Sponge zirconium reduction and evaporation integrated device and method

Abstract

The invention belongs to the technical field of sponge zirconium reduction, particularly relates to a sponge zirconium reduction and evaporation integrated device and a sponge zirconium reduction and evaporation integrated method, and aims to solve the problems that zirconium tetrachloride needs to be mixed with magnesium to react during magnesiothermic reduction, and the existing mixing efficiency is low, so that the production efficiency is low and the energy consumption is increased. A reduction module is arranged above the tool bottom plate and comprises a tool mounting frame, a heating frame body is mounted on the tool mounting frame, a reduction furnace body is fixedly connected to the interior of the heating frame body, and a reduction furnace sealing cover plate is connected to an opening of the reduction furnace body through a bolt; and a mounting round hole is formed in the reduction furnace sealing cover plate. The sponge zirconium reduction and evaporation integrated device and method disclosed by the invention have the effects that zirconium tetrachloride and magnesium liquid are mixed more quickly and uniformly, so that the reduction reaction effect is improved, the production efficiency is improved, and meanwhile, the energy consumption is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of zirconium sponge reduction, and in particular to a zirconium sponge reduction integrated device and method. Background Art

[0002] The reduction of zirconium sponge usually refers to the process of extracting and preparing zirconium sponge from zirconium ore or other zirconium-containing raw materials. Zirconium sponge is a porous material with a large specific surface area and pore structure, which makes it widely used in many fields, such as adsorption and separation of gases and liquids, material toughening, biomedical applications, photocatalysis and optoelectronic applications.

[0003] Zirconium sponge is an important metal material. However, in the existing zirconium sponge production process, the production steps are divided into sublimation of zirconium tetrachloride, magnesium thermal reduction of zirconium sponge and vacuum distillation. Since zirconium tetrachloride needs to be mixed with magnesium to react during magnesium thermal reduction, the existing mixing efficiency is slow, resulting in low production efficiency and increased energy consumption. Summary of the invention

[0004] The invention discloses an integrated device and method for reducing zirconium sponge, aiming to solve the technical problem in the background technology that zirconium tetrachloride needs to be mixed with magnesium to react during magnesium thermal reduction, and the existing mixing efficiency is slow, resulting in low production efficiency and increased energy consumption.

[0005] The invention provides a zirconium sponge reduction integrated device, comprising a tooling base plate, a reduction module is arranged above the tooling base plate, and the reduction module comprises a tooling installation frame, a heating frame is installed on the tooling installation frame, and the interior of the heating frame is fixedly connected to a reduction furnace body, and a reduction furnace sealing cover is connected to the opening of the reduction furnace body by bolts, a mounting circular hole is provided on the reduction furnace sealing cover, and a rotating circular tube is connected to the interior of the mounting circular hole by a bearing, and a rotating stirring support rod is fixedly connected to the exterior of the rotating circular tube, two slide grooves are provided on the rotating stirring support rod, and the interiors of the two slide grooves are both slidably connected with a hollow adjustment slide seat, one of the hollow adjustment slide seats is provided with a mounting opening facing the interior of the reduction furnace body, a hollow mounting column is fixedly connected to the interior of the mounting opening, mounting holes are equidistantly provided on the exterior of the hollow mounting column, and spray rods are fixedly connected to the interiors of the multiple mounting holes, one of the hollow adjustment slide seats is fixedly connected to a stirring and mixing column facing the interior of the reduction furnace body, and stirring plates are fixedly connected to the exterior of the stirring and mixing column at equidistant distances, and the outer walls of the multiple stirring plates are provided with flow openings.

[0006] In a preferred scheme, circular holes are provided at both ends of the rotating stirring support rod, and the interiors of the two circular holes are connected to rotating round rods through bearings, the exteriors of the two rotating round rods are fixedly connected to adjusting gears, the inner wall of the reduction furnace body is fixedly connected to a limited circular tooth frame, the tooth block end of the limited circular tooth frame is meshed with the adjusting gear, and the two hollow adjusting slides are fixedly connected to a fixed cylinder on the side away from the tooling bottom plate, one of the hollow adjusting slides is provided with a connecting port with the exterior of the rotating circular tube, and the interiors of the two connecting ports are fixedly connected to the same metal telescopic tube.

[0007] In a preferred solution, one end of the two rotating circular rods are fixedly connected with a protrusion, and the two protrusions are provided with two circular holes away from the center of the circle, the interiors of the two circular holes are connected with eccentric columns through bearings, the eccentric columns on the same side and the outside of the fixed cylinder are movably connected with the same reciprocating push-pull rod, an L support plate is connected to the reduction furnace sealing cover plate by bolts, one side of the L support plate is fixedly connected with a driving motor, the driving end of the driving motor and the outside of the rotating circular tube are fixedly connected with pulleys, and the outsides of the two pulleys are movably connected with the same belt.

[0008] In a preferred embodiment, the outside of the reduction furnace body is fixedly connected to an insulation box, and a pump body is arranged on the insulation box, the discharge end of the pump body is movably connected to the inside of the rotating circular tube through a feed pipe, a feed hole is provided on the side of the insulation box facing the tooling bottom plate, the inside of the feed hole is connected to the bottom of the reduction furnace body through a suction pipe, a feeding port is provided on the reduction furnace sealing cover plate, one side of the feeding port is connected to the feeding cover plate through a hinge, a circular hole three is provided on the reduction furnace sealing cover plate, a sealed feeding pipe two is fixedly connected to the inside of the circular hole three, a liquid material discharge pipe is fixedly connected to one side of the sealed feeding pipe two, and a gas injection connecting pipe is fixedly connected to the outside of the liquid material discharge pipe.

[0009] By providing a reduction module, when the zirconium tetrachloride and magnesium are thermally reduced, the magnesium material is first added to the reduction furnace body, and then the heating frame is started to heat the magnesium into a liquid, and then the pump body is started to suck the heated liquid magnesium into the insulation box, and at the same time the zirconium tetrachloride enters the reduction furnace body. At this time, the pump body transports the magnesium liquid to the rotating circular tube through the feed pipe, and then enters the corresponding hollow adjustment slide seat through the metal telescopic tube, and then sprays out through the spray holes on the multiple spray rods on the hollow mounting column, so that the magnesium liquid is in uniform contact with the zirconium tetrachloride, and at the same time the driving motor is started, and the belt is driven by the driving motor to rotate the rotating circular tube, so that the rotating circular tube drives the rotating stirring support rod to be circular. The rotating stirring support rod rotates in a circle, so that the spray rod under the rotating stirring support rod moves in a circle to spray the magnesium liquid, and at the same time, the stirring plate under the rotating stirring support rod stirs the zirconium tetrachloride and the magnesium liquid. When the rotating stirring support rod rotates in a circle, the adjusting gears at both ends of the rotating stirring support rod are meshed with the limit spherical gear frame, so that the adjusting gear drives the convex block to drive the reciprocating push-pull rod to drive the hollow adjusting slide to move back and forth in the slide groove on the rotating stirring support rod, so that the magnesium liquid is sprayed more evenly, and the zirconium tetrachloride and the magnesium liquid are mixed more evenly. Through the reduction module, the zirconium tetrachloride and the magnesium liquid are mixed more quickly and evenly, thereby improving the effect of the reduction reaction, improving production efficiency and reducing energy consumption.

[0010] In a preferred solution, a sublimation module is arranged above the tooling bottom plate, and the sublimation module includes a sublimation furnace body, an aisle assembly is arranged on one side of the sublimation furnace body, one end of the aisle assembly is connected to the interior of the reduction furnace body, an incision is opened on the outside of the aisle assembly, the inside of the two incisions are fixedly connected with the same filtering circular tube, and a flow monitoring regulator is arranged on the outside of the aisle assembly.

[0011] In a preferred embodiment, two notches are provided on the outside of the filter tube, and the opposite sides of the two notches are fixedly connected to the same guide cylinder, the outsides of the two guide cylinders are slidably connected to limit sealing slides, the two limit sealing slides are fixedly connected to the opposite sides of the notches with return springs, the return springs are located on the outside of the guide cylinder, and the opposite sides of the two limit sealing slides are fixedly connected to the same screening plate.

[0012] In a preferred solution, one side of the two limit sealing slides is connected to a linkage gear rod by bolts, one side of the sublimation furnace body is connected to a tooling support frame by bolts, two circular holes four are provided on one side of the tooling support frame, the interiors of the two circular holes four are connected to notched gears through bearings, one side of the tooling support frame is fixedly connected to two servo motors, the driving end of the servo motor is fixedly connected to one side of the notched gear, and the tooth block end of the notched gear is meshed with the linkage gear rod.

[0013] In a preferred embodiment, a discharge hole is provided on the outside of the filter circular tube, and a suction pump is fixedly connected to the inside of the discharge hole, a collecting box is fixedly connected to the upper side of the tooling bottom plate, the discharge end of the suction pump is connected to the inside of the collecting box through a collecting discharge pipe, and a feeding port is provided on one side of the sublimation furnace body, and a sealed feeding pipe is fixedly connected to the inside of the feeding port.

[0014] By providing a sublimation module, the reduction furnace body is connected with the sublimation furnace body through the aisle component, and the amount of zirconium tetrachloride entering the reduction furnace body is adjusted by the flow monitoring regulator. At the same time, when the zirconium tetrachloride enters the reduction furnace body through the aisle component, the zirconium tetrachloride is initially filtered through the sieve plate in the filter tube to prevent the zirconium tetrachloride from entering the reduction furnace body with impurities, thereby reducing the quality of the reduced sponge zirconium. During the screening process, the sieve plate starts the servo motor, and the notch gear is driven to rotate by the servo motor. When the tooth block end of the notch gear is engaged with the linkage gear rod, the linkage gear rod drives the limit sealing slide plate to move outside the guide cylinder. At the same time, the reset springs on both sides of the limit sealing slide plate are stretched and squeezed respectively. When the notch gear is separated from the linkage gear rod, the reset spring rebounds rapidly, so that the limit sealing slide plate drives the sieve plate to vibrate, thereby preventing the sieve plate from being blocked during screening. After the zirconium tetrachloride is transported, the suction pump is started, and the impurities filtered out of the filter tube are absorbed by the suction pump, and the impurities are transmitted to the collection box through the collection and discharge pipe.

[0015] In a preferred solution, a controller is disposed outside the heating frame, a vacuum component and a condensation component are disposed above the tooling bottom plate, and the condensation component and the vacuum component are connected via a connecting pipe.

[0016] A method for using a zirconium sponge reduction and steaming integrated device, using the zirconium sponge reduction and steaming integrated device as described above, comprising the following steps: Step 1: When thermally reducing zirconium tetrachloride and magnesium, first add the magnesium material into the reduction furnace body, then start the heating frame to heat the magnesium into liquid, and then start the pump to suck the heated liquid magnesium into the insulation box; Step 2: At the same time, zirconium tetrachloride enters the reduction furnace body. At this time, the pump body transports the magnesium liquid to the rotating circular tube through the feeding pipe, and then enters the corresponding hollow adjustment slide seat through the metal telescopic tube, and then sprays out through the spray holes on the multiple spray rods on the hollow mounting column, so that the magnesium liquid is in uniform contact with the zirconium tetrachloride; Step three, start the driving motor at the same time, and drive the belt through the driving motor to rotate the rotating circular tube, so that the rotating circular tube drives the rotating stirring support rod to rotate in a circle, so that the spray rod under the rotating stirring support rod moves in a circle to spray the magnesium liquid, and at the same time, the stirring plate under the rotating stirring support rod stirs the zirconium tetrachloride and the magnesium liquid. When the rotating stirring support rod rotates in a circle, the adjusting gears at both ends of the rotating stirring support rod are meshed with the limit spherical gear frame, so that the adjusting gear drives the protrusion to make the reciprocating push-pull rod drive the hollow adjusting slide to move back and forth in the slide groove on the rotating stirring support rod, so that the magnesium liquid is sprayed more evenly, and the zirconium tetrachloride and the magnesium liquid are mixed more evenly.

[0017] It can be seen from the above that the integrated zirconium sponge reduction and evaporation device provided by the present invention has the beneficial effects of making the zirconium tetrachloride and magnesium liquid mix more quickly and evenly, thereby improving the effect of the reduction reaction, improving production efficiency and reducing energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a schematic diagram of the main structure of a zirconium sponge reduction and evaporation integrated device proposed by the present invention; Figure 2 This is a schematic diagram of the top view of the structure of a zirconium sponge reduction and evaporation integrated device proposed by the present invention; Figure 3 This is a side structural schematic diagram of a zirconium sponge reduction and evaporation integrated device proposed by the present invention; Figure 4 for Figure 2 A schematic diagram of the enlarged structure of part A; Figure 5 This is a schematic diagram of the reduction module structure of a zirconium sponge reduction-evaporation integrated device proposed by the present invention; Figure 6 for Figure 5 A schematic diagram of the enlarged structure of part B; Figure 7 This is a schematic diagram of the structure of a reduction module of a zirconium sponge reduction-evaporation integrated device proposed by the present invention; Figure 8 This is a schematic diagram of the sublimation module structure of a zirconium sponge reduction and evaporation integrated device proposed by the present invention; Fig. 9 This is a schematic diagram of the structure of a sublimation module of a zirconium sponge reduction and evaporation integrated device proposed by the present invention; Fig.10 This is a schematic diagram of the filtering circular tube structure of a zirconium sponge reduction and evaporation integrated device proposed by the present invention.

[0019] In the figure: 1. tooling bottom plate; 2. reduction module; 201. tooling installation frame; 202. heating frame; 203. reduction furnace body; 204. reduction furnace sealing cover; 205. insulation box; 206. pump body; 207. suction pipe; 208. feeding pipe; 209. feeding cover; 210. rotating round pipe; 211. rotating stirring support rod; 212. L support plate; 213. driving motor; 214. belt; 215. limit round gear frame; 216. hollow adjustment slide; 217. metal telescopic tube; 218. hollow installation column; 219. spray rod; 220. fixed cylinder; 221. rotating round rod; 222. adjusting gear; 223. bump; 224. eccentric column; 225. Push-pull rod; 226, stirring and mixing column; 227, stirring plate; 3, sublimation module; 301, sublimation furnace body; 302, sealed feeding pipe 1; 303, aisle assembly; 304, filtering circular tube; 305, suction pump; 306, collecting and discharging pipe; 307, collecting box; 308, tooling support frame; 309, flow monitoring regulator; 310, servo motor; 311, notched gear; 312, linkage gear rod; 313, notch; 314, limit sealing slide plate; 315, guide cylinder; 316, reset spring; 317, sieve plate; 4, vacuum assembly; 5, condensation assembly; 6, connecting pipe; 7, controller; 8, sealed feeding pipe 2; 9, liquid material discharge pipe; 10, gas injection connection pipe. DETAILED DESCRIPTION

[0020] The technical solutions in the embodiments of the present invention will be described clearly and completely 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, rather than all the embodiments.

[0021] The zirconium sponge reduction integrated device disclosed in the present invention is mainly used in the scenario where zirconium tetrachloride needs to be mixed with magnesium for reaction during magnesium thermal reduction, and the existing mixing efficiency is slow, resulting in low production efficiency and increased energy consumption.

[0022] Reference Figure 1-Figure 7A sponge zirconium reduction and steaming integrated device comprises a tooling bottom plate 1, a reduction module 2 is arranged above the tooling bottom plate 1, and the reduction module 2 comprises a tooling installation frame 201, a heating frame 202 is installed on the tooling installation frame 201, and a reduction furnace body 203 is fixedly connected inside the heating frame 202, and a reduction furnace sealing cover plate 204 is connected to the opening of the reduction furnace body 203 by bolts, a mounting circular hole is opened on the reduction furnace sealing cover plate 204, and a rotating circular tube 210 is connected to the inside of the mounting circular hole by a bearing, and a rotating stirring support rod 211 is fixedly connected to the outside of the rotating circular tube 210, and a rotating stirring support rod 211 is fixedly connected to the rotating stirring support rod 211. Two slide grooves are provided, and hollow adjustment slides 216 are slidably connected inside the two slide grooves. One of the hollow adjustment slides 216 is provided with an installation opening facing the inner side of the reduction furnace body 203, and a hollow installation column 218 is fixedly connected inside the installation opening. The outside of the hollow installation column 218 is provided with installation holes at equal distances, and spray rods 219 are fixedly connected inside the multiple installation holes. One of the hollow adjustment slides 216 is fixedly connected with a stirring and mixing column 226 facing the inner side of the reduction furnace body 203, and stirring plates 227 are fixedly connected outside the stirring and mixing column 226 at equal distances, and the outer walls of the multiple stirring plates 227 are provided with flow openings.

[0023] Reference Figure 1-Figure 7 , circular holes 1 are provided at both ends of the rotating stirring support rod 211, and the interiors of the two circular holes 1 are connected to rotating round rods 221 through bearings, and the exteriors of the two rotating round rods 221 are fixedly connected to adjusting gears 222, and the inner wall of the reduction furnace body 203 is fixedly connected to a limited circular tooth frame 215, and the tooth block end of the limited circular tooth frame 215 is meshed with the adjusting gear 222, and the two hollow adjusting slides 216 are fixedly connected to a fixed cylinder 220 on the side away from the tooling bottom plate 1, and one of the hollow adjusting slides 216 is provided with a connecting port with the exterior of the rotating circular tube 210, and the interiors of the two connecting ports are fixedly connected to the same metal telescopic tube 217.

[0024] Reference Figure 1-Figure 7 One end of the two rotating rods 221 is fixedly connected with a protrusion 223, and the two protrusions 223 are opened with a circular hole 2 away from the center of the circle. The interior of the two circular holes 2 is connected with an eccentric column 224 through a bearing. The eccentric column 224 on the same side and the outside of the fixed cylinder 220 are movably connected with the same reciprocating push-pull rod 225. The reduction furnace sealing cover plate 204 is connected with an L support plate 212 by bolts, and one side of the L support plate 212 is fixedly connected with a driving motor 213. The driving end of the driving motor 213 is fixedly connected with a pulley on the outside of the rotating tube 210, and the outside of the two pulleys is movably connected with the same belt 214.

[0025] Reference Figure 1-Figure 7The outside of the reduction furnace body 203 is fixedly connected to an insulation box 205, and a pump body 206 is arranged on the insulation box 205. The discharge end of the pump body 206 is movably connected to the inside of the rotating circular tube 210 through a delivery pipe 208. A feed hole is provided on the side of the insulation box 205 facing the tooling bottom plate 1, and the inside of the feed hole is connected to the bottom of the reduction furnace body 203 through a suction pipe 207. A feeding port is provided on the reduction furnace sealing cover plate 204, and a feeding cover plate 209 is connected to one side of the feeding port through a hinge. A circular hole three is provided on the reduction furnace sealing cover plate 204, and a sealed feeding pipe two 8 is fixedly connected to the inside of the circular hole three, and a liquid material discharge pipe 9 is fixedly connected to one side of the sealed feeding pipe two 8, and a gas injection connecting pipe 10 is fixedly connected to the outside of the liquid material discharge pipe 9.

[0026] In a specific application scenario, when zirconium tetrachloride and magnesium are thermally reduced, magnesium material is first added to the reduction furnace body 203, and then the heating frame 202 is started to heat the magnesium into a liquid, and then the pump body 206 is started to suck the heated liquid magnesium into the insulation box 205, and at the same time the zirconium tetrachloride enters the reduction furnace body 203. At this time, the pump body 206 transports the magnesium liquid to the rotating circular tube 210 through the delivery pipe 208, and then enters the corresponding hollow adjustment slide 216 through the metal telescopic tube 217, and then sprays out through the spray holes on the multiple spray rods 219 on the hollow mounting column 218, so that the magnesium liquid is in uniform contact with the zirconium tetrachloride, and at the same time the drive motor 213 is started to drive the belt 214 through the drive motor 213 The rotating circular tube 210 is rotated, so that the rotating circular tube 210 drives the rotating stirring support rod 211 to rotate in a circle, so that the spray rod 219 under the rotating stirring support rod 211 moves in a circle to spray the magnesium liquid, and at the same time, the stirring piece 227 under the rotating stirring support rod 211 stirs the zirconium tetrachloride and the magnesium liquid. When the rotating stirring support rod 211 rotates in a circle, the adjusting gears 222 located at both ends thereof are meshed with the limiting round tooth frame 215, so that the adjusting gear 222 drives the protrusion 223 so that the reciprocating push-pull rod 225 drives the hollow adjusting slide 216 to move back and forth in the slide groove on the rotating stirring support rod 211, so that the magnesium liquid is sprayed more evenly, and the zirconium tetrachloride and the magnesium liquid are mixed more evenly.

[0027] Reference Figure 1 , Figure 5 , Figure 8 , Fig. 9 and Fig.10A sublimation module 3 is arranged above the tooling bottom plate 1, and the sublimation module 3 includes a sublimation furnace body 301, and an aisle component 303 is arranged on one side of the sublimation furnace body 301, one end of the aisle component 303 is connected to the inside of the reduction furnace body 203, and an incision is opened on the outside of the aisle component 303, and the inside of the two incisions is fixedly connected with the same filtering circular tube 304, and a flow monitoring regulator 309 is arranged on the outside of the aisle component 303.

[0028] Reference Figure 1 , Figure 8 , Fig. 9 and Fig.10 Two notches 313 are provided on the outside of the filtering tube 304, and the opposite sides of the two notches 313 are fixedly connected to the same guide cylinder 315, the outsides of the two guide cylinders 315 are slidably connected to the limiting sealing slides 314, the two limiting sealing slides 314 are fixedly connected to the opposite sides of the notches 313 with return springs 316, the return springs 316 are located on the outside of the guide cylinders 315, and the opposite sides of the two limiting sealing slides 314 are fixedly connected to the same screening plate 317.

[0029] Reference Figure 1 , Figure 8 , Fig. 9 and Fig.10 One side of the two limit sealing slide plates 314 is connected to the linkage gear rod 312 by bolts, one side of the sublimation furnace body 301 is connected to the tooling support frame 308 by bolts, one side of the tooling support frame 308 is provided with two circular holes four, the insides of the two circular holes four are connected with the notched gear 311 through bearings, one side of the tooling support frame 308 is fixedly connected to two servo motors 310, the driving end of the servo motor 310 is fixedly connected to one side of the notched gear 311, and the tooth block end of the notched gear 311 is meshed with the linkage gear rod 312.

[0030] Reference Figure 1 , Figure 8 , Fig. 9 and Fig.10 A discharge hole is provided on the outside of the filter circular tube 304, and a suction pump 305 is fixedly connected to the inside of the discharge hole. A collecting box 307 is fixedly connected to the upper side of the tooling bottom plate 1. The discharge end of the suction pump 305 is connected to the inside of the collecting box 307 through a collecting discharge pipe 306. A feeding port is provided on one side of the sublimation furnace body 301, and a sealed feeding pipe 302 is fixedly connected to the inside of the feeding port.

[0031] In a specific application scenario, the reduction furnace body 203 is connected to the sublimation furnace body 301 through the passage assembly 303, and the amount of zirconium tetrachloride entering the reduction furnace body 203 is adjusted by the flow monitoring regulator 309. At the same time, when the zirconium tetrachloride enters the reduction furnace body 203 through the passage assembly 303, the zirconium tetrachloride is initially filtered by the sieve plate 317 in the filter tube 304 to prevent the zirconium tetrachloride from entering the reduction furnace body 203 with impurities, thereby reducing the quality of the reduced zirconium sponge. During the sieving process, the sieve plate 317 starts the servo motor 310, and the notched gear 311 is driven to rotate by the servo motor 310. When the notched gear 31 When the tooth block end of 1 is meshed with the linkage gear rod 312, the linkage gear rod 312 drives the limiting sealing slide plate 314 to move outside the guide cylinder 315, and the return springs 316 on both sides of the limiting sealing slide plate 314 are stretched and squeezed respectively. When the notched gear 311 is separated from the linkage gear rod 312, the return spring 316 rebounds quickly, so that the limiting sealing slide plate 314 drives the sieve plate 317 to vibrate, thereby avoiding the sieve plate 317 from being blocked during sieving. After the zirconium tetrachloride is transported, the suction pump 305 is started, and the impurities filtered out of the filter tube 304 are absorbed by the suction pump 305, and the impurities are transmitted to the collection box 307 through the collection and discharge pipe 306.

[0032] Reference Figure 1 A controller 7 is disposed outside the heating frame 202 , and a vacuum component 4 and a condensation component 5 are disposed above the tooling bottom plate 1 , respectively. The condensation component 5 and the vacuum component 4 are connected via a connecting pipe 6 .

[0033] A method for using a zirconium sponge reduction and steaming integrated device, using the zirconium sponge reduction and steaming integrated device as described above, comprising the following steps: Step 1: When thermally reducing zirconium tetrachloride and magnesium, first add the magnesium material into the reduction furnace body 203, then start the heating frame 202 to heat the magnesium into liquid, and then start the pump 206 to suck the heated liquid magnesium into the insulation box 205; Step 2: At the same time, zirconium tetrachloride enters the reduction furnace body 203. At this time, the pump body 206 transports the magnesium liquid to the rotating circular tube 210 through the feeding pipe 208, and then enters the corresponding hollow adjustment slide 216 through the metal telescopic tube 217, and then sprays out through the spray holes on the multiple spray rods 219 on the hollow mounting column 218, so that the magnesium liquid is in uniform contact with the zirconium tetrachloride; Step three, start the driving motor 213 at the same time, and drive the belt 214 through the driving motor 213 to rotate the rotating tube 210, so that the rotating tube 210 drives the rotating stirring support rod 211 to rotate in a circle, so that the spray rod 219 under the rotating stirring support rod 211 moves in a circle to spray the magnesium liquid, and at the same time, the stirring blade 227 under the rotating stirring support rod 211 stirs the zirconium tetrachloride and the magnesium liquid. When the rotating stirring support rod 211 rotates in a circle, the adjusting gears 222 at both ends thereof are meshed with the limiting scallop frame 215, so that the adjusting gear 222 drives the protrusion 223 so that the reciprocating push-pull rod 225 drives the hollow adjusting slide 216 to move back and forth in the slide groove on the rotating stirring support rod 211, so that the magnesium liquid is sprayed more evenly, and the zirconium tetrachloride and the magnesium liquid are mixed more evenly.

[0034] Working principle: The reduction furnace body 203 is connected with the sublimation furnace body 301 through the passage assembly 303, and the amount of zirconium tetrachloride entering the reduction furnace body 203 is adjusted by the flow monitoring regulator 309. At the same time, when the zirconium tetrachloride enters the reduction furnace body 203 through the passage assembly 303, the zirconium tetrachloride is initially filtered by the sieve plate 317 in the filter tube 304 to prevent the zirconium tetrachloride from entering the reduction furnace body 203 with impurities. During the sieving process, the sieve plate 317 starts the servo motor 310, and the notch gear 311 is driven to rotate by the servo motor 310. When the tooth block end of the notch gear 311 is engaged with the linkage gear rod 312, the linkage gear rod 312 drives the limit seal slide The plate 314 moves outside the guide cylinder 315, and the return springs 316 on both sides of the limit sealing plate 314 are stretched and squeezed respectively. When the notched gear 311 is separated from the linkage gear rod 312, the return spring 316 rebounds quickly, so that the limit sealing plate 314 drives the sieve plate 317 to vibrate, thereby preventing the sieve plate 317 from being blocked during sieving. Then, the magnesium material is added to the reduction furnace body 203, and then the heating frame 202 is started to heat the magnesium into liquid first, and then the pump body 206 is started to suck the heated liquid magnesium into the insulation box 205, and at the same time, zirconium tetrachloride enters the reduction furnace body 203. At this time, the pump body 206 transports the magnesium liquid to the rotating circular tube 210 through the feed pipe 208. Then, it enters the corresponding hollow adjustment slide 216 through the metal telescopic tube 217, and then sprays out through the spray holes on the multiple spray rods 219 on the hollow mounting column 218, so that the magnesium liquid is in uniform contact with the zirconium tetrachloride. At the same time, the driving motor 213 is started, and the belt 214 is driven by the driving motor 213 to rotate the rotating tube 210, so that the rotating tube 210 drives the rotating stirring support rod 211 to rotate in a circle, so that the spray rod 219 under the rotating stirring support rod 211 moves in a circle to spray the magnesium liquid, and at the same time, the stirring blade 227 under the rotating stirring support rod 211 stirs the zirconium tetrachloride and the magnesium liquid. When the rotating stirring support rod 211 rotates in a circle, the adjusting gears 22 at both ends of the rotating stirring support rod 211 are at the same time. 2 is meshed with the limit scallop frame 215, so that the adjusting gear 222 drives the protrusion 223 so that the reciprocating push-pull rod 225 drives the hollow adjusting slide 216 to move back and forth in the slide groove on the rotating stirring support rod 211, so that the magnesium liquid is sprayed more evenly, and the zirconium tetrachloride and the magnesium liquid are mixed more evenly. After the zirconium tetrachloride is transported, the suction pump 305 is started, and the impurities filtered out of the filter tube 304 are absorbed by the suction pump 305, and the impurities are transmitted to the collection box 307 through the collection and discharge pipe 306. After the reduction reaction is completed, the reduction product can be vacuum distilled after the condensation component 5 and the vacuum component 4 work to obtain sponge zirconium and cool it to room temperature, and the sponge zirconium at room temperature is stored in a dry place.

[0035] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A zirconium sponge reduction and steaming integrated device, comprising a tooling bottom plate (1), characterized in that: A reduction module (2) is arranged above the tooling bottom plate (1), and the reduction module (2) comprises a tooling installation frame (201), a heating frame (202) is installed on the tooling installation frame (201), and a reduction furnace body (203) is fixedly connected to the interior of the heating frame (202), and a reduction furnace sealing cover plate (204) is connected to the opening of the reduction furnace body (203) via bolts, a mounting circular hole is provided on the reduction furnace sealing cover plate (204), and a rotating circular tube (210) is connected to the interior of the mounting circular hole via a bearing, and a rotating stirring support rod (211) is fixedly connected to the exterior of the rotating circular tube (210), and two rotating stirring support rods (211) are provided on the rotating stirring support rod (211). A slide groove, and the interiors of the two slide grooves are slidably connected with a hollow adjustment slide seat (216), one of the hollow adjustment slide seats (216) is provided with a mounting opening on the side facing the interior of the reduction furnace body (203), a hollow mounting column (218) is fixedly connected to the interior of the mounting opening, mounting holes are equidistantly provided on the exterior of the hollow mounting column (218), and spray rods (219) are fixedly connected to the interiors of the multiple mounting holes, one of the hollow adjustment slide seats (216) is fixedly connected with a stirring and mixing column (226) on the side facing the interior of the reduction furnace body (203), and stirring plates (227) are fixedly connected to the exterior of the stirring and mixing column (226) at equidistant intervals, and the outer walls of the multiple stirring plates (227) are provided with flow openings.

2. The zirconium sponge reduction and steaming integrated device according to claim 1, characterized in that: Both ends of the rotating stirring support rod (211) are provided with a circular hole, and the interiors of the two circular holes are connected to a rotating round rod (221) via a bearing, and the exteriors of the two rotating round rods (221) are fixedly connected to an adjusting gear (222), and the inner wall of the reduction furnace body (203) is fixedly connected to a limited circular tooth frame (215), and the tooth block end of the limited circular tooth frame (215) is meshed with the adjusting gear (222), and the two hollow adjusting slide seats (216) are fixedly connected to a fixed cylinder (220) on one side away from the tooling bottom plate (1), and one of the hollow adjusting slide seats (216) and the exterior of the rotating circular tube (210) are provided with a communication port, and the interiors of the two communication ports are fixedly connected to the same metal telescopic tube (217).

3. The zirconium sponge reduction and steaming integrated device according to claim 2, characterized in that: One end of the two rotating circular rods (221) is fixedly connected with a protrusion (223), and the two protrusions (223) are provided with a second circular hole away from the center of the circle. The inside of the two circular holes is connected with an eccentric column (224) through a bearing. The eccentric column (224) and the outside of the fixed cylinder (220) on the same side are movably connected with a same reciprocating push-pull rod (225). The reduction furnace sealing cover plate (204) is connected with an L support plate (212) through bolts. One side of the L support plate (212) is fixedly connected with a driving motor (213). The driving end of the driving motor (213) and the outside of the rotating circular tube (210) are fixedly connected with a pulley, and the outsides of the two pulleys are movably connected with a same belt (214).

4. The zirconium sponge reduction and steaming integrated device according to claim 3, characterized in that: The outside of the reduction furnace body (203) is fixedly connected to an insulation box (205), and a pump body (206) is arranged on the insulation box (205). The discharge end of the pump body (206) is movably connected to the inside of the rotating circular tube (210) through a feeding pipe (208). A feeding hole is provided on the side of the insulation box (205) facing the tooling bottom plate (1), and the inside of the feeding hole is connected to the bottom of the reduction furnace body (203) through a suction pipe (207). A feeding port is provided on the reduction furnace sealing cover plate (204), and one side of the feeding port is connected to a feeding cover plate (209) through a hinge. A circular hole three is provided on the reduction furnace sealing cover plate (204), and a sealed feeding pipe two (8) is fixedly connected to the inside of the circular hole three. A liquid material discharge pipe (9) is fixedly connected to one side of the sealed feeding pipe two (8), and a gas injection pipe (10) is fixedly connected to the outside of the liquid material discharge pipe (9).

5. The zirconium sponge reduction and steaming integrated device according to claim 4, characterized in that: A sublimation module (3) is arranged above the tooling bottom plate (1), and the sublimation module (3) comprises a sublimation furnace body (301), a passage assembly (303) is arranged on one side of the sublimation furnace body (301), one end of the passage assembly (303) is connected to the inside of the reduction furnace body (203), a cutout is opened on the outside of the passage assembly (303), the insides of the two cutouts are fixedly connected with a same filtering circular tube (304), and a flow monitoring regulator (309) is arranged on the outside of the passage assembly (303).

6. The zirconium sponge reduction and steaming integrated device according to claim 5, characterized in that: The filter tube (304) has two notches (313) formed on the outside, and the two notches (313) are fixedly connected to the same guide cylinder (315) on opposite sides thereof, and the two guide cylinders (315) are slidably connected to the outsides thereof with a limit sealing slide plate (314), and the two limit sealing slide plates (314) are fixedly connected to the sides opposite to the notches (313) with a return spring (316), and the return spring (316) is located on the outside of the guide cylinder (315), and the two limit sealing slide plates (314) are fixedly connected to the same sieve plate (317) on opposite sides thereof.

7. The zirconium sponge reduction and steaming integrated device according to claim 6, characterized in that: One side of the two limit sealing slide plates (314) is connected to a linkage gear rod (312) via bolts, one side of the sublimation furnace body (301) is connected to a tool support frame (308) via bolts, one side of the tool support frame (308) is provided with two circular holes four, the insides of the two circular holes four are connected to notched gears (311) via bearings, one side of the tool support frame (308) is fixedly connected to two servo motors (310), the driving end of the servo motor (310) is fixedly connected to one side of the notched gear (311), and the tooth block end of the notched gear (311) is meshed with the linkage gear rod (312).

8. The zirconium sponge reduction and steaming integrated device according to claim 7, characterized in that: The filter circular tube (304) is provided with a discharge hole on the outside, and a suction pump (305) is fixedly connected to the inside of the discharge hole; a collection box (307) is fixedly connected to the upper side of the tooling bottom plate (1); a discharge end of the suction pump (305) is connected to the inside of the collection box (307) via a collection discharge pipe (306); a feeding port is provided on one side of the sublimation furnace body (301), and a sealed feeding pipe (302) is fixedly connected to the inside of the feeding port.

9. The zirconium sponge reduction and steaming integrated device according to claim 8, characterized in that: A controller (7) is arranged outside the heating frame (202), and a vacuum component (4) and a condensation component (5) are arranged above the tooling bottom plate (1), respectively, and the condensation component (5) and the vacuum component (4) are connected via a connecting pipe (6).

10. A method for using a zirconium sponge reduction-evaporation integrated device, using the zirconium sponge reduction-evaporation integrated device according to claim 9, characterized in that: The steps include: Step 1: When thermally reducing zirconium tetrachloride and magnesium, firstly, the magnesium material is added into the reduction furnace body (203), and then the heating frame (202) is started to heat the magnesium into liquid, and then the pump (206) is started to suck the heated liquid magnesium into the heat preservation box (205); Step 2: At the same time, zirconium tetrachloride enters the reduction furnace body (203), and at this time, the pump body (206) transports the magnesium liquid to the rotating circular tube (210) through the feeding pipe (208), and then enters the corresponding hollow adjustment slide seat (216) through the metal telescopic tube (217), and then sprays out through the spray holes on the multiple spray rods (219) on the hollow mounting column (218), so that the magnesium liquid is in uniform contact with the zirconium tetrachloride; Step 3: simultaneously starting the driving motor (213), and driving the belt (214) through the driving motor (213) to rotate the rotating tube (210), so that the rotating tube (210) drives the rotating stirring support rod (211) to rotate in a circle, so that the spraying rod (219) below the rotating stirring support rod (211) moves in a circle to spray the magnesium liquid, and at the same time, the stirring blade (227) below the rotating stirring support rod (211) stirs the zirconium tetrachloride and the magnesium liquid. When the rotating stirring support rod (211) rotates in a circle, the adjusting gears (222) at both ends of the rotating stirring support rod are meshed with the limiting scalloped frame (215), so that the adjusting gear (222) drives the protrusion (223) so that the reciprocating push-pull rod (225) drives the hollow adjusting slide seat (216) to move back and forth in the slide groove on the rotating stirring support rod (211), so that the magnesium liquid is sprayed more evenly, and the zirconium tetrachloride and the magnesium liquid are mixed more evenly.

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