is added to the low-temperature reactor 2.

[0069] In practical applications, after separating high-temperature reactor 3, another high-temperature reactor 3 already equipped with high-purity titanium wire can be immediately installed and put into production. The separated high-temperature reactor 3 can be placed in the cooling zone for natural cooling, and then iodine vapor and titanium iodide vapor are recovered through the condensation recovery tank 18. Similarly, when the crude titanium raw material in low-temperature reactor 2 is consumed, the separated low-temperature reactor 2 can be placed in the cooling zone for natural cooling, and another low-temperature reactor 2 already filled with crude titanium raw material can be immediately installed and put into production. Generally, multiple sets of preparation equipment are set up simultaneously on the production line. Only one set of high-temperature reactor 3 and low-temperature reactor 2 needs to be prepared as a backup, which can be cyclically replaced to achieve uninterrupted production and improve production efficiency.

[0070] The working process of the above-mentioned high-purity titanium preparation equipment is as follows: S1. Preparation: Add solid iodine to iodine evaporator 1 and crude titanium raw material to the storage space of cryogenic reactor 2; then close iodine valve 8, open vacuum valve 1 7, use vacuum equipment to extract the gas from iodine evaporator 1, and then close vacuum valve 1 7; then close vacuum valve 3 12, open vacuum valve 2 11, use vacuum equipment to extract the gas from cryogenic reactor 2, and then close vacuum valve 2 11; then open vacuum valve 4 13, use vacuum equipment to extract the gas from high-temperature reactor 3, and then close vacuum valve 4 13; then open iodine valve 8, vacuum valve 3 12 and vacuum valve 4 13 to complete the preparation.

[0071] S2. Synthesize high-purity titanium. Start iodine evaporator 1, cryogenic reactor 2 and high-temperature reactor 3. Solid iodine sublimates into iodine vapor and enters cryogenic reactor 2 through a conveying pipe. The iodine vapor reacts with the crude titanium raw material in cryogenic reactor 2 to synthesize titanium iodide vapor. The titanium iodide vapor flows downward along connecting pipe 5 into high-temperature reactor 3, where it decomposes into iodine vapor and high-purity titanium. The high-purity titanium is deposited on high-purity titanium wire 17 in high-temperature reactor 3. The iodine vapor in high-temperature reactor 3 flows upward along connecting pipe 5 into cryogenic reactor 2 and participates in the cycle again.

[0072] Example 2: A method for preparing high-purity titanium, using the high-purity titanium preparation equipment provided in Example 1 above, includes the following steps: heating solid iodine raw material under vacuum at a temperature of 125°C, and the resulting iodine vapor entering a low-temperature reaction reactor; simultaneously heating crude titanium in the low-temperature reactor under vacuum at a temperature of 550°C, and the iodine vapor and crude titanium generating titanium iodide vapor; the titanium iodide vapor flowing downwards into a high-temperature reactor and being heated at a temperature of 1200°C, whereby the titanium iodide vapor decomposes to generate iodine vapor and high-purity titanium, and the iodine vapor flowing upwards into the low-temperature reactor to participate in the circulation, and the high-purity titanium being deposited on the heating wire (high-purity titanium wire) of the high-temperature reactor.

[0073] Example 3: A method for preparing high-purity titanium, using the high-purity titanium preparation equipment provided in Example 1 above, includes the following steps: heating solid iodine raw material under vacuum atmosphere at a heating temperature of 100°C, and the resulting iodine vapor entering a low-temperature reaction reactor; simultaneously heating crude titanium in the low-temperature reactor under vacuum atmosphere at a heating temperature of 500°C, and the iodine vapor and crude titanium generating titanium iodide vapor; the titanium iodide vapor flowing downwards into a high-temperature reactor and being heated at a heating temperature of 1100°C, whereby the titanium iodide vapor decomposes to generate iodine vapor and high-purity titanium, and the iodine vapor flowing upwards into the low-temperature reactor to participate in the circulation, and the high-purity titanium being deposited on the heating wire (high-purity titanium wire) of the high-temperature reactor.

[0074] Example 4: A method for preparing high-purity titanium, using the high-purity titanium preparation equipment provided in Example 1 above, includes the following steps: heating solid iodine raw material under vacuum at a temperature of 150°C, and the resulting iodine vapor entering a low-temperature reaction reactor; simultaneously heating crude titanium in the low-temperature reactor under vacuum at a temperature of 600°C, and the iodine vapor and crude titanium generating titanium iodide vapor; the titanium iodide vapor flowing downwards into a high-temperature reactor and being heated at a temperature of 1300°C, whereby the titanium iodide vapor decomposes to generate iodine vapor and high-purity titanium, and the iodine vapor flowing upwards into the low-temperature reactor to participate in the circulation, and the high-purity titanium being deposited on the heating wire (high-purity titanium wire) of the high-temperature reactor.

[0075] Comparative Example 1: A method for preparing high-purity titanium, using a high-purity titanium production apparatus provided by existing technology (the production apparatus can be found in patent CN100475990A). The high-purity titanium production apparatus includes a reaction vessel in which the iodination reaction and the deposition reaction are carried out.

[0076] The production steps include: Iodine vapor is fed into a vacuum-sealed reaction vessel (1). The crude titanium raw material (8) in the metal mesh ring (7) on the inner wall of the vessel is heated to 550°C. The titanium iodide gas comes into contact with the high-temperature deposition tube (3) and undergoes thermal decomposition. The working temperature of the surface of the high-temperature deposition tube (3) is 1200°C. The iodine vapor released by thermal decomposition reacts with the titanium raw material in a cycle to generate titanium iodide. The dense high-purity titanium generated by thermal decomposition is continuously deposited on the surface of the high-temperature deposition tube (3) to form a tubular high-purity titanium shell. The tubular high-purity titanium shell is peeled off to obtain tubular high-purity titanium.

[0077] Comparative Example 2: A method for preparing high-purity titanium, using a high-purity titanium production apparatus provided by existing technology (the production apparatus can be found in patent CN104141058A). The high-purity titanium production apparatus includes a raw material tank and a deposition tank, which are arranged horizontally. The upper part of the raw material tank and the upper part of the deposition tank are connected by a first pipe, and the lower part of the raw material tank and the lower part of the deposition tank are connected by a second pipe. Both the first and second pipes are equipped with air pumps.

[0078] The iodination reaction is carried out in the feed tank, and the deposition reaction is carried out in the deposition tank.

[0079] The production steps include: Solid iodine raw material is heated to 125°C under vacuum, and the resulting iodine vapor enters the raw material tank under the action of a gas pump. At the same time, crude titanium in the raw material tank is heated to 550°C under vacuum, and the iodine vapor and crude titanium generate titanium iodide vapor. The titanium iodide vapor enters the deposition tank through a second pipe under the action of a gas pump. The deposition tank is heated to 1200°C, and the titanium iodide vapor decomposes to generate iodine vapor and high-purity titanium. The iodine vapor enters the raw material tank through a first pipe to participate in the circulation, and the high-purity titanium is deposited on the titanium deposition tube of the raw material tank.

[0080] The purity of the high-purity titanium obtained in Examples 2-4 and Comparative Examples 1-2 was tested, and the production cycle of Examples 2-4 and Comparative Examples 1-2 was also tested. The volume of the reaction vessel in Comparative Example 1 was the same as the sum of the volumes of the low-temperature reactor and the high-temperature reactor in Example 2. The volume of the raw material tank in Comparative Example 2 was the same as the volume of the high-temperature reactor in Example 2. The volume of the deposition tank in Comparative Example 2 was the same as the volume of the low-temperature reactor in Example 2. The production efficiency was calculated, and the data are as follows: Table 1. Purity and production efficiency of high-purity titanium obtained in Examples 2-4 and Comparative Examples 1-2. As shown in Table 1, the purity of the high-purity titanium obtained by the preparation equipment and process provided by the present invention is further improved. Comparative analysis of Examples 2-4 reveals that in Example 2, the iodination and deposition reactions reach equilibrium under the proposed reaction conditions, resulting in high yield and purity. In Example 3, the iodination and deposition reactions occur at lower temperatures, affecting production efficiency. In Example 4, the iodination and deposition reactions occur at higher temperatures, improving the yield; however, the increased iodination temperature easily introduces impurities, affecting the purity of the high-purity titanium, thus causing a slight decrease in purity of the sample obtained in Example 4 compared to the sample obtained in Example 2.

[0081] Comparing the data from Example 2 and Comparative Example 1, the inventors propose that the preparation process provided by this invention achieves equilibrium between the iodization reaction and deposition. The temperature in the high-temperature reactor is directly proportional to the amount of iodine evaporation. A moderate amount of iodine evaporation maintains a stable iodine vapor concentration, promoting continuous deposition in the low-temperature reactor and improving the raw material conversion rate. In contrast, in Comparative Example 1, both the evaporation and deposition reactions occur in the same reactor, significantly impacting production efficiency. Furthermore, the high-temperature zone's thermal radiation affects the low-temperature zone's reaction temperature control, requiring frequent adjustments. This typically results in a long production cycle for high-purity titanium. Additionally, the overheating of the iodization reaction introduces impurities. Therefore, Comparative Example 1 has limited production efficiency, and the resulting high-purity titanium sample has low purity.

[0082] Based on the data from Comparative Example 2 and Comparative Example 2, the inventors proposed that: Adding an air pump to the connecting pipe of the dual reaction tanks used in Comparative Example 2 enhances the transmission efficiency of reactants and products to a certain extent, thus promoting production efficiency. Therefore, Comparative Example 2 has higher efficiency. However, in actual production, controlling the air pump blowing rate is difficult. Iodization and decomposition / deposition reactions are complex processes that cannot be detected. The reaction rates of iodization and deposition / decomposition reactions differ at different stages. Traditional flow meters have limited accuracy, and their accuracy decreases with increasing working time. Controlling the air pump flow rate is difficult, leading to an imbalance in the gas ratio between the synthesis reactor and the decomposition reactor, fluctuations in the titanium iodide decomposition rate, and affecting the uniformity of titanium deposition. Furthermore, the cost of metal plating materials, maintenance costs, and high power requirements associated with using an air pump are all detrimental to the commercialization of the product.

[0083] The above-described embodiments are merely preferred embodiments of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the technical scope of the present invention, based on the technical solution and concept of the present invention, should be covered within the scope of protection of the present invention.

Claims

1. A device for preparing high-purity titanium, characterized in that, The system includes an iodine evaporator (1), a low-temperature reactor (2), a high-temperature reactor (3), a feed pipe (4), and a connecting pipe (5). The iodine evaporator (1) and the low-temperature reactor (2) are connected through the feed pipe (4). The low-temperature reactor (2) is located above the high-temperature reactor (3). The low-temperature reactor (2) and the high-temperature reactor (3) are connected through the connecting pipe (5). The iodine evaporator (1) is used to place the iodine source. The low-temperature reactor (2) is used to place the crude titanium raw material. The high-temperature reactor (3) is used to deposit high-purity titanium.

2. The equipment for preparing high-purity titanium as described in claim 1, characterized in that, It also includes a condensation recovery tank (18) and an iodine recovery connecting pipe (19), wherein the condensation recovery tank (18) is detachably connected to the high-temperature reactor (3) via the iodine recovery connecting pipe (19).

3. The equipment for preparing high-purity titanium as described in claim 1, characterized in that, The iodine evaporator (1), the low-temperature reactor (2), and the high-temperature reactor (3) are provided with a shell, a heat insulation cotton layer (15), and a heating wire layer (14) from the outside to the inside, and the shell, the heat insulation cotton layer (15), and the heating wire layer (14) are arranged from the outer layer to the inner layer.

4. The equipment for preparing high-purity titanium as described in claim 2, characterized in that, The low-temperature reactor (2) is provided with a mesh cover (16), which is located inside the heating wire layer (14). A storage space is provided between the mesh cover (16) and the heating wire layer (14). The mesh cover (16) is arranged in a ring shape.

5. The equipment for preparing high-purity titanium as described in claim 1, characterized in that, The high-temperature reactor (3) is also equipped with a heating wire (17) in its reaction chamber. The heating wire (17) is a high-purity titanium wire.

6. The equipment for preparing high-purity titanium as described in claim 1, characterized in that, The two ends of the connecting pipe (5) are respectively connected to the bottom end of the low-temperature reactor (2) and the top end of the high-temperature reactor (3); two vacuum valves are provided on the connecting pipe (5), and the two vacuum valves are respectively located at the upper and lower parts of the connecting pipe (5); the low-temperature reactor (2) and the high-temperature reactor (3) are detachably connected; The equipment for preparing high-purity titanium also includes a vacuum device and a vacuum tube. The vacuum tube is installed on the vacuum device, and the vacuum device can evacuate the iodine evaporator (1), the high-temperature reactor (3), and the low-temperature reactor (2).

7. A method for preparing high-purity titanium, characterized in that, The preparation equipment described in any one of claims 1 to 6 is used; the method for preparing high-purity titanium includes: heating solid iodine raw material under vacuum atmosphere, and the resulting iodine vapor entering a low-temperature reaction reactor; heating crude titanium in the low-temperature reactor (2) under vacuum atmosphere, and the iodine vapor reacts with the crude titanium in the low-temperature reactor (2) to generate titanium iodide vapor; the titanium iodide vapor flows downward into the high-temperature reactor (3) and is pyrolyzed to generate iodine vapor and high-purity titanium, the iodine vapor flows upward into the low-temperature reactor (2) to participate in the circulation, and the high-purity titanium is deposited on the heating wire layer (14) of the high-temperature reactor (3).

8. The method for preparing high-purity titanium as described in claim 7, characterized in that, The iodine raw material is high-purity iodine; the crude titanium is sponge titanium; the heating temperature of the solid iodine raw material is 100~150℃; the heating temperature in the low-temperature reactor (2) is 200~700℃; the heating temperature in the high-temperature reactor (3) is 1000~1400℃.

9. The method for preparing high-purity titanium as described in claim 7 or 8, characterized in that, It also includes a recycling process. When high-purity titanium is deposited to a certain amount, the high-temperature reactor (3) and the low-temperature reactor (2) are separated. Then, the high-temperature reactor (3) is connected to the condensation recovery tank (18) to recover titanium iodide vapor and iodine vapor in the high-temperature reactor (3).

10. A high-purity titanium, characterized in that, It is prepared by the preparation method according to any one of claims 7 to 9.

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