A method for removing impurities from titanium tetrachloride

By using atomization reaction device and rotary nozzle technology in the titanium tetrachloride impurity removal process, the vanadium removal reaction is efficiently carried out, and the problems of high energy consumption, incomplete vanadium removal and waste of vanadium removal agents in the existing processes are solved, and a purer and more energy-saving titanium tetrachloride product is obtained.

CN116873974BActive Publication Date: 2025-06-17YUNNAN GUOTAI TITANIUM METAL CO LTD
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Patent Information

Application Number
CN202310810621.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-04
Publication Date
2025-06-17
Estimated Expiration
2043-07-04

AI Technical Summary

Technical Problem

The existing titanium tetrachloride impurity removal process has problems such as high energy consumption, incomplete vanadium removal and waste of vanadium removal agents. In particular, the high boiling point impurities generated by organic matter after vanadium removal cause damage to the equipment and requires additional evaporation treatment.

Method used

The atomization reaction device is adopted to control the spraying method of vanadium deletion agent through a pressurized pump and a water pump to make it fully contact with the titanium tetrachloride gas, and the contact area is increased by a rotary atomization nozzle, and the vanadium deletion agent is sprayed intermittently to reduce waste. Further deletion treatment is carried out through a distillation tower and a secondary dust collector.

Benefits of technology

The efficiency of vanadium removal reaction is improved, the waste of vanadium removal agent is reduced, energy consumption is reduced, and the damage to the equipment by high boiling point impurities is reduced. Through the use of distillation and the use of secondary dust collectors, a purer titanium tetrachloride product is obtained.

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Abstract

The present invention relates to the technical field of titanium chemical industry, and discloses a method for removing impurities from titanium tetrachloride, which includes removing solid particles by using a first dust collector, performing a vanadium removal reaction on titanium tetrachloride with an atomized vanadium removal agent, removing high-boiling impurities by using a secondary dust collector, condensing titanium tetrachloride into a liquid and filtering it by using a washing tower, obtaining a qualified product by low-temperature rectification in a rectification tower, and acidifying the high-boiling slag discharged from the secondary dust collector. By intermittently and rotationally spraying the atomized vanadium removal agent, the present invention promotes the full reaction between the vanadium removal agent and titanium tetrachloride, reduces the waste of the vanadium removal agent, does not require high-boiling impurities, eliminates distillation equipment, and reduces production energy consumption.
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Description

Technical Field

[0001] The present invention belongs to the technical field of titanium chemical industry, and specifically relates to a method for removing impurities from titanium tetrachloride. Background Art

[0002] Titanium tetrachloride is a key intermediate product in the production of titanium dioxide and titanium sponge. Its impurity content has a crucial impact on the quality of the final product. In the current process, during the refining process, impurities such as vanadium, silicon, aluminum, iron, and tin need to be removed. The main method for removal is through a combination of distillation and rectification. Through this impurity removal method, a large amount of energy is consumed. In addition, since the current process for removing vanadium from titanium tetrachloride mainly uses organic substances to remove vanadium, a large amount of high-boiling impurities will be generated during the removal of vanadium by organic substances. Moreover, these impurities have extremely strong adhesiveness, which can cause damage to heating equipment and result in the compression of the space in the distillation kettle. Additionally, for the high-boiling impurities after removing vanadium by organic substances, evaporation is required to evaporate the high-boiling impurities to dryness. Since the solid residue after drying has a high carbon content, water needs to be added to make it moist.

[0003] Patent CN211246498U discloses a novel device for removing impurities from titanium tetrachloride, which includes a feeding system, a reaction system, and a collection system. The feeding system includes an oil storage tank, a feeding pump, a flowmeter, and a crude titanium tank. The oil storage tank and the crude titanium tank are two pipelines respectively connected to the feeding pump and the flowmeter. The reaction system is provided with a reactor, and the reactor is provided with a mixing tank and an evaporation tank. The collection system is provided with a rectification column, a condensation tank, and a liquid storage tank. The feeding system, the reaction system, and the collection system are connected in sequence. Through the feeding system, mineral oil and crude titanium tetrachloride enter the mixing tank through different pipelines respectively, so that they can be fully mixed without a stirrer. Patent CN202122817950.1 discloses a pre-mixing device for removing vanadium from crude titanium tetrachloride, which includes a mixing tank. The top of the mixing tank is provided with two input pipes, and each input pipe is provided with a metering pump and a flowmeter. The metering pump and the flowmeter communicate with a control module. The mixing tank is provided with a horizontal first stirring shaft and a vertical second stirring shaft, and stirring blades are provided on the stirring shafts. The bottom of the mixing tank is provided with a discharge pipe. The control module controls the metering pump to regularly and quantitatively transport the mixture into the mixing tank through the input pipe, effectively controlling the dosage of the vanadium removal agent and ensuring the qualified rate of titanium tetrachloride products.

[0004] When the vanadium removal agent and crude titanium tetrachloride react in the above patents, due to the limited contact area, the vanadium removal may not be complete, and usually enough vanadium removal agent needs to be added to ensure complete vanadium removal, which often causes waste of the vanadium removal agent.

[0005] The information disclosed in this background art section is only intended to enhance the overall understanding of the present invention and should not be regarded as an admission or any form of suggestion that this information constitutes prior art already known to those of ordinary skill in the art. Summary of the Invention

[0006] The object of the present invention is to provide a method for removing impurities from titanium tetrachloride to solve the above problems of the prior art.

[0007] To achieve the above object, the present invention provides a method for removing impurities from titanium tetrachloride, comprising the following steps:

[0008] S1. After the chlorination is completed in the chlorination furnace, the temperature at the top of the chlorination furnace is controlled within the range of 300 ± 50 °C using condensed titanium tetrachloride;

[0009] S2. The titanium tetrachloride gas passes through the first dust collector, and the solid particles entrained in the titanium tetrachloride gas are removed by decelerating and cooling down through the first dust collector;

[0010] S3. The titanium tetrachloride gas continues to enter the atomization reaction device. The titanium tetrachloride gas enters the reaction tank after passing through the intake pipe, connecting pipe, draft tube and outlet pipe in sequence, and the titanium tetrachloride gas is evenly distributed around the installation cylinder;

[0011] S4. The pressure pump keeps the pressure in the storage tank at 50 ± 5 kPa. The output shaft of the control motor drives the turntable to rotate, and the turntable drives the movable column to reciprocate up and down in the control tank through the connecting rod, and the piston intermittently blocks the vanadium removal agent in the storage tank from entering the reaction tank;

[0012] S5. The water pump pumps the vanadium removal agent in the storage tank into the installation cylinder. The output shaft of the driving motor drives the rotating shaft to rotate, and the toothed ring rotates accordingly, so that the bevel gear rotates and the atomizing nozzle rotates, and the atomized vanadium removal agent is sprayed out rotationally;

[0013] S6. The temperature in the reaction tank is controlled between 300 ± 5 °C. When the temperature is higher than 305 °C, coolant is introduced into the two condenser tubes to take away heat. When the temperature is lower than 295 °C, the two heating plates work to increase the temperature;

[0014] S7. The atomized vanadium removal agent reacts fully with the titanium tetrachloride gas. After the reaction is completed, the titanium tetrachloride gas mixed with impurities such as vanadyl dichloride enters the secondary dust collector, and the high-boiling-point impurities such as vanadyl dichloride are removed by decelerating and cooling down through the secondary dust collector, and the vanadium removal is completed;

[0015] S8. The titanium tetrachloride gas continues to enter the scrubbing tower. The scrubbing tower condenses the titanium tetrachloride and the unseparated high-boiling-point impurities into a liquid and discharges them into the collection pool. At this time, the collection pool also contains high-boiling-point impurities such as aluminum trichloride, iron trichloride and vanadyl dichloride. The pore diameter of the filter membrane in the collection pool is between 0.038 - 0.045 mm, and the number of pores is between 325 - 400 meshes. After filtration, clear titanium tetrachloride is obtained;

[0016] S9. The filtered titanium tetrachloride is heated to between 60 and 70 °C using waste heat and then added into the distillation column. The distillation column is provided with 45 trays, has a diameter of 1200 mm, and titanium tetrachloride is added at the 23rd tray. The pressure inside the distillation column is controlled at 0 - 12 kPa, and the pressure at the bottom of the column is controlled within 50 kPa. Through distillation separation, titanium tetrachloride and tin tetrachloride impurities are separated to obtain qualified products;

[0017] S10. The high-boiling slag discharged from the secondary dust collector is added into the acidification tank and can be used for wet vanadium extraction later. After the vanadium extraction is completed, the solid slag is dried using the waste heat of the chlorination furnace, and then the solid slag is returned to the chlorination furnace as a carbon source for use.

[0018] In the technical solution of the present invention, the atomization reaction device includes, successively arranged from front to back, the reaction tank, the water pump, the control tank, and the storage tank. At the center of the bottom surface of the top wall of the reaction tank, an installation plate is fixed through a vertical column. At the edge of the bottom surface of the installation plate, several guide cylinders are fixedly arranged at equal intervals in a ring shape. On the opposite sides of several guide cylinders, several gas outlet pipes are installed at equal intervals.

[0019] In the technical solution of the present invention, the first dust collector and the reaction tank are connected through the intake pipe, and the intake pipe extends above the installation plate. The intake pipe and the guide cylinder are connected through the connecting pipe.

[0020] In the technical solution of the present invention, an installation cylinder is fixed at the center of the bottom surface of the installation plate. Several installation blocks are rotatably connected to the side wall of the installation cylinder in a regular manner. One end of the installation block far from the installation cylinder is equipped with an atomizing nozzle.

[0021] In the technical solution of the present invention, a driving motor is installed at the center of the top surface of the installation plate. The output shaft of the driving motor extends into the installation cylinder and is coaxially connected to a rotating shaft. A toothed ring is fixed on the outer side wall of the rotating shaft near several installation blocks of the same layer. One end of the installation block located inside the installation cylinder is fixedly sleeved with a bevel gear meshing with the adjacent toothed ring.

[0022] In the technical solution of the present invention, installation frames are fixed on both the front and back sides of the installation plate at the bottom surface of the top wall of the reaction tank. A condenser tube is fixed inside the installation frame, and both ends of the condenser tube extend outside the reaction tank. Heating plates are fixed on both the left and right sides of the bottom surface of the top wall of the reaction tank and the installation plate.

[0023] In the technical solution of the present invention, the water outlet end of the water pump is connected to the installation cylinder through a liquid outlet pipe, and the water inlet end of the water pump is connected to the control tank through a liquid inlet pipe.

[0024] In the technical solution of the present invention, the movable column is slidably inserted in the middle of the top wall of the control tank, and the piston is fixed at the bottom end of the movable column. The size of the piston is adapted to the internal size of the control tank.

[0025] In the technical solution of the present invention, a control motor is fixed on the top surface of the control tank near the movable column. The output shaft of the control motor is coaxially connected with a turntable. One side edge of the turntable near the movable column is hinged with a connecting rod, and the bottom end of the connecting rod is hinged at the top surface of the movable column.

[0026] In the technical solution of the present invention, a pressure pump is installed on the top surface of the storage tank, and the storage tank and the control tank are communicated through a connecting pipe.

[0027] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are as follows:

[0028] 1. In the present invention, the atomized vanadium removal agent is sprayed around, and the titanium tetrachloride gas moves closer to the middle installation cylinder, enabling the vanadium removal agent and titanium tetrachloride to come into efficient contact, promoting the occurrence of the vanadium removal reaction. At the same time, the atomizing nozzle rotates continuously, further increasing the contact area between the vanadium removal agent and titanium tetrachloride, improving the reaction efficiency, and intermittently spraying the vanadium removal agent to ensure that the vanadium removal agent can fully react with titanium tetrachloride and reduce the waste of the vanadium removal agent.

[0029] 2. In the present invention, the mud evaporation process is reduced, and low-temperature rectification using a rectification tower reduces energy consumption. In addition, the high-boiling-point slag discharged from the secondary dust collector does not need to be evaporated and can be directly diluted and used for wet vanadium extraction, further reducing energy consumption. The remaining fixed slag can also be returned to the chlorination furnace as a carbon source, which is energy-saving and environmentally friendly. Description of the Drawings

[0030] Figure 1 It is the impurity removal flow chart of the present invention;

[0031] Figure 2 It is the structural schematic diagram of the atomization reaction device in the present invention;

[0032] Figure 3 It is the partial structural schematic diagram of the atomization reaction device in the present invention;

[0033] Figure 4 It is the cross-sectional view of the reaction tank in the present invention;

[0034] Figure 5 It is the bottom view of the mounting plate in the present invention;

[0035] Figure 6 It is the longitudinal sectional view of the mounting plate in the present invention;

[0036] Figure 7 It is the longitudinal sectional view of the installation cylinder in the present invention;

[0037] Figure 8 Longitudinal sectional view of the control tank in the present invention.

[0038] Explanation of reference numerals:

[0039] 1. Chlorination furnace;

[0040] 2. First dust collector;

[0041] 3. Atomization reaction device; 30. Reaction tank; 300. Intake pipe; 301. Condensing pipe; 302. Heating plate; 303. Mounting plate; 3030. Draft tube; 3031. Exhaust pipe; 3032. Connecting pipe; 3033. Mounting cylinder; 3034. Driving motor; 3035. Rotating shaft; 3036. Ring gear; 3037. Mounting block; 3038. Atomizing nozzle; 3039. Bevel gear; 31. Water pump; 310. Liquid inlet pipe; 311. Liquid outlet pipe; 32. Control tank; 320. Movable column; 321. Piston; 322. Control motor; 323. Turntable; 324. Connecting rod; 33. Storage tank; 330. Pressurizing pump; 331. Connecting pipe;

[0042] 4. Secondary dust collector;

[0043] 5. Scrubbing tower;

[0044] 6. Acidification tank;

[0045] 7. Collection tank;

[0046] 8. Rectification column. Detailed implementation manners

[0047] The following combines the accompanying drawings to describe in detail the specific implementation manners of the present invention, but it should be understood that the protection scope of the present invention is not limited by the specific implementation manners.

[0048] Unless otherwise clearly stated, throughout the specification and claims, the term "comprise" or its variations such as "comprises" or "comprising" etc. will be understood to include the stated elements or components, without excluding other elements or other components.

[0049] Refer to Figures 1 - 8 , the method for removing impurities from titanium tetrachloride of the present invention includes the following steps:

[0050] S1. After chlorination is completed in the chlorination furnace 1, use the condensed titanium tetrachloride to control the temperature at the top of the chlorination furnace 1 within the range of 300 ± 50 °C;

[0051] S2. The titanium tetrachloride gas passes through the first dust collector 2, decelerates and cools down through the first dust collector 2, and removes the solid particles entrained in the titanium tetrachloride gas;

[0052] S3. The titanium tetrachloride gas continues to enter the atomization reaction device 3. The titanium tetrachloride gas enters the reaction tank 30 after passing through the inlet pipe 300, the connecting pipe 3032, the draft tube 3030 and the outlet pipe 3031 in sequence, and the titanium tetrachloride gas is evenly distributed around the installation cylinder 3033;

[0053] S4. The pressure pump 330 keeps the pressure in the storage tank 33 at 50 ± 5 kPa. Control the output shaft of the motor 322 to drive the turntable 323 to rotate, and the turntable 323 drives the movable column 320 to reciprocate up and down in the control tank 32 through the connecting rod 324, and the piston 321 intermittently blocks the vanadium remover in the storage tank 33 from entering the reaction tank 30;

[0054] S5. The water pump 31 pumps the vanadium remover in the storage tank 33 into the installation cylinder 3033. Drive the output shaft of the motor 3034 to drive the rotating shaft 3035 to rotate, and the toothed ring 3036 rotates accordingly, so that the bevel gear 3039 rotates and the atomizing nozzle 3038 rotates, and the atomized vanadium remover is sprayed out rotationally;

[0055] S6. The temperature in the reaction tank 30 is controlled between 300 ± 5 °C. When the temperature is higher than 305 °C, coolant is introduced into the two condenser pipes 301 to take away the heat. When the temperature is lower than 295 °C, the two heating plates 302 work to increase the temperature;

[0056] S7. The atomized vanadium remover is in full contact with the titanium tetrachloride gas and reacts. After the reaction is completed, the titanium tetrachloride gas mixed with impurities such as vanadyl dichloride enters the secondary dust collector 4, and high-boiling impurities such as vanadyl dichloride are removed by decelerating and cooling down in the secondary dust collector 4 to complete vanadium removal;

[0057] S8. The titanium tetrachloride gas continues to enter the scrubbing tower 5. The scrubbing tower 5 condenses the titanium tetrachloride and the unseparated high-boiling impurities into a liquid and introduces it into the collection pool 7. At this time, the collection pool 7 also contains high-boiling impurities such as aluminum trichloride, iron trichloride, and vanadyl dichloride. The pore diameter of the filter membrane in the collection pool 7 is between 0.038 - 0.045 mm, and the number of pores is between 325 - 400 meshes. After filtration, clarified titanium tetrachloride is obtained;

[0058] S9. The filtered titanium tetrachloride is heated to between 60 - 70 °C using waste heat and added to the distillation column 8. The distillation column 8 is provided with 45 trays and has a diameter of 1200 mm. The titanium tetrachloride is added at the 23rd tray. The pressure in the distillation column 8 is controlled between 0 - 12 kPa, and the pressure at the bottom of the column is controlled within 50 kPa. After distillation separation of the titanium tetrachloride and tin tetrachloride impurities, a qualified product is obtained;

[0059] S10. Add the high-boiling slag discharged from the secondary dust collector 4 into the acidification tank 6, which can then be used for wet vanadium extraction. After the vanadium extraction is completed, the solid slag is dried by the waste heat of the chlorination furnace 1, and then the fixed slag is returned to the chlorination furnace 1 as a carbon source for use.

[0060] In the present invention, in order to promote complete vanadium removal and reduce the waste of vanadium removal agent, therefore, referring to Figures 2 - 8 , the atomization reaction device 3 includes a reaction tank 30, a water pump 31, a control tank 32, and a storage tank 33 arranged in sequence from front to back. At the center of the bottom surface of the top wall of the reaction tank 30, a mounting plate 303 is fixed by a vertical column. At the edge of the bottom surface of the mounting plate 303, a plurality of guide cylinders 3030 are fixedly arranged at equal intervals in a ring shape. On one side of the plurality of guide cylinders 3030 opposite to each other, a plurality of gas outlet pipes 3031 are installed at equal intervals, so that the titanium tetrachloride gas converges towards the middle, thereby ensuring that the titanium tetrachloride can contact and react with the vanadium removal agent in a timely manner.

[0061] In the above solution, between the first dust collector 2 and the reaction tank 30, they are connected by an air inlet pipe 300. The air inlet pipe 300 extends above the mounting plate 303. Between the air inlet pipe 300 and the guide cylinder 3030, they are connected by a connecting pipe 3032. After the titanium tetrachloride gas is dust-removed by the first dust collector 2, it enters the reaction tank 30 through the air inlet pipe 300, and the titanium tetrachloride gas is evenly distributed around the mounting cylinder 3033 by the guide cylinder 3030.

[0062] Specifically, at the center of the bottom surface of the mounting plate 303, a mounting cylinder 3033 is fixed. On the side wall of the mounting cylinder 3033, a plurality of mounting blocks 3037 are rotatably connected regularly. At one end of the mounting block 3037 away from the mounting cylinder 3033, an atomizing nozzle 3038 is installed. The atomizing nozzle 3038 sprays the atomized vanadium removal agent, enabling the vanadium removal agent to contact with the titanium tetrachloride efficiently and making the vanadium removal agent react completely.

[0063] Furthermore, at the center of the top surface of the mounting plate 303, a driving motor 3034 is installed. The output shaft of the driving motor 3034 extends into the mounting cylinder 3033 and is coaxially connected to a rotating shaft 3035. On the outer side wall of the rotating shaft 3035 near several mounting blocks 3037 of the same layer, a toothed ring 3036 is fixed. At one end of the mounting block 3037 located inside the mounting cylinder 3033, a bevel gear 3039 meshing with the adjacent toothed ring 3036 is fixedly sleeved. When the rotating shaft 3035 rotates, the toothed ring 3036 will rotate synchronously, thereby causing the bevel gear 3039 and the mounting block 3037 to rotate, and the atomizing nozzle 3038 rotates accordingly, spraying the vanadium removal agent in a rotating manner, further increasing the contact area between the vanadium removal agent and the titanium tetrachloride.

[0064] Further, mounting frames are fixed to the bottom surface of the top wall of the reaction tank 30 on both the front and rear sides of the mounting plate 303. A condenser tube 301 is fixed inside the mounting frame, and both ends of the condenser tube 301 extend outside the reaction tank 30. Heating plates 302 are fixed to the bottom surface of the top wall of the reaction tank 30 and on both the left and right sides of the mounting plate 303, facilitating the control of the temperature inside the reaction tank 30 and keeping the temperature inside the reaction tank 30 between 300 ± 5 °C.

[0065] Further, the water outlet end of the water pump 31 is connected to the mounting cylinder 3033 through a liquid outlet pipe 311, and the water inlet end of the water pump 31 is connected to the control tank 32 through a liquid inlet pipe 310. The vanadium removal agent is pumped into the mounting cylinder 3033 by the water pump 31.

[0066] In addition, a movable column 320 is slidably inserted into the middle of the top wall of the control tank 32. A piston 321 is fixed to the bottom end of the movable column 320. The size of the piston 321 is adapted to the internal size of the control tank 32. When the piston 321 blocks the liquid inlet pipe 310 and the connecting pipe 331, the atomizing nozzle 3038 stops spraying the vanadium removal agent, causing the vanadium removal agent to be sprayed intermittently and ensuring that the sprayed vanadium removal agent fully reacts with titanium tetrachloride.

[0067] It should be noted that a control motor 322 is fixed to the top surface of the control tank 32 near the movable column 320. The output shaft of the control motor 322 is coaxially connected to a turntable 323. A connecting rod 324 is hinged to the side edge of the turntable 323 near the movable column 320, and the bottom end of the connecting rod 324 is hinged to the top surface of the movable column 320. The output shaft of the control motor 322 drives the turntable 323 to rotate, driving the movable column 320 to move up and down through the connecting rod 324, causing the piston 321 to intermittently block the liquid inlet pipe 310 and the connecting pipe 331.

[0068] It should be noted that a pressure pump 330 is installed on the top surface of the storage tank 33. The storage tank 33 and the control tank 32 are connected through a connecting pipe 331. The pressure pump 330 increases the pressure in the storage tank 33 to 50 ± 5 kPa, making the reaction more complete.

[0069] The working principle of promoting complete vanadium removal and reducing waste of the vanadium removal agent in the titanium tetrachloride impurity removal method of the present invention is specifically as follows:

[0070] The titanium tetrachloride gas passes through the inlet pipe 300, the connecting pipe 3032, the guide cylinder 3030, and the outlet pipe 3031 in sequence and is evenly distributed around the mounting cylinder 3033;

[0071] The pressure pump 330 increases the pressure in the storage tank 33. The control motor 322 operates, and the output shaft of the control motor 322 drives the turntable 323 to rotate. During the rotation of the turntable 323, the movable column 320 is driven to move up and down reciprocally through the connecting rod 324, and the piston 321 also moves up and down reciprocally, causing the vanadium removal agent to be intermittently sprayed finally;

[0072] The water pump 31 pumps the vanadium remover into the installation cylinder 3033. The driving motor 3034 operates, and the output shaft of the driving motor 3034 drives a plurality of toothed rings 3036 to rotate. The bevel gear 3039 rotates accordingly, causing the installation block 3037 and the atomizing nozzle 3038 to rotate accordingly. The vanadium remover is sprayed out rotationally, promoting the full reaction of the vanadium remover with titanium tetrachloride. During the reaction, the temperature in the reaction tank 30 is maintained between 300 ± 5 °C through the condenser tube 301 and the heating plate 302.

[0073] The foregoing description of the specific exemplary embodiments of the present invention is for purposes of illustration and exemplification. These descriptions are not intended to limit the invention to the precise forms disclosed, and obviously, many changes and variations are possible in light of the above teaching. The purpose of selecting and describing the exemplary embodiments is to explain the specific principles of the invention and its practical applications, so that those skilled in the art can implement and utilize the various different exemplary embodiments of the invention, as well as various different selections and changes. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A method for removing impurities from titanium tetrachloride, characterized in that, It includes the following steps: S1. After chlorination is completed in the chlorination furnace (1), use condensed titanium tetrachloride to control the temperature at the top of the chlorination furnace (1) within the range of 300 ± 50 °C; S2. The titanium tetrachloride gas passes through the first dust collector (2), is decelerated and cooled in the first dust collector (2), and the solid particles entrained in the titanium tetrachloride gas are removed; S3. The titanium tetrachloride gas continues to enter the atomization reaction device (3). After the titanium tetrachloride gas passes through the inlet pipe (300), the connecting pipe (3032), the guide cylinder (3030) and the outlet pipe (3031) in sequence, it enters the reaction tank (30), and the titanium tetrachloride gas is evenly distributed around the installation cylinder (3033); S4. The pressure pump (330) keeps the pressure in the storage tank (33) at 50 ± 5 kPa. Control the output shaft of the motor (322) to drive the turntable (323) to rotate. The turntable (323) then drives the movable column (320) to reciprocate up and down in the control tank (32) through the connecting rod (324). The piston (321) intermittently blocks the vanadium removal agent in the storage tank (33) from entering the reaction tank (30); S5. The water pump (31) pumps the vanadium removal agent in the storage tank (33) into the installation cylinder (3033). The output shaft of the driving motor (3034) drives the rotating shaft (3035) to rotate, and the toothed ring (3036) rotates accordingly, so that the bevel gear (3039) rotates and the atomizing nozzle (3038) rotates, and the atomized vanadium removal agent is sprayed out rotationally; S6. The temperature in the reaction tank (30) is controlled between 300 ± 5 °C. When the temperature is higher than 305 °C, coolant is introduced into the two condenser pipes (301) to take away heat. When the temperature is lower than 295 °C, the two heating plates (302) work to increase the temperature; S7. The atomized vanadium removal agent is in full contact with the titanium tetrachloride gas and reacts. After the reaction is completed, the titanium tetrachloride gas mixed with vanadyl dichloride impurities enters the secondary dust collector (4), is decelerated and cooled in the secondary dust collector (4), and the vanadyl dichloride high-boiling impurities are removed to complete vanadium removal; S8. The titanium tetrachloride gas continues to enter the scrubbing tower (5). The scrubbing tower (5) condenses the titanium tetrachloride and the unseparated high-boiling impurities into a liquid and introduces them into the collection pool (7). At this time, the collection pool (7) also contains high-boiling impurities such as aluminum trichloride, iron trichloride, and vanadyl dichloride. The pore diameter of the filter membrane in the collection pool (7) is between 0.038 - 0.045 mm, and the number of pores is between 325 - 400 meshes. After filtration, clarified titanium tetrachloride is obtained; S9. The filtered titanium tetrachloride is heated to between 60 - 70 °C using waste heat and added to the rectification column (8). The rectification column (8) has 45 trays and a diameter of 1200 mm. The titanium tetrachloride is added at the 23rd tray. The pressure in the rectification column (8) is controlled at 0 - 12 kPa, and the pressure at the bottom of the column is controlled within 50 kPa. After rectification separation of the titanium tetrachloride and tin tetrachloride impurities, a qualified product is obtained; S10. Add the high-boiling slag discharged from the secondary dust collector (4) into the acidification tank (6), which can then be used for wet vanadium extraction. After the vanadium extraction is completed, the solid slag is dried by the waste heat of the chlorination furnace (1), and then the fixed slag is returned to the chlorination furnace (1) as a carbon source for use; The atomization reaction device (3) includes the reaction tank (30), the water pump (31), the control tank (32), and the storage tank (33) arranged in sequence from front to back. At the center of the bottom surface of the top wall of the reaction tank (30), a mounting plate (303) is fixed by a vertical column. At the edge of the bottom surface of the mounting plate (303) near the edge, a number of the guide cylinders (3030) are fixed at equal intervals in a ring shape. On the opposite sides of a number of the guide cylinders (3030), a number of gas outlet pipes (3031) are installed at equal intervals; The first dust collector (2) and the reaction tank (30) are connected through the air inlet pipe (300). The air inlet pipe (300) extends above the mounting plate (303). The air inlet pipe (300) and the guide cylinder (3030) are connected through the connecting pipe (3032); At the center of the bottom surface of the mounting plate (303), the mounting cylinder (3033) is fixed. A number of mounting blocks (3037) are regularly rotatably connected to the side wall of the mounting cylinder (3033). At one end of the mounting block (3037) away from the mounting cylinder (3033), an atomizing nozzle (3038) is installed.

2. The method for removing impurities from titanium tetrachloride according to claim 1, characterized in that: At the center of the top surface of the mounting plate (303), a driving motor (3034) is installed. The output shaft of the driving motor (3034) extends into the mounting cylinder (3033) and is coaxially connected to a rotating shaft (3035). A toothed ring (3036) is fixed on the outer side wall of the rotating shaft (3035) near a number of the mounting blocks (3037) on the same layer. At one end of the mounting block (3037) located inside the mounting cylinder (3033), a bevel gear (3039) meshing with the adjacent toothed ring (3036) is fixedly sleeved; 3. The method for removing impurities from titanium tetrachloride according to claim 1, characterized in that: On the bottom surface of the top wall of the reaction tank (30), mounting frames are fixed on both the front and rear sides of the mounting plate (303). Inside the mounting frames, the condenser tubes (301) are fixed. Both ends of the condenser tubes (301) extend outside the reaction tank (30). On both the left and right sides of the bottom surface of the top wall of the reaction tank (30) and the mounting plate (303), heating plates (302) are fixed; 4. The method for removing impurities from titanium tetrachloride according to claim 1, characterized in that: The water outlet end of the water pump (31) is connected to the mounting cylinder (3033) through the liquid outlet pipe (311). The water inlet end of the water pump (31) is connected to the control tank (32) through the liquid inlet pipe (310); 5. The method for removing impurities from titanium tetrachloride according to claim 1, characterized in that: In the middle of the top wall of the control tank (32), the movable column (320) is slidably inserted. At the bottom end of the movable column (320), the piston (321) is fixed. The size of the piston (321) is adapted to the internal size of the control tank (32).

6. The method for removing impurities from titanium tetrachloride according to claim 1, characterized in that: A control motor (322) is fixed near the movable column (320) on the top surface of the control tank (32). The output shaft of the control motor (322) is coaxially connected to a turntable (323). A connecting rod (324) is hinged to the side edge of the turntable (323) near the movable column (320), and the bottom end of the connecting rod (324) is hinged to the top surface of the movable column (320).

7. The method for removing impurities from titanium tetrachloride according to claim 1, characterized in that: A pressure pump (330) is installed on the top surface of the storage tank (33), and the storage tank (33) is communicated with the control tank (32) through a communicating pipe (331).

Citation Information

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