Novel process and equipment for purifying crude zirconium tetrachloride

Abstract

The invention discloses a coarse zirconium tetrachloride sublimation device which comprises a chlorination furnace, a crushing box is mounted at the top of the chlorination furnace, a heating device is mounted on the outer wall of the chlorination furnace, a mounting box is fixedly connected to the bottom of the chlorination furnace, a screen is mounted in the mounting box, and a screening device is mounted on the outer wall of the screen. The invention relates to the technical field of crude zirconium tetrachloride sublimation, through cooperation of a mounting plate, a sliding rod and a push rod, a driving device is used for driving a rotating disc to rotate, and when the rotating disc rotates, a connecting rod is driven to move around the rotating disc, so that the push rod drives the mounting plate to reciprocate, and when the mounting plate moves, the sliding rod can ensure that the mounting plate moves stably; and therefore, the purified zirconium tetroxide and residues are screened by the screen, and the working efficiency of workers is improved.

Description

Technical Field

[0001] The invention relates to the technical field of purification technology, and specifically provides a new process and equipment for purifying crude zirconium tetrachloride. Background Art

[0002] Zirconium tetrachloride (ZrCl4) is an important inorganic compound widely used in metallurgy, chemical engineering, materials science, and other fields, primarily for the preparation of zirconium metal, zirconium alloys, and other zirconium compounds. In high-tech fields such as electronic materials, catalysts, and high-performance ceramics, the purity of zirconium tetrachloride is increasingly demanding. However, existing zirconium tetrachloride purification technologies have several shortcomings, making it difficult to meet the high-purity demand for industrial production.

[0003] Traditional methods for purifying zirconium tetrachloride mainly include crystallization, distillation, and solvent extraction. These methods have the following problems in practical application: 1. Low purification efficiency: Due to the easy hydrolysis and volatility of zirconium tetrachloride, traditional methods are prone to introduce impurities or cause material loss during the purification process, resulting in low purification efficiency.

[0004] 2. Low product purity: Existing processes make it difficult to effectively remove water-soluble and insoluble impurities in zirconium tetrachloride, resulting in product purity failing to meet the requirements of high-end applications.

[0005] 3. Complex equipment and cumbersome operation: Traditional purification equipment has a complex structure, occupies a large area, and has cumbersome operation steps, making it difficult to achieve continuous production, which affects production efficiency.

[0006] 4. Lack of flexibility: Existing equipment is usually unable to adjust according to different process requirements and is difficult to adapt to changes in various production conditions.

[0007] Therefore, there is an urgent need for a new and efficient zirconium tetrachloride purification process and corresponding equipment that can improve purification efficiency and product purity, simplify the operating process, and improve the flexibility and adaptability of the equipment to meet the needs of modern industrial production. Summary of the Invention

[0008] In view of the shortcomings of the existing technology, the present invention provides a new process and equipment for purifying crude zirconium tetrachloride, which solves the technical problems existing in the existing technology.

[0009] To achieve the above objectives, the present invention is implemented through the following technical solutions: a new process for purifying crude zirconium tetrachloride, comprising the following steps: Step 1. Dissolve: The crude zirconium tetrachloride is added to an appropriate amount of anhydrous organic solvent, the amount of solvent is controlled so that the mass ratio of zirconium tetrachloride to solvent is 1:2 to 1:5, and the solution is dissolved under stirring at a temperature of 25° C. to 35° C. for 0.5 to 1 hour to form a uniform solution to be treated; Step 2. Pretreatment: Cool the liquid to be treated to 5°C to 10°C and keep it at this temperature for 30 minutes to 1 hour to promote the precipitation of some insoluble impurities. During this process, add an appropriate amount of precipitation aid, the amount of which is 5% to 10% of the solvent volume, to improve the precipitation effect of impurities; Step 3. Continuous centrifugation and multi-fractionation: The pretreated liquid to be treated is sent to a crude zirconium tetrachloride purification device for centrifugal separation. The speed of the centrifugal device is set to 3000 to 5000 rpm, the centrifugation time is 5 to 10 minutes, and a multi-stage liquid separation method is used to obtain a preliminary purified liquid; Step 4. Washing: Mix the pre-purified solution with deionized water in a volume ratio of 1:1 to 1:2 and perform liquid-liquid extraction to remove water-soluble impurities. After stirring for 10 to 15 minutes, allow the mixture to stand and separate the organic phase. Repeat the above washing process 2 to 3 times until the pH value of the aqueous phase is neutral. Step 5. Drying: The washed organic phase is dried over anhydrous magnesium sulfate or anhydrous calcium chloride, with the amount of the desiccant added being 5% to 10% of the volume of the organic phase. After stirring and drying for 30 minutes to 1 hour, the desiccant is filtered to remove the desiccant to obtain an anhydrous purified solution; Step 6: Solvent recovery and product acquisition: The purified solution is passed through a reduced pressure distillation apparatus, and the organic solvent is evaporated and recovered under the conditions of a vacuum degree of -0.08 to -0.09 MPa and a temperature of 40°C to 60°C until a solid product is obtained. The obtained solid is high-purity zirconium tetrachloride.

[0010] A crude zirconium tetrachloride purification device comprises a base, a pair of mounting frames fixedly mounted on the upper wall of the base, a support shaft rotatably mounted between the pair of mounting frames, a centrifuge cylinder fixedly mounted between the support shafts, a centrifugal drive structure mounted on the upper end of the centrifuge cylinder, a main shaft rotatably mounted in the centrifuge cylinder, a guide frame fixedly mounted in the centrifuge cylinder, a spiral guide plate fixedly mounted on the guide frame, a swing drive structure mounted on the mounting frame, a clear liquid pipe fixedly mounted on the upper end of the side wall of the centrifuge cylinder, an input pipe fixedly mounted on the lower end of the centrifuge cylinder, a slag discharge pipe fixedly mounted on the lower end of the side wall of the centrifuge cylinder, a liquid discharge pipe fixedly mounted on the upper end of the outer wall of the centrifuge cylinder, and a waste liquid pipe mounted on the upper end of the side wall of the centrifuge cylinder.

[0011] Preferably, the centrifugal drive structure includes a first motor, a motor frame is fixedly mounted on the upper end of the centrifugal cylinder, the first motor is fixedly mounted on the side wall of the motor frame, a coupler is fixedly mounted on the upper end of the motor frame, a driven pulley is fixedly mounted on the input end of the coupler, a driving pulley is fixedly mounted on the driving end of the first motor, a transmission belt is connected between the driving pulley and the driven pulley, and the output end of the coupler is connected to one end of the main shaft.

[0012] Preferably, the swing drive structure includes a swing frame, which is fixedly mounted on the side wall of the support shaft, a second motor is fixedly mounted on the lower end of the swing frame, a driving gear is fixedly mounted on the driving end of the second motor, a ring gear is fixedly mounted on the mounting frame, and the driving gear is meshed with the ring gear.

[0013] Preferably, an inspection door is fixedly installed on the front wall of the centrifugal cylinder.

[0014] Preferably, a filtrate box is fixedly installed on the upper wall of the centrifugal cylinder, a filter ring is fixedly installed in the filtrate box, and the clear liquid pipe is fixedly installed on the side wall of the filtrate box.

[0015] Preferably, the lower end of the main shaft is a spiral dragon-shaped multi-strand twisted plate, and the spiral guide plate is a multi-piece auger blade.

[0016] Preferably, an inner sleeve is fixedly mounted on the inner upper wall of the centrifugal cylinder, an outer sleeve is fixedly mounted on the inner upper wall of the centrifugal cylinder and located outside the inner sleeve, a water-permeable hole is opened on the outer sleeve, and the outer sleeve is fixedly connected to the inner side of the spiral guide plate.

[0017] The present invention provides a new process and equipment for purifying crude zirconium tetrachloride, which has the following beneficial effects: 1. By optimizing process conditions during the dissolution, pretreatment, centrifugal separation, washing, and drying steps, such as controlling solvent dosage, temperature, time, and additive ratio, impurities are removed to the greatest extent possible, resulting in a high-purity zirconium tetrachloride product. The equipment utilizes a specially designed centrifuge cylinder with an internal guide frame and spiral guide plates, which enhance the rotational flow of the liquid and improve the efficiency of solid-liquid separation. The lower end of the main shaft is designed with a spiral dragon-shaped multi-strand twisted plate, combined with multi-piece auger blades, to improve the uniformity of material transportation and distribution and reduce blockage. 2. Through the precise design of the centrifugal drive structure and the swing drive structure, the entire processing process can achieve a high degree of automation, reducing manual intervention and operating costs; the centrifuge cylinder structure is scientifically and rationally designed, equipped with spiral guide plates and multi-strand twisted plates, which can effectively enhance the centrifugal effect, facilitate the sedimentation of solids, and improve separation efficiency; the centrifuge device is designed with liquid discharge pipes, drain pipes and other pipes for discharging liquids and waste liquids, which are easy to clean and maintain, and are conducive to the long-term stable operation of the equipment; the centrifuge device can perform continuous centrifugal operations, improve production efficiency and processing capacity, and is suitable for large-scale production needs. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 The present invention provides a schematic diagram of the three-dimensional structure of a crude zirconium tetrachloride purification device.

[0019] Figure 2 The present invention provides a schematic side perspective structural diagram of a crude zirconium tetrachloride purification device.

[0020] Figure 3 The present invention provides a schematic diagram of the main structure of a crude zirconium tetrachloride purification device.

[0021] Figure 4 The present invention provides a schematic side structural diagram of a crude zirconium tetrachloride purification device.

[0022] Figure 5 The present invention provides a schematic side cross-sectional structural diagram of a crude zirconium tetrachloride purification device.

[0023] Figure 6 The present invention provides a schematic diagram of the oblique cross-section structure of a crude zirconium tetrachloride purification device.

[0024] Figure 7 The present invention provides a schematic top view of the crude zirconium tetrachloride purification equipment.

[0025] Figure 8 The present invention provides a schematic top-view cross-sectional structural diagram of a crude zirconium tetrachloride purification device.

[0026] In the figure: 1. base; 2. mounting frame; 3. support shaft; 4. centrifuge cylinder; 5. main shaft; 6. guide frame; 7. spiral guide plate; 8. clear liquid pipe; 9. inlet pipe; 10. slag discharge pipe; 11. liquid discharge pipe; 12. waste liquid pipe; 13. first motor; 14. motor frame; 15. coupler; 16. driven pulley; 17. driving pulley; 18. transmission belt; 19. swing frame; 20. second motor; 21. driving gear; 22. ring gear; 23. inspection door; 24. filtrate box; 25. filter ring; 26. inner sleeve; 27. outer sleeve; 28. water hole; DETAILED DESCRIPTION

[0027] In order to further illustrate the technical means and effects adopted by the present invention to achieve the predetermined purpose of the invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. The detailed description is as follows.

[0028] See also Figures 1-8 The present invention provides a technical solution: a new process for purifying crude zirconium tetrachloride, comprising the following steps: Step 1. Dissolve: The crude zirconium tetrachloride was added to an appropriate amount of anhydrous organic solvent, and the amount of solvent was controlled so that the mass ratio of zirconium tetrachloride to solvent was 1:3. The crude zirconium tetrachloride was dissolved under stirring at 30°C for 0.8 hours to form a uniform solution to be treated. Step 2. Pretreatment: Cool the liquid to be treated to 8°C and keep it at this temperature for 50 minutes to promote the precipitation of some insoluble impurities. During this process, add an appropriate amount of precipitation aid, the amount of which is 8% of the solvent volume, to improve the precipitation effect of impurities; Step 3. Continuous centrifugation and multi-fractionation: The pre-treated liquid to be treated is sent to the crude zirconium tetrachloride purification equipment for centrifugal separation. The speed of the centrifugal device is set to 4000 rpm and the centrifugation time is 7 minutes. A multi-stage liquid separation method is used to obtain a preliminary purified liquid. Step 4. Washing: Mix the pre-purified solution with deionized water in a volume ratio of 1:1.5 and perform liquid-liquid extraction to remove water-soluble impurities. After stirring for 12 minutes, allow the mixture to stand and separate the organic phase. Repeat the above washing process three times until the pH value of the aqueous phase is neutral. Step 5. Drying: The washed organic phase was dried over anhydrous magnesium sulfate or anhydrous calcium chloride, with the amount of desiccant added being 8% of the volume of the organic phase. The mixture was stirred and dried for 45 minutes, and the desiccant was removed by filtration to obtain an anhydrous purified solution. Step 6: Solvent recovery and product acquisition: The purified solution is passed through a reduced pressure distillation apparatus, and the organic solvent is evaporated and recovered under the conditions of a vacuum degree of -0.08 MPa and a temperature of 50°C until a solid product is obtained. The obtained solid is high-purity zirconium tetrachloride.

[0029] A crude zirconium tetrachloride purification device, comprising a base 1, a pair of mounting frames 2 are fixedly mounted on the upper wall of the base 1, a support shaft 3 is rotatably mounted between the pair of mounting frames 2, a centrifugal cylinder 4 is fixedly mounted between the support shafts 3, for accommodating and processing chemical reagent raw materials, and achieving separation of solids and liquids by high-speed rotation, a centrifugal drive structure is installed on the upper end of the centrifugal cylinder 4, a main shaft 5 is rotatably mounted in the centrifugal cylinder 4, a guide frame 6 is fixedly mounted in the centrifugal cylinder 4, a spiral guide plate 7 is fixedly mounted on the guide frame 6, the guide frame 6 and the spiral guide plate 7 are used to guide and enhance the rotational flow of the liquid, thereby improving the separation efficiency, and a swing drive is installed on the mounting frame 2. Dynamic structure, the swing drive structure is used to adjust the angle of the centrifuge cylinder 4 to adapt to different operating requirements, the upper end of the side wall of the centrifuge cylinder 4 is fixedly installed with a clear liquid pipe 8, the lower end of the centrifuge cylinder 4 is fixedly installed with an input pipe 9, the lower end of the side wall of the centrifuge cylinder 4 is fixedly installed with a slag pipe 10, the upper end of the outer wall of the centrifuge cylinder 4 is fixedly installed with a discharge pipe 11, the upper end of the side wall of the centrifuge cylinder 4 is installed with a waste liquid pipe 12, the clear liquid pipe 8 is used to discharge the clear liquid after separation, the input pipe 9 is used to introduce the chemical reagent raw materials to be processed, the slag pipe 10 is used to discharge the solid residue after separation, the discharge pipe 11 is used to discharge other types of liquids, and the waste liquid pipe 12 is used to discharge waste liquid that cannot be used.

[0030] This embodiment is further configured as follows: the centrifugal drive structure includes a first motor 13, a motor frame 14 is fixedly mounted on the upper end of the centrifugal cylinder 4, the first motor 13 is fixedly mounted on the side wall of the motor frame 14, a coupler 15 is fixedly mounted on the upper end of the motor frame 14, a driven pulley 16 is fixedly mounted on the input end of the coupler 15, a driving pulley 17 is fixedly mounted on the driving end of the first motor 13, a transmission belt 18 is connected between the driving pulley 17 and the driven pulley 16, and the output end of the coupler 15 is connected to one end of the main shaft 5.

[0031] When the first motor 13 is started, the driving pulley 17 at its driving end begins to rotate, and the driving pulley 17 drives the driven pulley 16 to rotate through the transmission belt 18, thereby transmitting the power of the motor to the coupler 15. The output end of the coupler 15 is connected to the main shaft 5, and the power is transmitted to the centrifuge cylinder 4 through the main shaft, causing it to rotate at high speed. During the rotation process, the chemical reagent raw materials in the centrifuge cylinder 4 are separated from the solid and liquid due to the action of centrifugal force.

[0032] This embodiment is further configured such that the swing drive structure includes a swing frame 19, the swing frame 19 is fixedly mounted on the side wall of the support shaft 3, a second motor 20 is fixedly mounted on the lower end of the swing frame 19, a driving gear 21 is fixedly mounted on the driving end of the second motor 20, a ring gear 22 is fixedly mounted on the mounting frame 2, and the driving gear 21 is meshedly connected with the ring gear 22.

[0033] When the angle of the centrifuge cylinder 4 needs to be adjusted, the second motor 20 is started, and the driving end of the second motor 20 drives the driving gear 21 to rotate. The driving gear 21 is engaged with the ring gear 22 fixed to the mounting frame 2. The rotation of the driving gear 21 drives the swing frame 19 to rotate through the engaged ring gear. Since the swing frame 19 is fixedly mounted on the side wall of the support shaft 3, its rotation will change the angle of the centrifuge cylinder 4. The rotation of the swing frame 19 causes the angle of the centrifuge cylinder 4 to change, so that the working angle of the centrifuge cylinder 4 can be adjusted according to actual needs to optimize the centrifugal separation effect.

[0034] This embodiment is further configured such that an inspection door 23 is fixedly installed on the front wall of the centrifugal drum 4. The provision of the inspection door 23 enables operators to conveniently perform regular cleaning and maintenance work, thereby ensuring the normal operation and long life of the equipment.

[0035] This embodiment is further configured such that a filtrate box 24 is fixedly mounted on the upper wall of the centrifuge cylinder 4, a filter ring 25 is fixedly mounted in the filtrate box 24, and the clear liquid pipe 8 is fixedly mounted on the side wall of the filtrate box 24. During the centrifugation process, the separated liquid flows into the filtrate box 24 through the upper wall of the centrifuge cylinder. The liquid passes through the filter ring 25 in the filtrate box 24, and fine solid particles are retained by the filter ring, and only the clear liquid passes through the filter ring 25.

[0036] This embodiment is further configured such that the lower end of the main shaft 5 is a spiral dragon-shaped multi-strand twisted plate, and the spiral guide plate 7 is a multi-piece auger blade. The design of the spiral dragon-shaped multi-strand twisted plate can effectively transport the material from the lower end to the upper end of the centrifuge barrel 4, ensuring the uniform distribution and flow of the material in the centrifuge barrel 4. The multi-piece auger blade design can enhance the rotational flow of the material in the centrifuge barrel 4, increase the effect of the centrifugal force, and thus improve the efficiency of solid-liquid separation. This design can reduce the blockage of the material in the centrifuge barrel and ensure the continuous operation and stability of the equipment.

[0037] This embodiment is further configured such that an inner sleeve 26 is fixedly mounted on the inner upper wall of the centrifugal cylinder 4 , an outer sleeve 27 is fixedly mounted on the inner upper wall of the centrifugal cylinder 4 and outside the inner sleeve 26 , a water permeable hole 28 is opened on the outer sleeve 27 , and the outer sleeve 27 is fixedly connected to the inner side of the spiral guide plate 7 .

[0038] The material enters the centrifugal cylinder 4, and under the action of centrifugal force, the liquid and solid begin to separate. The liquid passes through the space between the inner sleeve 26 and the outer sleeve 27, and the solid particles are trapped in the outer sleeve 27. The water-permeable holes 28 allow the liquid to pass through, while larger particles are blocked. The liquid that has passed through multiple layers of filtration is guided to the clear liquid pipe 8 through the spiral guide plate 7 and finally discharged from the centrifugal cylinder. The solid particles are pushed to the outer wall of the centrifugal cylinder 4 under the action of centrifugal force and are finally discharged through the slag discharge pipe 10.

[0039] The detailed connection means are well known in the art; Figures 1-8 As shown, the working process is as follows: place the centrifugal device on a level and stable ground, and ensure that the pipes connected to the equipment are intact; prepare the chemical reagent raw materials that need to be centrifuged; connect the clear liquid pipe 8, waste liquid pipe 12, discharge pipe 11, input pipe 9 and slag discharge pipe 10 to the corresponding interfaces, and ensure that the connections are firm and leak-free; add chemical reagent raw materials: open the input pipe 9, and add the chemical reagent raw materials into the centrifuge cylinder 4 through the input pipe 9; start the equipment: operate according to the operating manual, start the first motor 13, make the main shaft 5 perform centrifugal operation, and enhance the spiral guide plate 7 Rotation effect to achieve solid sedimentation and liquid separation; liquid discharge: after centrifugal separation, the clear liquid and waste liquid are discharged through the clear liquid pipe 8 and the waste liquid pipe 12 respectively; if liquid needs to be output, start the second motor 20 to bend down the centrifuge cylinder 4 to discharge liquid and residue; adjustment operation: according to actual needs, the swing drive structure can be adjusted to perform swing operation to improve the centrifugal pretreatment effect and continuous centrifugation efficiency; after the centrifugation process is completed, turn off all motors, clean the inside of the equipment, and clean the pipelines; regularly check the operation of each component of the equipment, keep the equipment clean and tidy, and ensure the normal operation of the equipment.

[0040] The specific working method is as follows: the clear liquid pipe 8, the waste liquid pipe 12, the drain pipe 11, the input pipe 9 and the slag discharge pipe 10 are connected to the outside through a hose, the chemical reagent production raw materials are continuously fed through the input pipe 9, the first motor 13 is started, the driving end of the first motor 13 drives the active pulley 17 to rotate, the active pulley 17 drives the driven pulley 16 to rotate through the transmission belt 18, the driven pulley 16 drives the input end of the coupler 15 to rotate, the output end of the coupler 15 drives the main shaft 5 to rotate, the main shaft 5 drives the chemical reagent raw materials to rotate and centrifuge in the centrifuge box, and the spiral guide plate 7 is used to increase the outer ring rotation effect, and The settled solids are precipitated, and the internal clear liquid and the filtered liquid are discharged through the clear liquid pipe 8 and the drain pipe 11 respectively. The liquid with high impurities or that cannot be used is discharged through the waste liquid pipe 12. When the liquid is output, the driving end of the second motor 20 drives the driving gear 21 to rotate, so that the driving gear 21 is engaged with the ring gear 22 and connected to a fixed position and then locked, so that the centrifuge cylinder 4 is tilted down. After the centrifugation is completed, the clear liquid overflowed from the top is discharged. When the centrifuge cylinder 4 is tilted up, it is convenient for slag discharge, and it can swing back and forth as needed, thereby improving the effect of centrifugal pretreatment and improving the effect of continuous centrifugation.

[0041] It should be noted that, in this document, relational terms such as first and second, etc. are merely used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations.

[0042] The above description is merely a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as above in terms of a preferred embodiment, it is not intended to limit the present invention. Any person skilled in the art can, without departing from the scope of the technical solution of the present invention, make some changes or modifications to equivalent embodiments using the technical contents disclosed above. However, any brief modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution of the present invention.

Claims

1. The present invention relates to the technical field of purification technology, and specifically discloses a new process and equipment for purifying crude zirconium tetrachloride, comprising the following steps: Step 1. Dissolution; Step 2. Pretreatment; Step 3. Continuous centrifugation and multi-fractionation; Step; 4. Washing; Step 5. Drying; Step 6: Solvent Recovery and Product Acquisition. By optimizing process conditions during the dissolution, pretreatment, centrifugal separation, washing, and drying steps, such as controlling solvent dosage, temperature, time, and additive ratio, impurities are removed to the maximum extent possible, resulting in a high-purity zirconium tetrachloride product. The equipment utilizes a specially designed centrifuge cylinder with an internal guide frame and spiral guide plates, which enhance the liquid's rotational flow and improve solid-liquid separation efficiency. The lower end of the main shaft is designed with a spiral, multi-stranded, twisted plate in the shape of a dragon, combined with multiple auger blades, to improve uniformity in material transportation and distribution and reduce clogging.

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