Process for reducing titanium sponge iron with oxygen

Abstract

The application discloses a process for reducing the iron and oxygen of titanium sponge in the technical field of titanium sponge production, which comprises the following steps: cleaning a reactor, assembling a titanium infiltration frame, adding titanium sponge for titanium infiltration, and assembling the reactor; putting the assembled reactor into a distillation furnace, increasing the temperature of the furnace to a certain temperature, and then baking the reactor; increasing the temperature of the distillation furnace to a specified temperature; rapidly increasing the temperature of the distillation furnace after constant temperature, and simultaneously performing vacuumizing to perform first titanium infiltration; taking out the titanium infiltration device after furnace cooling, disassembling the reactor. Assembling the reactor, leak detection after vacuumizing in a reduction furnace, and argon filling. Adding a small amount of liquid magnesium to assemble the reactor, increasing the temperature, and adding a small amount of titanium tetrachloride to perform second titanium infiltration. The reduction, distillation and crushing obtain the titanium sponge. The process in the application can remove the water adsorbed on the surface of the reactor and the large cover after cleaning and the water adsorbed on the surface of titanium used for titanium infiltration, and avoids the influence of oxygen and hydrogen on the titanium infiltration process.

Description

Technical Field

[0001] This invention belongs to the field of sponge titanium production technology, specifically a process for reducing iron and oxygen in sponge titanium. Background Technology

[0002] The presence of impurities in titanium sponge significantly affects its physical, chemical, mechanical, corrosion resistance, and Brinell hardness. The presence of oxygen and nitrogen can cause distortions in the titanium lattice, further impacting its various properties. Brinell hardness is commonly used as a comprehensive indicator of the quality of titanium sponge; higher impurity content results in greater Brinell hardness and lower quality. Different impurities have different effects on the hardness of titanium sponge. Oxygen, nitrogen, carbon, iron, cobalt, and silicon all have a significant impact on hardness, and the effects of several impurities present simultaneously are additive. The relationship between the hardness of titanium sponge and its impurity content is as follows: HB = 158 (% O). 0.5 +196 (%N) 0.5 +45% C 0.5 +20% Fe 0.5 +57. The combined method, namely magnesium reduction-vacuum distillation, for producing sponge titanium faces challenges such as suboptimal reactor titanium diffusion, water absorption by distilled magnesium, and issues with process conditions and product sampling. These problems lead to some sponge titanium products having high levels of impurities like ferrite and oxygen, resulting in reduced product grades and potentially even product scrap. Therefore, clarifying the sources of ferrite and oxygen impurities in sponge titanium products and proposing measures to reduce them, thereby mitigating the impact of ferrite and oxygen impurities on product quality, is one of the key issues that need to be addressed in the combined method for producing sponge titanium.

[0003] In the magnesium-based titanium sponge production process, the reduction of titanium tetrachloride by magnesium is an exothermic reaction. The higher the reduction rate of titanium tetrachloride, the more vigorous the reaction and the greater the heat released, with the temperature in the central reaction region exceeding 1200℃. At high temperatures, on the one hand, the steel reactor contains liquid magnesium, which has a certain solubility in the steel reactor, and the higher the temperature, the greater the solubility. The dissolved iron and the iron on the steel reactor will react chemically with titanium tetrachloride (3TiCl4 + Fe = FeCl3 + 3TiCl3, 3TiCl4 + 2Fe = 2FeCl3 + 3TiCl2, 2FeCl3 + 3Mg = 2Fe + 3MgCl2), ultimately transferring the iron product to the titanium sponge. On the other hand, when rust is present in the reactor, its iron oxide will react chemically with titanium tetrachloride (Fe2O3 + 3TiCl4 = 2FeCl3).

[0004] The reaction ⇌ 3TiOCl₂ to form ferric chloride. This ferric chloride, once in the reaction zone, readily undergoes a reduction reaction (2FeCl₃ + 3Mg = 2Fe + 3MgCl₂), resulting in iron impurities that enter the sponge titanium. This series of reactions can simultaneously introduce both iron and oxygen impurities into the sponge titanium mass, affecting its quality.

[0005] To address the aforementioned technical issues, we propose a process for reducing the oxygen content in sponge titanium iron.

[0006] The information disclosed in this background section is intended only to enhance the understanding of the overall background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0007] The purpose of this invention is to provide a process for reducing the oxygen content in sponge titanium iron, thereby solving the aforementioned problems in the prior art.

[0008] To achieve the above objectives, the present invention provides a process for reducing the oxygen content in sponge titanium iron, comprising the following steps:

[0009] Step 1: Clean the titanium diffusion reactor, add sponge titanium for titanium diffusion, and assemble the titanium diffusion reactor;

[0010] Step 2: The assembled titanium diffusion reactor is placed on the bottom of the heating furnace. Then, the titanium diffusion reactor is sent into the heating furnace through the opening assembly and the lid is closed and sealed. The temperature of the heating furnace is raised to a certain temperature and maintained for 2 hours to bake the titanium diffusion reactor. After baking, the vacuum device is opened and the first valve is opened and the second valve is closed to evacuate and remove the evaporated water vapor while checking the air tightness.

[0011] Step 3: After the sealing is qualified, vacuum is drawn. At the same time, the heating furnace is divided into four zones from top to bottom, and the four zones are heated to the specified temperature and kept at the temperature for 5 hours.

[0012] Step 4: After the temperature is constant, the four areas are rapidly heated to a certain temperature, and at the same time, the air is evacuated by a vacuum device. The temperature is maintained for 25±1h to carry out the first titanium infiltration.

[0013] Step 5: After the first titanium diffusion process is completed, remove the reactor from the furnace for cooling, disassemble the reactor, and take out the titanium diffusion unit;

[0014] Step 6: Assemble the titanium diffusion reactor, place it in the heating furnace to raise the furnace temperature to 200±50℃, maintain for 1 hour, turn on the vacuum device and open the first valve, close the second valve and evacuate the air, then check for leaks. After the check is completed, close the first valve and open the second valve to purge with argon through the argon generator.

[0015] Step 7: Then, a small amount of liquid magnesium is added through the feeding structure, the temperature is raised, a small amount of titanium tetrachloride is added for 1 hour, the feeding is stopped, the temperature is kept constant for 5 hours, and a second titanium diffusion is carried out.

[0016] Step 8: Reduce, distill, and crush to obtain sponge titanium.

[0017] In the technical solution of the present invention, in step 3, the vacuum is evacuated to 2±0.1kPa, and the four regions are simultaneously heated to 950±5℃ at a programmed temperature of 35±1℃ / min and kept at a constant temperature for 10±1h to perform the first titanium infiltration.

[0018] In the technical solution of the present invention, in step 4, the four regions are simultaneously heated to 1085±5℃ at a programmed rate of 15±1℃ / min and held at that temperature for 30±1h.

[0019] In the technical solution of the present invention, in step 7, the amount of liquid magnesium added is 550±50kg, the four regions are simultaneously heated to 850±5℃, and titanium tetrachloride is added at a feed rate of 350±10kg / h for 1h to carry out the second titanium infiltration.

[0020] In the technical solution of the present invention, the bottom surface of the heating furnace is provided with a bottom support, the top surface of the bottom support is provided with a placement groove adapted to the lower half of the titanium diffusion reactor, the top of the heating furnace is provided with a matching sealing furnace cover, the bottom surface of the sealing furnace cover is provided with a sealing ring adapted to the opening size of the top of the titanium diffusion reactor, the bottom surface of the heating furnace is provided with a cover opening assembly, and the top surface of the sealing furnace cover is provided with a feeding structure in the middle.

[0021] In the technical solution of the present invention, the cover opening assembly includes a motor, a shaft structure, and a transmission gear set structure located at the bottom of the central axis on the outer wall of the rear side of the heating furnace. The output end of the motor is connected to the shaft structure, and the shaft structure includes a first shaft. The bottom end of the first shaft is connected to the output end of the motor through a first transmission gear set. The top end of the first shaft is connected to a connecting shaft through a second transmission gear set. The two ends of the connecting shaft pass through the left and right side walls of the heating furnace and are fixedly connected to the left and right inner side walls of the sealed furnace cover.

[0022] In the technical solution of the present invention, the output end of the motor is coaxially connected to a second shaft, the front end of the second shaft is connected to a third shaft symmetrically arranged on the left and right sides by a third transmission gear set, and the outer end of the third shaft is connected to a threaded rod by a fourth transmission gear set.

[0023] In the technical solution of the present invention, the threads on the left and right threaded rods are opposite in direction, the bottom surface of the threaded rods is rotatably connected to the bottom surface of the heating furnace, the bottom surface of the base is provided with threaded grooves symmetrically on the left and right, and the base is threadedly connected to the threaded rods on the same side through the threaded grooves.

[0024] In the technical solution of the present invention, the feeding structure includes a feeding pipe located in the middle of the top surface of the sealed furnace cover. A diverter is provided on the left side inside the feeding pipe. The diverter is in the shape of an inverted umbrella. The top sidewall of the diverter is fixed to the inner wall of the feeding pipe by connecting rods arranged symmetrically on the left and right.

[0025] In the technical solution of the present invention, a vacuum device is provided on the left side of the top surface of the sealed furnace cover, a vacuum tube is provided in the middle of the right side wall of the vacuum device, the other end of the vacuum tube passes through the sealed furnace cover and the connection port is located within the sealing ring, an argon generator is provided on the left side of the rear side of the top surface of the sealed furnace cover, a gas pipe is provided in the middle of the front side wall of the argon generator and communicates with the right end of the vacuum tube, and a first valve and a second valve are respectively provided in the middle section of the vacuum tube and the gas pipe.

[0026] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0027] 1. In this invention, the preheating furnace can remove water adsorbed on the surface of the titanium diffusion reactor and the sealed furnace cover after cleaning, as well as water adsorbed on the surface of the titanium used for titanium diffusion, thus avoiding the influence of oxygen and hydrogen elements on the titanium diffusion process. The second heating furnace after the second heating furnace can remove water adsorbed on the surface of the reactor after the cover is opened, reducing the influence of oxygen and hydrogen elements on the reduction distillation process of sponge titanium, thereby reducing the influence of oxygen elements on the quality of sponge titanium.

[0028] 2. In this invention, titanium diffusion is performed twice. By increasing the number of titanium diffusion cycles, the uniformity of titanium diffusion is improved, the titanium diffusion area and the thickness of the titanium diffusion layer are increased, thereby enhancing the titanium diffusion effect and reducing the impact of iron on the quality of the sponge titanium. The first titanium diffusion process uses high temperature to reach the eutectic point of the titanium-iron alloy, generating a titanium-iron alloy protective layer on the surface of the titanium diffusion reactor, preventing direct contact between iron and titanium. The second titanium diffusion process directly uses the reaction of liquid magnesium and titanium tetrachloride to produce titanium particles, resulting in a new titanium layer on the surface of the titanium diffusion reactor. Through these two titanium diffusion processes, the surface of the titanium diffusion reactor simultaneously possesses both a titanium-iron alloy layer and a titanium layer, completely avoiding contact and reaction between the reacted titanium and iron, thus reducing the impact of iron on the quality of the sponge titanium.

[0029] 3. In this invention, the motor in the cover opening assembly drives the shaft structure and the transmission gear structure to drive the sealing furnace cover to seal while the bottom support sinks down to send the titanium diffusion reactor into the heating furnace, reducing the manpower, material resources and time resources required for repeatedly sending and taking out the titanium diffusion reactor. Attached Figure Description

[0030] Figure 1 This is a simplified schematic diagram of the overall structure of the present invention;

[0031] Figure 2 This is a schematic diagram of the internal structure of the present invention;

[0032] Figure 3 This is a schematic diagram of the opening component structure in this invention;

[0033] Figure 4 This is a cross-sectional view of the sealed furnace cover structure in this invention.

[0034] Explanation of reference numerals in the attached figures:

[0035] 1. Heating furnace;

[0036] 2. Titanium diffusion reactor;

[0037] 3. Sealed furnace cover; 31. Sealing ring;

[0038] 4. Base support;

[0039] 5. Cover opening assembly; 51. Motor; 52. Shaft structure; 521. First shaft; 522. Connecting shaft; 523. Second shaft; 524. Third shaft; 53. Transmission gear structure; 531. First transmission gear set; 532. Second transmission gear set; 533. Third transmission gear set; 534. Fourth transmission gear set; 54. Threaded rod;

[0040] 6. Feeding structure; 61. Feeding inlet; 62. Diverter; 63. Connecting rod;

[0041] 7. Vacuum device; 71. Vacuum tube; 72. First valve;

[0042] 8. Argon generator; 81. Gas pipe; 82. Second valve. Detailed Implementation

[0043] The specific embodiments of the present invention will now be described in detail with reference to the accompanying drawings, but it should be understood that the scope of protection of the present invention is not limited to the specific embodiments.

[0044] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.

[0045] Reference Figures 1-4 The present invention provides a process for reducing the oxygen content in sponge titanium iron, comprising the following embodiments:

[0046] Example 1

[0047] Step 1: Clean the titanium diffusion reactor 2, assemble the titanium diffusion frame, add 550 kg of small-particle titanium sponge, and assemble the titanium diffusion reactor 2.

[0048] Step 2: The assembled titanium diffusion reactor 2 is placed on the base 4 of the heating furnace 1. Then, the titanium diffusion reactor 2 is sent into the heating furnace 1 through the opening assembly 5 and the cover is closed and sealed. The temperature of the heating furnace 1 is raised to 150℃ and maintained for 2 hours to bake the titanium diffusion reactor 2. After baking, the vacuum device 7 is opened and the first valve 72 is opened and the second valve 82 is closed to evacuate and remove the evaporated water vapor while checking the air tightness.

[0049] Step 3: After the sealing is qualified, the vacuum is drawn to 1.9 kPa, and the temperature is increased to 945℃ at a programmed rate of 34℃ / min and kept at the temperature for 9 hours to carry out the first titanium infiltration.

[0050] Step 4: After the temperature is stabilized, rapidly increase the temperature of the four areas simultaneously to 1080℃ at a program speed of 14℃ / min, and stabilize the temperature for 31 hours.

[0051] Step 5: Remove from the furnace and cool for 48 hours; disassemble titanium diffusion reactor 2 and remove the titanium diffusion device.

[0052] Step 6: Assemble the titanium diffusion reactor 2, place it in the heating furnace 1 to raise the furnace temperature to 150℃, maintain it for 1 hour, evacuate and check for leaks, and purge with argon to 100kPa;

[0053] Step 7: After assembling the reactor, add 500 kg of liquid magnesium, heat to 845℃, add titanium tetrachloride at a rate of 340 kg / h for 1 hour, then stop feeding, keep the temperature constant for 5 hours, and carry out secondary titanium infiltration.

[0054] Step 8: Reduce, distill, and crush to obtain sponge titanium.

[0055] Example 2

[0056] Step 1: Clean the titanium diffusion reactor 2, assemble the titanium diffusion frame, add 600 kg of small-particle titanium sponge, and assemble the titanium diffusion reactor 2.

[0057] Step 2: The assembled titanium diffusion reactor 2 is placed on the base 4 of the heating furnace 1. Then, the titanium diffusion reactor 2 is sent into the heating furnace 1 through the opening component 5 and the cover is closed and sealed. The furnace temperature is raised to 200℃ and maintained for 2 hours to bake the titanium diffusion reactor 2. After baking, the steam is evacuated to remove the steam and the air tightness is checked.

[0058] Step 3: After the sealing is qualified, the vacuum is drawn to 2.0 kPa, and the temperature is increased to 950℃ at a programmed rate of 35℃ / min and kept at the temperature for 10 hours to carry out the first titanium infiltration.

[0059] Step 4: After the temperature is constant, rapidly increase the temperature of the four areas simultaneously to 1085℃ at a program speed of 15℃ / min, and hold the temperature for 30 hours.

[0060] Step 5: Remove from the furnace and cool for 48 hours; disassemble titanium diffusion reactor 2 and remove the titanium diffusion device.

[0061] Step 6: Assemble the titanium diffusion reactor 2, place it in the heating furnace 1 to heat the furnace to 20°C, maintain for 1 hour, evacuate and check for leaks, and purge with argon to 100 kPa;

[0062] Step 7: After assembling the titanium diffusion reactor 2, add 550 kg of liquid magnesium, heat to 850℃, add titanium tetrachloride at a feed rate of 350 kg / h for 1 hour, then stop feeding, keep the temperature constant for 5 hours, and carry out the second titanium diffusion.

[0063] Step 8: Reduce, distill, and crush to obtain sponge titanium.

[0064] Example 3

[0065] Step 1: Clean the titanium infiltration reactor 2, assemble the titanium infiltration frame, add 650 kg of small-particle titanium sponge, and assemble the reactor;

[0066] Step 2: The assembled titanium diffusion reactor 2 is placed on the base 4 of the heating furnace 1. Then, the titanium diffusion reactor 2 is sent into the heating furnace 1 through the opening assembly 5 and the cover is closed and sealed. The furnace temperature is raised to 250℃ and maintained for 2 hours to dry the reactor. After drying, the steam is evacuated to remove the steam and the airtightness is checked.

[0067] Step 3: After the sealing is qualified, the vacuum is drawn to 2.1 kPa, and the temperature is simultaneously increased to 945℃ at a programmed rate of 36℃ / min and kept at the temperature for 11 hours to carry out the first titanium infiltration.

[0068] Step 4: After the temperature is constant, rapidly increase the temperature of the four areas simultaneously to 1090℃ at a program speed of 16℃ / min, and hold the temperature for 29 hours.

[0069] Step 5: Remove from the furnace and cool for 48 hours; disassemble titanium diffusion reactor 2 and remove the titanium diffusion device.

[0070] Step 6: Assemble the titanium diffusion reactor 2, place it in the heating furnace 1 to raise the furnace temperature to 250℃, maintain it for 1 hour, evacuate and check for leaks, and purge with argon to 100kPa;

[0071] Step 7: After assembling the titanium diffusion reactor 2, add 650 kg of liquid magnesium, raise the temperature to 855℃, add titanium tetrachloride at a feed rate of 360 kg / h for 1 hour, then stop feeding, keep the temperature constant for 5 hours, and carry out the second titanium diffusion.

[0072] Step 8: Reduce, distill, and crush to obtain sponge titanium.

[0073] Comparative Example 1

[0074] Step 1: Clean the titanium diffusion reactor 2, assemble the titanium diffusion frame, add 600 kg of sponge titanium, and assemble the titanium diffusion reactor 2.

[0075] Step 2: After the sealing is qualified, vacuum is drawn, and the four areas are heated to 1050℃ at the same time and kept at the temperature for 40 hours to carry out titanium infiltration.

[0076] Step 3: Reduce, distill, and crush to obtain sponge titanium.

[0077] Comparative Example 2

[0078] Step 1: Clean the titanium diffusion reactor 2. Place the assembled titanium diffusion reactor 2 into the heating furnace 1 and raise the furnace temperature to 250℃. Maintain the temperature for 2 hours to dry the titanium diffusion reactor 2. After drying, evacuate the furnace to remove the evaporated water vapor and check the airtightness.

[0079] Step 2: After the sealing is qualified, vacuum is drawn, 650 kg of liquid magnesium is added, the temperature is raised to 855℃, titanium tetrachloride is added at a rate of 360 kg / h for 1 hour, then the feeding is stopped and the temperature is kept constant for 5 hours to carry out titanium infiltration.

[0080] Step 3: Reduce, distill, and crush to obtain sponge titanium.

[0081] The performance of the sponge titanium obtained in Examples 1-3 and Comparative Examples 1-2 was tested, and the results are shown in Table 1:

[0082] Table 1

[0083] sample Level Titanium Diffusion Area % Fe% O％ Example 1 Level 0 96 0.03 0.03 Example 2 Level 0 88 0.04 0.02 Example 3 Level 1 80 0.04 0.02 Comparative Example 1 Level 4 70 0.10 0.23 Comparative Example 2 Extra-high titanium 0 0.5 0.37

[0084] The above embodiments demonstrate that the method provided by the present invention improves the quality of the sponge titanium product produced from unqualified to Grade 1-0. After the titanium diffusion area is increased and the titanium diffusion effect is improved, the content of iron impurities in the sponge titanium is greatly reduced, and the furnace drying process also reduces the oxygen content by orders of magnitude.

[0085] In addition, the bottom surface of the heating furnace 1 is provided with a base support 4, and the top surface of the base support 4 is provided with a placement groove that matches the lower half of the titanium diffusion reactor 2, so that the titanium diffusion reactor 2 can be placed on the base support 4. The top of the heating furnace 1 is provided with a matching sealing furnace cover 3, and the bottom surface of the sealing furnace cover 3 is provided with a sealing ring 31 that matches the opening size of the top of the titanium diffusion reactor 2. After the cover is closed, the sealing ring 31 can seal the titanium diffusion reactor 2. The bottom surface of the heating furnace 1 is provided with a cover opening component 5, and the top surface of the sealing furnace cover 3 is provided with a feeding structure 6.

[0086] Specifically, the cover opening assembly 5 includes a motor 51 located at the bottom of the central axis on the outer wall of the rear side of the heating furnace 1, a shaft structure 52, and a transmission gear structure 53. The output end of the motor 51 is connected to the shaft structure 52. The shaft structure 52 includes a first shaft 521. The bottom end of the first shaft 521 is connected to the output end of the motor 51 through a first transmission gear set 531. The top end of the first shaft 521 is connected to a connecting shaft 522 through a second transmission gear set 532. The two ends of the connecting shaft 522 pass through the left and right side walls of the heating furnace 1 and are fixedly connected to the left and right inner side walls of the sealed furnace cover 3. In use, the motor 51 drives the first shaft 521 and the second transmission gear set 532 to drive the connecting shaft 522 to rotate, thereby driving the sealed furnace cover 3 to open and close.

[0087] Furthermore, the output end of the motor 51 is coaxially connected to a second shaft 523. The front end of the second shaft 523 is connected to the third shaft 524 symmetrically arranged on the left and right sides through a third transmission gear set 533. The outer end of the third shaft 524 is connected to a threaded rod 54 through a fourth transmission gear set 534. When the motor 51 drives the sealing furnace cover 3 to open and close, it will drive the threaded rod 54 to rotate through the second shaft 523, the third transmission gear set 533, the third shaft 524 and the fourth transmission gear set 534.

[0088] Specifically, the threads on the left and right threaded rods 54 are in opposite directions. The bottom surface of the threaded rods 54 is rotatably connected to the bottom surface of the heating furnace 1. The bottom surface of the base 4 is symmetrically provided with threaded grooves on the left and right sides. The base 4 is threadedly connected to the threaded rods 54 on the same side through the threaded grooves. After the threaded rods 54 rotate, the base 4 will move up and down together with the opening and closing of the cover.

[0089] In addition, the feeding structure 6 includes a feeding port 61 located in the middle of the top surface of the sealed furnace cover 3. A diverter 62 is provided on the left side inside the feeding port 61. The diverter 62 is in the shape of an inverted umbrella. The top side wall of the diverter 62 is fixed to the inner wall of the feeding port 61 by connecting rods 63 arranged symmetrically on the left and right. Liquid magnesium flows through the feeding port 61 and the diverter 62 into the titanium diffusion reactor 2. The inverted umbrella-shaped diverter 62 can divert the liquid magnesium to prevent it from accumulating only in the middle of the titanium diffusion reactor 2.

[0090] Finally, a vacuum device 7 is provided on the left side of the top surface of the sealed furnace cover 3. A vacuum tube 71 is provided in the middle of the right side wall of the vacuum device 7. The other end of the vacuum tube 71 passes through the sealed furnace cover 3 and the connection port is located within the sealing ring 31. The vacuum device 7 is used to evacuate the titanium diffusion reactor 2 and extract water vapor. An argon generator 8 is provided on the left side of the rear side of the top surface of the sealed furnace cover 3. A gas pipe 81 is provided in the middle of the front side wall of the argon generator 8, which is connected to the right end of the vacuum tube 71. A first valve 72 and a second valve 82 are respectively provided in the middle section of the vacuum tube 71 and the gas pipe 81. Argon gas is introduced into the titanium diffusion reactor 2 through the argon generator 8.

[0091] The working principle of the process for reducing oxygen in sponge titanium iron in this invention is as follows:

[0092] The first titanium diffusion process involves using high temperature to reach the eutectic point of the titanium-iron alloy, creating a protective titanium-iron alloy layer on the reactor surface to prevent direct contact between iron and titanium. The second titanium diffusion process directly involves reacting liquid magnesium with titanium tetrachloride to produce titanium particles, resulting in a new titanium layer on the reactor surface. Through these two titanium diffusion processes, the reactor surface simultaneously possesses both a titanium-iron alloy layer and a titanium layer, completely avoiding contact and reaction between the reacted titanium and iron, thus reducing the impact of iron on the quality of the sponge titanium.

[0093] When placing the titanium infiltration reactor 2 into the heating furnace 1, align the titanium infiltration reactor 2 with the placement slot on the base 4, and then start the motor 51. At this time, the output end of the motor 51 will drive the first shaft 521 to rotate through the first transmission gear set 531, and then drive the horizontal connecting shaft 522 to rotate through the second transmission gear set. The connecting shaft 522 will drive the sealing furnace cover 3 to rotate downward for sealing. At the same time, the output end of the motor 51 will also drive the second shaft 523 at the bottom to rotate, and then drive the third shafts 524 on both sides to rotate through the third transmission gear set 533. Finally, the vertical threaded rod 54 will rotate through the fourth transmission gear set 534. The bottom surface of the base 4 is threaded to the threaded rod 54 through the threaded grooves on both sides. After the threaded rod 54 rotates, it will drive the base 4 to move downward, so that the titanium infiltration reactor 2 enters the heating furnace 1.

[0094] The foregoing description of specific exemplary embodiments of the invention is for illustrative and explanatory purposes. These descriptions are not intended to limit the invention to the precise forms disclosed, and it will be apparent that many changes and variations can be made in accordance with the foregoing teachings. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application, thereby enabling those skilled in the art to implement and utilize various different exemplary embodiments of the invention, as well as various different choices and variations. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A process for reducing titanium-iron with oxygen, characterized in that, The method comprises the following steps: Step 1: clean the titanium infiltration reactor (2), add titanium sponge for titanium infiltration, and assemble the titanium infiltration reactor (2); Step 2: place the assembled titanium infiltration reactor (2) on the bottom support (4) of the heating furnace (1), then send the titanium infiltration reactor (2) into the heating furnace (1) through the cover opening assembly (5) and seal the cover, increase the temperature of the heating furnace (1) to a certain temperature, maintain for 2 h, and bake the titanium infiltration reactor (2); after baking, open the vacuum device (7) and open the first valve (72) and close the second valve (82) to evacuate and remove the evaporated water vapor, and check the air tightness at the same time; Step 3: after the air tightness is qualified, vacuumize, and at the same time, divide the heating furnace (1) into four areas from top to bottom, and increase the temperature of the four areas to the specified temperature respectively, and maintain for 10±1 h; Step 4: after constant temperature, rapidly increase the temperature of the four areas to a certain temperature, maintain for 30±1 h, and at the same time, vacuumize through the vacuum device (7) to carry out the first titanium infiltration; Step 5: after the first titanium infiltration is completed, take out the titanium infiltration reactor (2) after cooling and disassembling the titanium infiltration reactor (2); Step 6: assemble the titanium infiltration reactor (2), bake in the heating furnace (1), increase the temperature to 200±50℃, maintain for 1 h, open the vacuum device (7) and open the first valve (72) and close the second valve (82) to evacuate, then check the leakage, close the first valve (72) and open the second valve (82) after the checking is completed, and fill argon through the argon generator (8); Step 7: then add a small amount of liquid magnesium through the feeding structure (6), increase the temperature, stop feeding after adding a small amount of titanium tetrachloride for 1 h, maintain for 5 h, and carry out the second titanium infiltration; Step 8: reduce, distill and crush to obtain titanium sponge; The inner bottom surface of the heating furnace (1) is provided with a bottom support (4), the top surface of the bottom support (4) is provided with a placing groove matched with the lower half of the titanium infiltration reactor (2), the top of the heating furnace (1) is provided with a matched sealing furnace cover (3), the bottom surface of the sealing furnace cover (3) is provided with a sealing ring (31) matched with the opening size of the top of the titanium infiltration reactor (2), the inner bottom surface of the heating furnace (1) is provided with a cover opening assembly (5), and the top surface of the sealing furnace cover (3) is provided with a feeding structure (6) in the middle; The cover opening assembly (5) comprises a motor (51) located in the middle axis of the rear side outer wall of the heating furnace (1) and close to the bottom, a shaft rod structure (52) and a transmission gear set structure (53), the output end of the motor (51) is connected with the shaft rod structure (52), the shaft rod structure (52) comprises a first shaft rod (521), the bottom end of the first shaft rod (521) is in transmission connection with the output end of the motor (51) through the first transmission gear set (531), the top end of the first shaft rod (521) is in transmission connection with a connecting shaft (522) through the second transmission gear set (532), and the two ends of the connecting shaft (522) penetrate through the left and right side walls of the heating furnace (1) and are fixedly connected with the left and right inner side walls of the sealing furnace cover (3). The output end of the motor (51) is coaxially connected with a second shaft rod (523), the front end of the second shaft rod (523) is in transmission connection with the third shaft rods (524) symmetrically arranged on the left and right sides through the third transmission gear set (533), and the outer ends of the third shaft rods (524) are in transmission connection with threaded rods (54) through fourth transmission gear sets (534).

2. The process of reducing the titanium iron sponge with oxygen according to claim 1, characterized by the fact that: In step 3, vacuum is extracted to 2±0.1kPa, and the four areas are simultaneously heated to 950±5℃ at a rate of 35±1℃ / min.

3. The process of reducing the titanium iron sponge with oxygen according to claim 1, characterized by the fact that: In step 4, the four areas are simultaneously heated to 1085±5℃ at a rate of 15±1℃ / min from top to bottom.

4. The process of reducing the titanium iron sponge with oxygen according to claim 1, characterized in that: In step 7, 550±50kg of liquid magnesium is added, and the four areas are simultaneously heated to 850±5℃, and 350±10kg / h of titanium tetrachloride is added for 1h.

5. The process of reducing the titanium iron sponge with oxygen according to claim 1, characterized in that: The threaded rods (54) are reversely threaded on the left and right sides, and the bottom surfaces of the threaded rods (54) are rotationally connected to the bottom surface of the heating furnace (1), the bottom support (4) is symmetrically provided with threaded grooves on the bottom surface, and the bottom support (4) is in threaded connection with the threaded rods (54) on the same side through the threaded grooves.

6. The process of reducing the titanium iron sponge with oxygen according to claim 1, characterized in that: The feeding structure (6) comprises a feeding pipe (61) arranged on the top surface of the sealing furnace cover (3), a flow divider (62) is arranged in the feeding pipe (61) on the left side, the flow divider (62) is in an inverted umbrella shape, and the top side wall of the flow divider (62) is fixed to the inner wall of the feeding pipe (61) through the left and right symmetrically arranged connecting rods (63).

7. The process of reducing the titanium iron sponge with oxygen according to claim 1, characterized in that: The top surface of the sealing furnace cover (3) is provided with a vacuum device (7) on the left side, the middle part of the right side wall of the vacuum device (7) is provided with a vacuum pipe (71), the other end of the vacuum pipe (71) penetrates through the sealing furnace cover (3) and is connected to the sealing ring (31), the top surface of the sealing furnace cover (3) is provided with an argon generator (8) on the left end of the rear side, the middle part of the front side wall of the argon generator (8) is provided with a gas pipe (81) in communication with the right end of the vacuum pipe (71), and the middle sections of the vacuum pipe (71) and the gas pipe (81) are respectively provided with first and second valves (72) and (82).

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