A still and evaporator integrated device and process for producing sponge zirconium

Abstract

The application discloses a reduction and distillation integrated device and process for producing sponge zirconium, and relates to the technical field of sponge zirconium production. The device comprises a frame, a reduction furnace fixedly connected to the frame in a penetrating manner, a distillation chamber fixedly connected to the bottom of the frame, a connecting pipe fixedly connected to the upper end of the distillation chamber, the upper end of the connecting pipe being fixedly connected to the bottom of the reduction furnace, a sealing cover being clamped to the upper end of the reduction furnace, symmetrical grooves being formed in the upper end face of the sealing cover, a stirring angle adjusting mechanism and a gas conveying mechanism. The stirring angle adjusting mechanism comprises a stirring shaft and a support frame, the support frame being fixedly connected to the upper end face of the sealing cover, the stirring shaft being rotatably connected to the support frame in a penetrating manner, and the stirring shaft penetrating the sealing cover. During the rotation of the stirring blade driven by the stirring shaft, the inclination angle of the stirring blade can be synchronously adjusted in a reciprocating manner, the laminar flow state in the stirring process can be broken, the turbulent flow degree of the mixture can be enhanced, the mixing of the zirconium tetrachloride gas and the magnesium liquid can be more sufficient and uniform, and the reaction efficiency and the product quality can be improved.

Description

Technical Field

[0001] This invention relates to the field of sponge zirconium production technology, specifically to an integrated evaporation and re-evaporation equipment and process for producing sponge zirconium. Background Technology

[0002] Sponge zirconium is a primary metallurgical product with a porous and loose structure, mainly composed of metallic zirconium. It is usually prepared by the Klauer process, which uses zircon sand as raw material, chlorinates it to obtain zirconium tetrachloride, and then reduces it with metallic magnesium in an inert atmosphere to finally obtain metallic zirconium blocks with a typical sponge-like morphology. In the existing sponge zirconium production process, the mixing of zirconium tetrachloride and magnesium is crucial. In the production of sponge zirconium, traditional integrated reduction and distillation equipment has significant shortcomings in the stirring stage. In the past, the stirring blades of the equipment could only rotate at a fixed angle. This single stirring method easily leads to a laminar flow state, resulting in insufficient and uneven mixing of zirconium tetrachloride gas and magnesium liquid, low reaction efficiency, and thus affecting product quality. Moreover, the fixed-angle stirring limits the contact area and collision frequency between materials, resulting in a slow reaction process, a long production cycle, and difficulty in improving overall production efficiency. In addition, traditional equipment cannot guarantee the uniformity of material stirring in different areas of the reduction furnace, which can easily lead to insufficient or excessive local reactions, seriously affecting the stability of product quality.

[0003] Therefore, this invention proposes an integrated equipment and process for producing sponge zirconium using a evaporation process to solve the above problems. Summary of the Invention

[0004] (a) Technical problems to be solved To address the shortcomings of existing technologies, this invention provides an integrated equipment and process for producing sponge zirconium using a evaporation process, which can effectively solve the problems in existing technologies.

[0005] (II) Technical Solution To achieve the above objectives, the present invention can be accomplished through the following technical solutions: An integrated distillation and reduction equipment for producing sponge zirconium includes a frame, a reduction furnace fixedly connected through the frame, a distillation chamber fixedly connected to the bottom of the frame, a connecting pipe fixedly connected to the upper end of the distillation chamber, the upper end of the connecting pipe fixedly connected to the bottom of the reduction furnace, a sealing cover snapped onto the upper end of the reduction furnace, and a sliding groove symmetrically formed on the upper surface of the sealing cover. The equipment also includes a stirring angle adjustment mechanism and a gas conveying mechanism. The stirring angle adjustment mechanism includes a stirring shaft and a support frame. The support frame is fixedly connected to the upper surface of the sealing cover, the stirring shaft is rotatably connected through the support frame and passes through the sealing cover, and connecting shafts are equidistantly rotatably connected to the outer surface of the stirring shaft. Stirring blades are fixedly connected to the ends of the connecting shafts away from the stirring shaft. The stirring angle adjustment mechanism is used to adjust the tilt angle of the stirring blades during the mixing of zirconium tetrachloride gas and magnesium liquid. The gas conveying mechanism is used to uniformly convey zirconium tetrachloride gas into the reduction furnace.

[0006] As a further embodiment of the present invention: Each of the connecting shafts has a fixed post fixedly connected to its outer surface; each fixed post has a through groove; each through groove has a sliding lever connected to its inner surface; each lever has a vertical plate fixedly connected to its outer surface away from the fixed post; a collar is fixedly connected between the upper ends of the vertical plates; the collar is fitted onto the outer surface of the stirring shaft; vertical grooves are symmetrically formed on the outer surface of the stirring shaft; each vertical groove has a sliding lifting plate connected to its inner surface; each lifting plate is fixedly connected to the inner sidewall of the collar; the collar passes through the sealing cover; a bushing is rotatably connected to the center of the sealing cover; and the collar is vertically slidably connected to the bushing.

[0007] As a further embodiment of the present invention: a circular ring is rotatably connected to the upper end of the outer surface of the collar, and a lifting plate is rotatably connected to both sides of the circular ring. A slider is rotatably connected to the side of the lifting plate away from the circular ring, and the slider is slidably connected in the groove.

[0008] As a further embodiment of the present invention: a horizontal plate is fixedly connected between the two sliders, a piston rod is fixedly connected to the side of the horizontal plate away from the stirring shaft, a cylinder is fixedly connected to the end of the piston rod away from the horizontal plate, and the cylinder is fixedly connected to the upper end face of the sealing cover.

[0009] As a further embodiment of the present invention: the gas delivery mechanism includes symmetrically arranged connecting pipes, which are symmetrically fixedly connected to the lower end of the stirring shaft. The stirring shaft has a gas delivery channel inside, and the connecting pipes are all connected to the gas delivery channel. Nozzles are fixedly connected at equal intervals on the outer surface of the connecting pipes. A connecting ring is rotatably connected to the upper end of the stirring shaft, and a gas delivery pipe is fixedly connected to the upper end of the connecting ring. The gas delivery pipe is connected to the gas delivery channel.

[0010] As a further embodiment of the present invention: a second bevel gear is fixedly connected to the upper end of the outer surface of the stirring shaft, a first bevel gear is meshed with one side of the second bevel gear, a protective shell is sleeved on the outer surface of the first and second bevel gears, the protective shell is fixedly connected to the upper end of the support frame, a drive shaft is fixedly connected to the side of the first bevel gear away from the second bevel gear, the drive shaft and the stirring shaft are both rotatably connected through the protective shell, a drive motor is fixedly connected to the end of the drive shaft away from the first bevel gear, and the drive motor is fixedly connected to the upper end of the support frame.

[0011] As a further embodiment of the present invention: the upper end face of the frame is symmetrically and fixedly connected with side plates, and each side plate is provided with a slide rail on the side near the sealing cover. Each slide rail is slidably connected with a lifting block, and each lifting block is fixedly connected to the sealing cover.

[0012] An integrated vaporization process for producing sponge zirconium includes the following steps: Step 1: Install and debug the operation of the integrated reduction and evaporation equipment, and add molten magnesium into the reduction furnace; Step 2: Zirconium tetrachloride gas is introduced into the reduction furnace and mixed with molten magnesium to produce sponge zirconium and magnesium chloride; Step 3: After the reaction is complete, stop the zirconium tetrachloride gas supply and heat the distillation chamber to vaporize magnesium chloride and allow it to enter the distillation chamber; Step 4: Magnesium chloride entering the distillation chamber is pre-cooled and condensed into liquid, while sponge zirconium remains inside the reduction furnace, thus completing the separation of sponge zirconium and magnesium chloride; Step 5: After the magnesium chloride in the distillation chamber has been completely condensed and collected, open the reduction furnace and collect the generated sponge zirconium product.

[0013] As a further aspect of the present invention: in step 1, the magnesium liquid is filtered before being added to the reduction furnace.

[0014] As a further aspect of the present invention: In step 5, after the generated sponge zirconium product is collected, the reduction furnace and distillation chamber are cleaned to remove residual reactants and impurities.

[0015] (III) Beneficial Effects Compared with the prior art, the present invention provides an integrated equipment and process for producing sponge zirconium, which has the following beneficial effects: By using a stirring angle adjustment mechanism, the tilt angle of the stirring blades can be adjusted simultaneously and repeatedly during the rotation of the stirring shaft. This not only breaks the laminar flow state during the stirring process and enhances the turbulence of the mixture, making the zirconium tetrachloride gas and magnesium liquid mix more thoroughly and evenly, thus improving reaction efficiency and product quality, but also increases the contact area and collision frequency between materials through multi-state stirring, accelerating the reaction process between reactants, shortening the production cycle, and improving overall production efficiency. Furthermore, the combination of stirring blades with different tilt angles ensures that materials in all areas of the reduction furnace are fully stirred, avoiding incomplete or excessive reactions in certain areas and ensuring the uniformity of the reaction.

[0016] By changing the way the cylinder pushes the piston rod, the stirring blade can be stabilized at a fixed angle, and the stirring process can be carried out according to the preset precise parameters. This ensures that the stirring effect of the material in the reduction furnace meets the specific process requirements, improves the stability and consistency of product quality, and allows for flexible adaptation to various specific process needs by stirring at specific angles at different production stages or for materials with different properties. This enhances the controllability and pertinence of the production process.

[0017] The bushing allows the collar to rotate and slide back and forth while maintaining a tight connection with the sealing cover, effectively preventing leakage of reaction gases inside the reduction furnace, ensuring a stable and safe reaction environment, and preventing external impurities from entering and affecting product quality.

[0018] The gas delivery mechanism allows the nozzles to rotate synchronously with the stirring shaft, ensuring that gaseous zirconium tetrachloride is evenly sprayed throughout the reduction furnace, guaranteeing full contact between zirconium tetrachloride and the internal materials and ensuring uniform reaction within the furnace, thus improving product quality consistency. Furthermore, the evenly sprayed gaseous zirconium tetrachloride, combined with the stirring action, further promotes material mixing, enhancing the overall mixing effect and accelerating the reaction process. The uniformly distributed gaseous zirconium tetrachloride also helps maintain a stable reaction environment within the reduction furnace, preventing excessively high or low concentrations in certain areas, providing more suitable conditions for the reaction, and improving reaction efficiency and product yield. Attached Figure Description

[0019] To facilitate understanding by those skilled in the art, the present invention will be further described below with reference to the accompanying drawings.

[0020] Figure 1 This is a schematic diagram of the overall structure of the present invention; Figure 2 This is a schematic diagram of the internal structure of the reduction furnace of the present invention; Figure 3 For the present invention Figure 2 Enlarged structural diagram of region A in the middle; Figure 4 For the present inventionFigure 2 Enlarged structural diagram of region B in the middle; Figure 5 This is a schematic diagram of the support frame and collar connection structure of the present invention; Figure 6 This is a schematic diagram of the connection structure between the stirring shaft and the gas delivery pipe of the present invention; Figure 7 This is a schematic diagram of the connection structure between the drive motor and the stirring shaft of the present invention.

[0021] In the diagram: 1. Frame; 2. Reduction furnace; 3. Distillation chamber; 4. Connecting pipe; 5. Sealing cap; 601. Stirring shaft; 602. Support frame; 603. Stirring blade; 604. Cylinder; 605. Connecting shaft; 606. Fixed column; 607. Through slot; 608. Pulley; 609. Vertical plate; 610. Bushing; 611. Piston rod; 612. Horizontal plate; 613. Sliding block; 614. Lifting plate; 615. Ring; 616. Vertical slot; 617. Lifting plate; 618. Collar; 701. Gas delivery pipe; 702. Protective shell; 703. Drive motor; 704. Connecting pipe; 705. Nozzle; 706. Connecting ring; 707. Gas delivery channel; 708. Drive shaft; 709. First bevel gear; 710. Second bevel gear; 8. Side panel; 9. Lifting block; 10. Slide rail; 11. Slide groove. Detailed Implementation

[0022] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0023] This embodiment describes an integrated steam distillation and evaporation equipment for producing sponge zirconium, such as... Figures 1-7As shown, the system includes a frame 1, a reduction furnace 2 fixedly connected through the frame 1, a distillation chamber 3 fixedly connected to the bottom of the frame 1, a connecting pipe 4 fixedly connected to the upper end of the distillation chamber 3, the upper end of the connecting pipe 4 fixedly connected to the bottom of the reduction furnace 2, a sealing cover 5 snapped onto the upper end of the reduction furnace 2, and a sliding groove 11 symmetrically opened on the upper end face of the sealing cover 5. The system also includes a stirring angle adjustment mechanism and a gas conveying mechanism. The stirring angle adjustment mechanism includes a stirring shaft 601 and a support frame 602. The support frame 602 is fixedly connected to the upper end face of the sealing cover 5. The stirring shaft 601 is rotatably connected through the support frame 602 and passes through the sealing cover 5. A connecting shaft 605 is rotatably connected annularly at equal intervals to the outer surface of the stirring shaft 601. Stirring blades 603 are fixedly connected to the end of the connecting shaft 605 away from the stirring shaft 601. The stirring angle adjustment mechanism is used to adjust the tilt angle of the stirring blades 603 during the mixing of zirconium tetrachloride gas and magnesium liquid.

[0024] In this embodiment, as Figure 2 and Figure 3 As shown, each of the connecting shafts 605 has a fixed post 606 fixedly connected to its outer surface. Each fixed post 606 has a through groove 607, and each through groove 607 has a sliding lever 608 slidably connected to it. Each lever 608 has a vertical plate 609 fixedly connected to its end away from the fixed post 606. Each vertical plate 609 has a collar 618 fixedly connected to its upper end. The collar 618 is fitted onto the outer surface of the stirring shaft 601. Each of the stirring shafts 601 has a vertical groove 616 symmetrically provided on its outer surface, and each vertical groove 616 has a lifting plate 617 slidably connected to it. The lifting plates 617 are all fixedly connected to the inner wall of the collar 618. The collar 618 passes through the sealing cover 5. The center of the sealing cover 5 is rotatably connected to the bushing 610. The collar 618 is vertically slidably connected to the bushing 610. When the collar 618 drives the vertical plate 609 to move up and down on the outer surface of the stirring shaft 601, the vertical plate 609 can drive the lever 608 to move the through groove 607 to drive one end of the fixed column 606 to move up and down reciprocally, so that the fixed column 606 moves the connecting shaft 605 to rotate reciprocally.

[0025] In this embodiment, as Figure 4 As shown, a ring 615 is rotatably connected to the upper end of the outer surface of the collar 618. A lifting plate 614 is rotatably connected to both sides of the ring 615. A slider 613 is rotatably connected to the side of the lifting plate 614 away from the ring 615. The slider 613 is slidably connected in the slide groove 11. The slide groove 11 is only opened on the surface of the sealing cover 5 and does not penetrate the sealing cover 5, so it does not affect the sealing between the sealing cover 5 and the reduction furnace 2. When the slider 613 is driven to slide in the slide groove 11, the lifting plate 614 connected between the upper end of the slider 613 and the ring 615 can drive the ring 615 to move up and down reciprocally, and move the collar 618 to move up and down reciprocally.

[0026] In this embodiment, as Figure 4As shown, a horizontal plate 612 is fixedly connected between the two sliders 613. A piston rod 611 is fixedly connected to the side of the horizontal plate 612 away from the stirring shaft 601. A cylinder 604 is fixedly connected to the end of the piston rod 611 away from the horizontal plate 612. The cylinder 604 is fixedly connected to the upper end face of the sealing cover 5. When the cylinder 604 is opened to drive the piston rod 611 to extend and retract, the horizontal plate 612 can drive the sliders 613 on both sides to slide in the slide groove 11.

[0027] Compared with existing technologies, the ability to simultaneously adjust the tilt angle of the stirring blades 603 while the stirring shaft 601 drives the stirring blades 603 to rotate and stir not only breaks the laminar flow state during the stirring process and enhances the turbulence of the mixture, making the zirconium tetrachloride gas and magnesium liquid mix more fully and evenly, thus improving reaction efficiency and product quality, but also increases the contact area and collision frequency between materials through multi-state stirring, accelerating the reaction process between reactants, shortening the production cycle, and improving overall production efficiency. Furthermore, the combination of stirring blades 603 at different tilt angles ensures that the materials in each area of ​​the reduction furnace 2 are fully stirred, avoiding insufficient or excessive local reactions and ensuring the uniformity of the reaction.

[0028] In other aspects, this embodiment also provides a gas conveying mechanism for uniformly conveying zirconium tetrachloride gas into the reduction furnace 2, such as... Figure 1 , Figure 6 and Figure 7 As shown, the gas delivery mechanism includes symmetrically arranged connecting pipes 704, which are symmetrically fixedly connected to the lower end of the stirring shaft 601. A gas delivery channel 707 is opened inside the stirring shaft 601, and the connecting pipes 704 are all connected to the gas delivery channel 707. Nozzles 705 are fixedly connected at equal intervals on the outer surface of the connecting pipes 704. A connecting ring 706 is rotatably connected to the upper end of the stirring shaft 601, and a gas delivery pipe 701 is fixedly connected to the upper end of the connecting ring 706. The gas delivery pipe 701 is connected to the gas delivery channel 707.

[0029] In this embodiment, as Figure 1 and Figure 7As shown, a second bevel gear 710 is fixedly connected to the upper end of the outer surface of the stirring shaft 601. A first bevel gear 709 is meshed with one side of the second bevel gear 710. A protective shell 702 is fitted onto the outer surfaces of the first bevel gear 709 and the second bevel gear 710. The protective shell 702 is fixedly connected to the upper end of the support frame 602. A drive shaft 708 is fixedly connected to the side of the first bevel gear 709 away from the second bevel gear 710. Both the drive shaft 708 and the stirring shaft 601 are rotatably connected to the protective shell 702. The drive shaft 708 is located away from the first bevel gear 709. A drive motor 703 is fixedly connected to one end of a bevel gear 709. The drive motor 703 is fixedly connected to the upper end of the support frame 602. When the drive motor 703 is turned on to drive the drive shaft 708 to rotate, it can drive the first bevel gear 709 connected to the output end of the drive shaft 708 to rotate. Since the first bevel gear 709 and the second bevel gear 710 are meshed with each other, the rotation of the first bevel gear 709 can drive the second bevel gear 710 to rotate synchronously, thereby driving the stirring shaft 601 to rotate.

[0030] In this embodiment, as Figure 1 As shown, the upper end of the frame 1 is symmetrically and fixedly connected to a side plate 8. Each side plate 8 is provided with a slide rail 10 on the side near the sealing cover 5. Each slide rail 10 is slidably connected to a lifting block 9. Each lifting block 9 is fixedly connected to the sealing cover 5. Through the slidable connection between the lifting block 9 and the slide rail 10, the sealing cover 5 can be driven to rise and fall.

[0031] Compared with existing technologies, the nozzle 705 can rotate synchronously with the stirring shaft 601, which not only allows the gaseous zirconium tetrachloride to be evenly sprayed throughout the reduction furnace 2, ensuring full contact between the zirconium tetrachloride and the internal materials and guaranteeing uniform reaction within the furnace, thus improving product quality consistency, but also, while the stirring blade 603 is stirring, the evenly sprayed gaseous zirconium tetrachloride can further promote the mixing between materials, complementing the stirring action, enhancing the overall mixing effect, accelerating the reaction process, and the evenly distributed gaseous zirconium tetrachloride helps maintain a stable reaction environment within the reduction furnace 2, avoiding excessively high or low local concentrations, providing more suitable conditions for the reaction, and improving reaction efficiency and product yield.

[0032] At other levels, this embodiment also provides an integrated evaporation process for producing sponge zirconium, such as... Figures 1-7 As shown, it includes the following steps: Step 1: Install and debug the operation of the integrated reduction and steaming equipment, and add magnesium liquid into the reduction furnace 2; Step 2: Zirconium tetrachloride gas is introduced into the reduction furnace 2 and mixed with molten magnesium to produce sponge zirconium and magnesium chloride; Step 3: After the reaction is complete, stop the zirconium tetrachloride gas supply and heat the distillation chamber 3 to vaporize magnesium chloride and enter the distillation chamber 3; Step 4: Magnesium chloride entering the distillation chamber 3 is pre-cooled and condensed into liquid, while sponge zirconium remains inside the reduction furnace 2, thus completing the separation of sponge zirconium and magnesium chloride. Step 5: After the magnesium chloride in distillation chamber 3 has been completely condensed and collected, open reduction furnace 2 and collect the generated sponge zirconium product.

[0033] In this embodiment, in step 1, the magnesium liquid is filtered before being added to the reduction furnace 2.

[0034] In this embodiment, after the generated sponge zirconium product is collected in step 5, the reduction furnace 2 and distillation chamber 3 are cleaned to remove residual reactants and impurities.

[0035] The overall working process and principles involved in the above embodiments are as follows: When workers need to produce sponge zirconium, they first turn on the drive motor 703 to rotate the drive shaft 708. The first bevel gear 709 connected to the drive shaft 708 and the second bevel gear 710 connected to the outer surface of the stirring shaft 601 mesh with each other, causing the stirring shaft 601 to rotate synchronously. At this time, the stirring shaft 601, through the connecting shaft 605 connected to its outer surface, drives the stirring blades 603 to rotate inside the reduction furnace 2, mixing the zirconium tetrachloride gas and magnesium liquid inside the reduction furnace 2. Then, the workers can open the cylinder 604, pushing the piston rod 611 at the output end of the cylinder 604 to move... The reciprocating motion causes the horizontal plate 612 connected to the end of the piston rod 611 away from the cylinder 604 to move horizontally back and forth. This causes the sliders 613 connected to both sides of the horizontal plate 612 to slide horizontally back and forth within the symmetrically opened grooves 11 on the upper end face of the sealing cover 5. Since the upper ends of the sliders 613 are rotatably connected to lifting plates 614, the end of the lifting plates 614 away from the sliders 613 is rotatably connected to the outer surface of the ring 615. The ring 615 is rotatably connected to the outer surface of the collar 618, and the collar 618 is slidably connected to the outer surface of the stirring shaft 601 through the lifting plate 617 and the vertical groove 616, thus, with the horizontal reciprocating motion of the sliders 613... The slider 613 pushes the lifting plate 614 to reciprocate and change its tilt angle, causing the lifting plate 614 to push the ring 615, which in turn drives the collar 618 to move up and down. At this time, the collar 618 slides on the outer surface of the stirring shaft 601 via the lifting plate 617 and the vertical groove 616. As the stirring shaft 601 rotates, it moves the lifting plate 617 via the vertical groove 616, causing the collar 618 to rotate synchronously on the ring 615. This allows the collar 618 to move up and down synchronously as it rotates with the stirring shaft 601. When 618 rotates, the collar 618 will push the bushing 610 to rotate synchronously on the sealing cover 5. When the collar 618 moves up and down, it will slide up and down synchronously on the bushing 610. Therefore, the bushing 610 can connect the collar 618 and the sealing cover 5 and improve the sealing between the collar 618 and the sealing cover 5. The design of the bushing 610 allows the collar 618 to both rotate and slide up and down and be tightly connected to the sealing cover 5, effectively preventing the leakage of reaction gas in the reduction furnace 2, ensuring the stability and safety of the reaction environment, and avoiding the entry of external impurities that affect product quality. During the reciprocating motion of the collar 618, the collar 618 drives the vertical plates 609, which are equidistantly connected on the lower end face, to move synchronously. Since each vertical plate 609 has a lever 608 connected to its side wall, and the levers 608 are slidably connected to the through slots 607 on the fixed posts 606, and the fixed posts 606 are fixed to the outer surface of the connecting shaft 605, the reciprocating motion of the collar 618 drives the levers 608 to move up and down synchronously. This causes the levers 608 to move the fixed posts 606 through the through slots 607, causing the connecting shaft 605 to rotate reciprocally on the outer surface of the stirring shaft 601. This changes the tilt angle of the stirring blades 603 connected to the stirring shaft 601, thereby causing the stirring shaft 601 to rotate more rapidly and more powerfully. During the rotation and stirring process of the stirring blade 603, the tilt angle of the stirring blade 603 can be changed simultaneously, so that the stirring blade 603 can stir and mix zirconium tetrachloride gas and magnesium liquid in different states. This not only breaks the laminar flow state during the stirring process and enhances the turbulence of the mixing, making the zirconium tetrachloride gas and magnesium liquid mix more fully and evenly, improving reaction efficiency and product quality, but also increases the contact area and collision frequency between materials, accelerates the reaction process between reactants, shortens the production cycle, and improves the overall production efficiency. Furthermore, the combination of stirring blades 603 at different tilt angles can ensure that the materials in each area of ​​the reduction furnace 2 are fully stirred, avoiding insufficient or excessive local reaction and ensuring the uniformity of the reaction. When the operator needs to tilt the stirring blade 603 to a fixed angle, the cylinder 604 can be opened to push the piston rod 611 to the designated position, and then the cylinder 604 can be closed. At this time, the piston rod 611 will fix the collar 618 at the designated height of the stirring shaft 601 through the slider 613, the lifting plate 614, and the ring 615. This allows the collar 618 to rotate the connecting shaft 605 at a designated angle on the outer surface of the stirring shaft 601 through the vertical plate 609, the lever 608, the through groove 607, and the fixing post 606. At this time, the connecting shaft 605 can be tilted to a fixed angle. The angle of the connected stirring blade 603 is fixed, so that the stirring blade 603 stirs and mixes the material inside the reduction furnace 2 at a specified angle. This not only stabilizes the stirring blade 603 at a fixed angle, so that the stirring process is carried out according to the preset precise parameters, ensuring that the stirring effect of the material inside the reduction furnace 2 meets the specific process requirements and improving the stability and consistency of product quality, but also allows for flexible adaptation to various specific process requirements and enhances the controllability and pertinence of the production process, as different production stages or materials with different properties require stirring at specific angles. During the process of stirring and mixing the materials inside the reduction furnace 2 by rotating the stirring shaft 601 and driving the stirring blades 603, the operator can transport the volatilized gaseous zirconium tetrachloride through the gas supply pipe 701 into the gas supply channel 707 inside the stirring shaft 601. Then, the gas enters along the gas supply channel 707 into the connecting pipe 704 symmetrically connected to the lower end of the stirring shaft 601, and is then sprayed out through the nozzle 705 connected to the connecting pipe 704. Because the stirring shaft 601 needs to rotate to drive the stirring blades 603 for stirring, during the process of the zirconium tetrachloride gas being transported into the reduction furnace 2 through the gas supply channel 707 inside the stirring shaft 601, the stirring shaft 601 will drive the connecting pipe 704 to rotate synchronously, causing the nozzle 705 on the connecting pipe 704 to rotate. 5. The nozzle 705 rotates synchronously inside the reduction furnace 2, evenly spraying zirconium tetrachloride gas throughout the furnace. The nozzle 705 rotates synchronously with the stirring shaft 601, which not only evenly sprays gaseous zirconium tetrachloride throughout the reduction furnace 2, ensuring that the zirconium tetrachloride is in full contact with the internal materials and that the reaction proceeds uniformly in the furnace, thus improving product quality consistency, but also, while the stirring blade 603 is stirring, the evenly sprayed gaseous zirconium tetrachloride can further promote the mixing between materials, complementing the stirring action, enhancing the overall mixing effect, accelerating the reaction process, and the evenly distributed gaseous zirconium tetrachloride helps maintain a stable reaction environment inside the reduction furnace 2, avoiding excessively high or low local concentrations, providing more suitable conditions for the reaction, and improving reaction efficiency and product yield. After the materials inside the reduction furnace 2 are stirred and mixed, the staff can vaporize magnesium chloride through the connecting pipe 4 and transport it to the distillation chamber 3 for further processing. After processing, the staff can use an external power source to drive the lifting block 9 to slide upward on the slide rail 10 opened on the side wall of the side plate 8, causing the sealing cover 5 to separate from the reduction furnace 2. After the sealing cover 5 separates from the reduction furnace 2, the staff can take out the sponge zirconium product inside the reduction furnace 2.

[0036] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to the specific implementations described. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims

1. An integrated distillation and reduction equipment for producing sponge zirconium, comprising a frame (1), a reduction furnace (2) fixedly connected through the frame (1), a distillation chamber (3) fixedly connected to the bottom of the frame (1), a connecting pipe (4) fixedly connected to the upper end of the distillation chamber (3), the upper end of the connecting pipe (4) fixedly connected to the bottom of the reduction furnace (2), a sealing cover (5) snapped onto the upper end of the reduction furnace (2), and a sliding groove (11) symmetrically opened on the upper end of the sealing cover (5), characterized in that, It also includes a stirring angle adjustment mechanism and a gas delivery mechanism; The stirring angle adjustment mechanism includes a stirring shaft (601) and a support frame (602). The support frame (602) is fixedly connected to the upper end face of the sealing cover (5). The stirring shaft (601) is rotatably connected to the support frame (602) and passes through the sealing cover (5). A connecting shaft (605) is rotatably connected to the outer surface of the stirring shaft (601) at equal intervals. A stirring blade (603) is fixedly connected to the end of the connecting shaft (605) away from the stirring shaft (601). The stirring blade (603) can automatically adjust its tilt angle during stirring.

2. The integrated steam distillation equipment for producing sponge zirconium according to claim 1, characterized in that, Each connecting shaft (605) has a fixed post (606) fixedly connected to its outer surface. Each fixed post (606) has a through groove (607). Each through groove (607) has a sliding lever (608) slidably connected to its inner surface. Each lever (608) has a vertical plate (609) fixedly connected to its outer surface away from the fixed post (606). Each vertical plate (609) has a collar (618) fixedly connected to its upper surface. The collar (618) is fitted onto the stirring shaft (605). 1) On the outer surface, vertical grooves (616) are symmetrically provided on the outer surface of the stirring shaft (601). Lifting plates (617) are slidably connected in each of the vertical grooves (616). The lifting plates (617) are fixedly connected to the inner side wall of the collar (618). The collar (618) passes through the sealing cover (5). A bushing (610) is rotatably connected at the center of the sealing cover (5). The collar (618) is vertically slidably connected to the bushing (610).

3. The integrated steam distillation equipment for producing sponge zirconium according to claim 2, characterized in that, The upper end of the outer surface of the collar (618) is rotatably connected to a ring (615), and both sides of the ring (615) are rotatably connected to a lifting plate (614). The side of the lifting plate (614) away from the ring (615) is rotatably connected to a slider (613), and the slider (613) is slidably connected in the groove (11).

4. The integrated steam distillation equipment for producing sponge zirconium according to claim 3, characterized in that, A horizontal plate (612) is fixedly connected between the two sliders (613). A piston rod (611) is fixedly connected to the side of the horizontal plate (612) away from the stirring shaft (601). A cylinder (604) is fixedly connected to the end of the piston rod (611) away from the horizontal plate (612). The cylinder (604) is fixedly connected to the upper end face of the sealing cover (5).

5. The integrated steam distillation equipment for producing sponge zirconium according to claim 1, characterized in that, The gas delivery mechanism includes symmetrically arranged connecting pipes (704), which are symmetrically fixedly connected to the lower end of the stirring shaft (601). The stirring shaft (601) has a gas delivery channel (707) inside. The connecting pipes (704) are all connected to the gas delivery channel (707). The outer surface of the connecting pipes (704) is fixedly connected with nozzles (705) at equal intervals. The upper end of the stirring shaft (601) is rotatably connected to a connecting ring (706). The upper end of the connecting ring (706) is fixedly connected to a gas delivery pipe (701). The gas delivery pipe (701) is connected to the gas delivery channel (707).

6. The integrated steam distillation equipment for producing sponge zirconium according to claim 5, characterized in that, A second bevel gear (710) is fixedly connected to the upper end of the outer surface of the stirring shaft (601). A first bevel gear (709) is meshed with one side of the second bevel gear (710). A protective shell (702) is fitted on the outer surfaces of the first bevel gear (709) and the second bevel gear (710). The protective shell (702) is fixedly connected to the upper end of the support frame (602). A drive shaft (708) is fixedly connected to the side of the first bevel gear (709) away from the second bevel gear (710). The drive shaft (708) and the stirring shaft (601) are both rotatably connected through the protective shell (702). A drive motor (703) is fixedly connected to the end of the drive shaft (708) away from the first bevel gear (709). The drive motor (703) is fixedly connected to the upper end of the support frame (602).

7. The integrated steam distillation equipment for producing sponge zirconium according to claim 1, characterized in that, The upper end of the frame (1) is symmetrically and fixedly connected with side plates (8). Each side plate (8) is provided with a slide rail (10) on the side near the sealing cover (5). Each slide rail (10) is slidably connected with a lifting block (9). Each lifting block (9) is fixedly connected to the sealing cover (5).

8. An integrated process for producing sponge zirconium, wherein the integrated process is based on an integrated equipment for producing sponge zirconium according to any one of claims 1-7, characterized in that, Includes the following steps: Step 1: Install and debug the operation status of the integrated reduction and steaming equipment, and add magnesium liquid into the reduction furnace (2); Step 2: Zirconium tetrachloride gas is introduced into the reduction furnace (2), and the zirconium tetrachloride gas is mixed with magnesium liquid to generate sponge zirconium and magnesium chloride; Step 3: After the reaction is complete, stop the supply of zirconium tetrachloride gas and heat the distillation chamber (3) to vaporize magnesium chloride and enter the distillation chamber (3); Step 4: Magnesium chloride entering the distillation chamber (3) is pre-cooled and condensed into liquid, while sponge zirconium remains inside the reduction furnace (2), thus completing the separation of sponge zirconium and magnesium chloride; Step 5: After the magnesium chloride in the distillation chamber (3) has been completely condensed and collected, open the reduction furnace (2) and collect the generated sponge zirconium product.

9. The integrated steam distillation equipment for producing sponge zirconium according to claim 1, characterized in that, In step 1, the magnesium liquid is filtered before being added to the reduction furnace (2).

10. The integrated steam distillation equipment for producing sponge zirconium according to claim 1, characterized in that, In step 5, after the generated sponge zirconium product is collected, the reduction furnace (2) and distillation chamber (3) are cleaned to remove residual reactants and impurities.

Images