A low-temperature crystallization apparatus for regenerating electrolyte in electrolytic fluorine production.

Abstract

This invention discloses a low-temperature crystallization device for regenerating electrolyte in electrolytic fluorine production, comprising: a crystallization tank, a crystallization input pipe, a swing assembly, and a temperature control component; further comprising: a swingable cooling structure, wherein the temperature control component is a coil divided into an input section, a swirl section, and a reflux section; the swingable cooling structure includes a separator membrane, a refrigerant zone, a temperature control zone, a nested cylinder, and an inner support component; and a lower rotating fixing structure, wherein the lower half of the crystallization tank is connected to several threaded channels, and the lower rotating fixing structure includes a lower rotating plate and several lower clamping plates, wherein the lower clamping plates are attached to the outer circumferential surface of the swirl section and are spaced apart. This invention can improve the automation efficiency of the crystallization process, not only reducing the crystallization waiting time but also eliminating the need for frequent manual transfer.

Description

Technical Field

[0001] This invention relates to an electrolyte regeneration device, and more particularly to a low-temperature crystallization device for regenerating electrolytes used in electrolytic fluorine production. Background Technology

[0002] Industrially, fluorine gas is produced by electrolyzing anhydrous hydrogen fluoride (HF). The electrolyte is a molten mixture (KF·2HF) made from potassium hydrogen fluoride (KHF2, containing 20.4% HF) and anhydrous hydrogen fluoride (HF). During electrolysis, the electrolyte solution corrodes the electrolytic cell and its components, causing perforations and water ingress into the inner wall. Corrosion of the electrolytic cell leads to excessive impurities in the electrolyte solution, resulting in electrolyte aging. Side reactions or impurity accumulation in the electrolyte can occur, leading to an imbalance in the proportion of effective components, directly affecting current efficiency and the purity of fluorine products. If the electrolyte is not replaced in time, irreversible electrode damage may occur due to impurity accumulation. Therefore, the electrolyte needs to be replaced after a period of use. In traditional processes, the replaced electrolyte is directly treated externally, which is not only costly to recover but also wastes a large amount of useful materials.

[0003] In the traditional process of regenerating electrolyte, an alkali is added to dissolve the electrolyte solution, and the reacted electrolyte solution is filtered. The filtered product is then crystallized and dried. During the crystallization process, existing technologies often place the filtered electrolyte solution in a crystallization tank, and then place several crystallization tanks in a crystallization chamber at the same time for crystallization. Although this can achieve the effect of constant temperature crystallization, the overall settling time is more than 24 hours, resulting in low crystallization efficiency. Furthermore, both the feeding and unloading processes require continuous manual transfer of materials, which also takes a considerable amount of time.

[0004] Therefore, this invention aims to provide a low-temperature crystallization device for regenerating electrolyte in electrolytic fluorine production. It can stably control the temperature, avoid the phenomenon of micro-crystals caused by excessive instantaneous saturation, reduce the difficulty of solid-liquid separation in the tank, and improve the automation efficiency of the crystallization process. It not only reduces the crystallization waiting time, but also eliminates the need for frequent manual transfer. Summary of the Invention

[0005] This invention provides a low-temperature crystallization apparatus for regenerating electrolyte in electrolytic fluorine production, which can effectively solve the above-mentioned problems.

[0006] This invention is implemented as follows:

[0007] A low-temperature crystallization apparatus for regenerating electrolyte in electrolytic fluorine production includes: a crystallization tank, a crystallization input pipe disposed at the top of the crystallization tank, the crystallization input pipe being connected to an electrolyte regeneration filtration device via a flow pump, a rocking assembly disposed at the center of the top of the crystallization tank, and a temperature regulating component connected to the lower end of the rocking assembly; and further includes:

[0008] The swingable cooling structure includes a temperature regulating component that is a coil, which is divided into an input section, a swirl section, and a reflux section. The swingable cooling structure includes a separator membrane disposed inside the coil, which divides the interior of the coil into a refrigerant zone and a temperature control zone. A nested cylinder is disposed at the lower end of the swing assembly. The input section is inserted into the nested cylinder, and the bottom of the reflux section extends to the center of the crystallizing tank and into the nested cylinder. An inner support member is disposed on the outer side of the reflux section, and the inner support member is attached to the inner side of the swirl section.

[0009] The lower rotating fixing structure has several threaded channels connected to the lower half of the crystallization tank. The lower rotating fixing structure includes a lower rotating plate disposed in the threaded channels. Several lower clamping pieces are disposed on the lower rotating plate. The lower clamping pieces are attached to the outer peripheral surface of the rotating section and are spaced apart.

[0010] As a further improvement, the swing assembly includes a swing motor disposed on the top surface of the crystallization tank, the lower end of the swing motor being connected to a short connecting rod, and a single pendulum restraint being disposed on the portion of the short connecting rod located outside the crystallization tank.

[0011] As a further improvement, the pendulum limiting member includes a pendulum limiting rod disposed on the outside of the short connecting rod, a limiting cylinder disposed on the outside of the pendulum limiting rod, and two one-way limiting seats disposed on the inside of the limiting cylinder.

[0012] As a further improvement, the nested cylinder is connected to the portion of the short connecting rod located inside the crystallizer. The nested cylinder includes a sleeve fixed to the short connecting rod. A suspension bracket extends outward from the bottom edge of the nested cylinder and is connected to the swirl section. The input section and the reflux section are both connected to the short connecting rod through the sleeve.

[0013] As a further improvement, the inner support member includes an inner support cylinder sleeved on the outside of the recirculation section, and the outer wall of the inner support cylinder is provided with a plurality of inner support rods, which are pressed against the lower clamping plate.

[0014] As a further improvement, the lower swivel plate includes a hollow frame for supporting the bottom surface of the return section, and an extrusion frame for supporting the return section is connected to the outside of the hollow frame. The extrusion frame is fixed on a rotating frame, and the rotating frame mates with the threaded track.

[0015] As a further improvement, the lower clamping plate includes a clamping plate vertically arranged on the extrusion frame, and a plurality of clamping hoops are provided on the inner side of the clamping plate, the clamping hoops being fitted onto the rotary section.

[0016] As a further improvement, both the beginning and end of the refrigerant zone and the temperature control zone are extended to the outside of the short connecting rod via pipelines.

[0017] The beneficial effects of this invention are:

[0018] While existing technologies can achieve constant-temperature crystallization, the overall settling time needs to exceed 24 hours, resulting in low crystallization efficiency. Furthermore, both feeding and unloading processes require continuous manual material transfer, which is time-consuming. Therefore, this invention utilizes a swing-type cooling structure to directly add the filtered electrolyte solution to the crystallization tank, allowing the solution to be cooled within the tank for crystallization. However, since static crystallization is slow, this invention allows the temperature control component to rotate cyclically under the action of the swing assembly. The oscillation of the crystals allows the electrolyte solution to sway slightly, thereby improving crystallization efficiency. However, if the cooling is too rapid, the crystals will become small and powdery, easily trapping impurities and making filtration difficult. Therefore, the temperature control component of this invention is divided into two paths. First, room temperature liquid is introduced into the temperature control zone, which restricts the amount of refrigerant that can flow into the refrigerant zone, making the cooling rate of the electrolyte solution slower. Then, the amount of liquid flowing into the temperature control zone is gradually reduced, thereby lowering the temperature and making the generated crystals more uniform and stable in size. Moreover, the entire process does not require frequent manual crystal switching, and the crystals can be generated automatically and orderly and discharged automatically.

[0019] As mentioned above, the temperature control component can be shaken by the swing assembly. However, due to its multi-layered metal ring design, it is easily damaged by rotation. Therefore, the swing assembly in this case only uses a slight swinging motion. That is, when the swing motor rotates, it is restricted by the short connecting rod and the pendulum limiter, and only rotates less than 180 degrees. This ensures that the swing amplitude is small, does not affect the static effect, and can also play a certain role in promoting crystallization.

[0020] The swaying component and the temperature regulating component need to be connected to achieve a stable swaying effect. Therefore, in this invention, the swaying component and the temperature regulating component are connected by a nested cylinder. The temperature regulating component is suspended by a suspension frame, so that it can be suspended and connected to a short connecting rod through a sleeve, thereby achieving the effect of transmitting swaying.

[0021] The outer side of the temperature control component can be supported by the inner wall of the crystallization tank, but the inner side of the temperature control component cannot be supported by other structures. Therefore, an inner support component is provided on the outer side of the reflux section of this invention. The inner support component is provided with an inner support cylinder and an inner support rod on the outer side of the reflux section, so as to fix the bottom part of the bottom of the swirl section at the inlet position, thereby ensuring the stability of the swirl section during the shaking process.

[0022] Although the swingable cooling structure can improve the crystallization effect after rotation, because the swingable cooling structure is a coil structure, it will cause downward swinging diffusion and deformation when rotating. Therefore, the present invention sets up a lower rotation fixing structure on the basis of the swingable cooling structure. First, the entire coil can be pushed upward by rotating the lower plate to make the gap between the tubes tightly fit together. Then, the bottom of the coil is supported by the restraint of the lower clamp, thereby making the bottom of the entire coil more stable and preventing damage during swinging, thus achieving a stable cooling effect.

[0023] In the process of supporting the lower rotating plate, it is not just a solid plate, nor is it just a single-end support. In this invention, the lower rotating plate is first supported by the bottom surface of the reflux section through the hollow frame, and at the edge, it is supported and fixed by the extrusion frame. Finally, the rotating frame cooperates with the threaded channel inside the crystallizer to ensure the position of the adjusted lower rotating plate, so that the lower half of the entire temperature control component is very compact. Attached Figure Description

[0024] To more clearly illustrate the technical solutions of the embodiments of the present invention, the accompanying drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of the present invention and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0025] Figure 1 This is a schematic diagram of the structure of the present invention.

[0026] Figure 2 This is a schematic diagram of the temperature regulating component of the present invention.

[0027] Figure 3 This is a schematic diagram of the structure of the recirculation section and the inner support component of the present invention.

[0028] Figure 4 This is a schematic diagram of the rotating fixed structure of the present invention.

[0029] Figure 5 This is the present invention. Figure 1 A magnified view of region C in the middle.

[0030] In the picture:

[0031] Crystallization tank 31, threaded channel 311, crystallization input pipe 32, swing assembly 33, swing motor 331, short connecting rod 332, single pendulum limiting component 333, single pendulum limiting rod 3331, limiting cylinder 3332, one-way limiting seat 3333, swingable cooling structure 34, separator membrane 341, refrigerant zone 342, temperature control zone 343, nested cylinder 344, sleeve 3441, suspension frame 3442, inner support component 345, inner support cylinder 3451, inner support rod 3452, lower rotating fixing structure 35, lower rotating plate 351, hollow frame 3511, extrusion frame 3512, rotating frame 3513, lower clamping plate 352, clamping plate 3521, clamping hoop 3522, temperature regulating component 38, input section 381, swirl section 382, ​​reflux section 383. Detailed Implementation

[0032] All embodiments of the present invention are intended to fall within the scope of protection of the present invention. Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the claimed invention, but merely to illustrate selected embodiments of the invention. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.

[0033] In the description of this invention, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating that the purpose, technical solution, and advantages of the method are clearer. The technical solutions in the embodiments of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of this invention, not all of them. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without inventive effort indicate or imply the relative importance of the indicated technical features. Therefore, features defined with "first" and "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.

[0034] Reference Figures 1-5As shown, a low-temperature crystallization device for regenerating electrolyte in electrolytic fluorine production includes: a crystallization tank 31, with a crystallization input pipe 32 at the top of the crystallization tank 31. The crystallization input pipe 32 is connected to an electrolyte regeneration filtration device via a flow pump. A swing assembly 33 is located at the center of the top of the crystallization tank 31, and a temperature regulating component 38 is connected to the lower end of the swing assembly 33. The device also includes: a swingable cooling structure 34, where the temperature regulating component 38 is a coil divided into an input section 381, a swirling section 382, ​​and a reflux section 383. The swingable cooling structure 34 includes a separating membrane 341 disposed within the coil, which divides the interior of the coil into a refrigerant zone 342 and a temperature control zone 343. The lower end of the swing assembly 33 is provided with a nested cylinder 344. The input section 381 is inserted into the nested cylinder 344, and the bottom of the reflux section 383 extends to the center of the crystallization tank 31 and into the nested cylinder 344. An inner support member 345 is provided on the outside of the reflux section 383, and the inner support member 345 is attached to the inner side of the swivel section 382. The lower rotation fixing structure 35 is provided with a plurality of threaded channels 311 connected to the lower half of the crystallization tank 31. The lower rotation fixing structure 35 includes a lower rotating plate 351 disposed in the threaded channels 311. A plurality of lower clamping pieces 352 are provided on the lower rotating plate 351. The lower clamping pieces 352 are attached to the outer peripheral surface of the swivel section 382 and are spaced apart.

[0035] In this embodiment, the temperature regulating element 38 is made of a single alloy tube. After it is made, a separator 341 is embedded inside, forming two spaces through the separator 341. Therefore, the beginning and end of the refrigerant zone 342 and the temperature control zone 343 are both extended to the outside of the short connecting rod 332 through pipelines. The refrigerant is introduced into the refrigerant zone 342, while the room temperature liquid is introduced into the temperature control zone 343. By controlling the amount of liquid introduced into the temperature control zone 343, the amount of refrigerant input can be controlled, thereby controlling the temperature of the crystallizer 31 to decrease more slowly.

[0036] While existing technologies can achieve constant-temperature crystallization, the overall settling time needs to exceed 24 hours, resulting in low crystallization efficiency. Furthermore, both feeding and unloading processes require continuous manual material transfer, which also takes considerable time. Therefore, this invention utilizes a swingable cooling structure 34 to directly add the filtered electrolyte solution into the crystallization tank 31, allowing the electrolyte solution to be cooled within the tank and thus crystallize. However, since static crystallization is slow, this invention incorporates a temperature control element 3... 8 can oscillate periodically under the drive of the oscillating component 33, thereby allowing the electrolyte solution to sway slightly, thus improving the crystallization efficiency. Furthermore, if the cooling is too rapid, the crystals will become small and powdery, easily trapping impurities and making filtration difficult. Therefore, the temperature regulating component 38 of this invention is divided into two paths. First, room temperature liquid is introduced through the temperature control zone 343, which restricts the amount of refrigerant that can flow into the refrigerant zone 342, making the cooling rate of the electrolyte solution slower. Then, the amount of liquid flowing into the temperature control zone 343 is gradually reduced, thereby lowering the temperature and making the generated crystals more uniform and stable in size.

[0037] As mentioned above, the temperature regulating component 38 can be oscillated by the swing assembly 33. However, due to its multi-layered metal ring design, it is easily damaged by rotation. Therefore, the swing assembly 33 in this embodiment includes a swing motor 331 disposed on the top surface of the crystallization tank 31. The lower end of the swing motor 331 is connected to a short connecting rod 332. The portion of the short connecting rod 332 located outside the crystallization tank 31 is provided with a pendulum limiting member 333. The swing assembly 33 only swings slightly, that is, when the swing motor 331 rotates, it is restricted by the pendulum limiting member 333 and only rotates less than 180 degrees. This ensures that the swaying amplitude is small, does not affect the static effect, and can also promote crystallization to a certain extent. In the limiting process of the pendulum limiting component 333, specifically, the pendulum limiting component 333 includes a pendulum limiting rod 3331 set outside the short connecting rod 332. A limiting cylinder 3332 is set outside the pendulum limiting rod 3331. Two one-way limiting seats 3333 are set inside the limiting cylinder 3332. The two one-way limiting seats 3333 are used for limiting and fixing, thereby ensuring that the pendulum limiting rod 3331 can be subject to a certain limiting effect when swinging, even if the swing motor 331 is not precise enough.

[0038] The swaying assembly 33 and the temperature regulating component 38 need to be connected to achieve a stable swaying effect. Therefore, in this invention, the nested cylinder 344 is connected to the part of the short connecting rod 332 located inside the crystallization tank 31. The nested cylinder 344 includes a sleeve 3441 fixed to the short connecting rod 332. A suspension frame 3442 extends outward from the bottom edge of the nested cylinder 344. The suspension frame 3442 is connected to the swivel section 382. The input section 381 and the reflux section 383 are both connected to the short connecting rod 332 through the sleeve 3441. The swaying assembly 33 and the temperature regulating component 38 are connected through the nested cylinder 344. The temperature regulating component 38 is suspended by the suspension frame 3442, so that the temperature regulating component 38 can be suspended and connected to the short connecting rod 332 through the sleeve 3441, thereby achieving the effect of transmitting swaying.

[0039] The outer side of the temperature regulating component 38 can be supported by the inner wall of the crystallizing tank 31, but the inner side of the temperature regulating component 38 cannot be supported by other structures. Therefore, the inner support component 345 of the present invention includes an inner support cylinder 3451 sleeved on the outer side of the reflux section 383. The outer wall of the inner support cylinder 3451 is provided with a plurality of inner support rods 3452. The inner support rods 3452 are pressed against the lower clamping plate 352. The inner support component 345 includes the inner support cylinder 3451 sleeved on the outer side of the reflux section 383. The inner support cylinder 3451 has several inner support rods 3452 on its outer wall. The inner support rods 3452 are pressed against the lower clamping plate 352. An inner support member 345 is provided on the outer side of the return section 383. The inner support member 345 is provided with the inner support cylinder 3451 and the inner support rods 3452 on the outer side of the return section 383, so as to fix the bottom part of the wire inlet position of the swivel section 382, ​​thereby ensuring the stability of the swivel section 382 during the shaking process.

[0040] Although the swingable cooling structure 34 can improve the crystallization effect after rotation, since the swingable cooling structure 34 is a coil structure, it will experience downward swinging diffusion and deformation when rotating. Therefore, the present invention sets up a lower rotating fixing structure 35 on the basis of the swingable cooling structure 34. First, the entire coil can be pushed upward by the upward rotation of the lower rotating plate 351, so that the gap between the tubes is tightly fitted. Then, the bottom of the coil is supported by the restraint of the lower clamp 352, so that the bottom of the entire coil is more stable and will not be damaged when swinging, thus achieving a stable cooling effect.

[0041] During the support process of the lower rotating plate 351, it is not merely a solid plate, nor is it simply supported at one end. In this invention, the lower rotating plate 351 includes a hollow frame 3511 for supporting the bottom surface of the reflux section 383. An extrusion frame 3512 for supporting the reflux section 382 is connected to the outside of the hollow frame 3511. The extrusion frame 3512 is fixed on a rotating frame 3513. The rotating frame 3513 cooperates with the threaded channel 311. The lower rotating plate 351 first supports the bottom surface of the reflux section 383 through the hollow frame 3511, and at the edge, it is supported and fixed by the extrusion frame 3512. Finally, the rotating frame 3513 cooperates with the threaded channel 311 inside the crystallizer 31 to ensure the position of the adjusted lower rotating plate 351, thereby making the lower half of the entire temperature regulating component 38 very compact.

[0042] Based on the lower swivel plate 351, the lateral direction of the return section 383 is limited by the lower clamping plate 352. The return section 383 of the arc segment is limited by the clamping hoop 3522 set on the inner side, and is supported by the inner support rod 3452, thereby ensuring the stability of the entire lower swing position.

[0043] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the invention by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of the invention should be included within the scope of protection of the invention.

Claims

1. A low-temperature crystallization apparatus for regenerating electrolyte in electrolytic fluorine production, characterized in that, The utility model relates to a crystallization tank (31) top is provided with a crystallization input pipe (32), and the crystallization input pipe (32) is connected with electrolyte regeneration filtering device through a flow pump, the utility model relates to a crystallization tank (31) top center is provided with a swing assembly (33), and the lower end of swing assembly (33) is connected with a temperature adjusting part (38), and the temperature adjusting part (38) is a coil pipe, and the coil pipe is divided into input section (381), convolution section (382) and backflow section (383), the utility model relates to a crystallization tank (31) top surface swing motor (331) of setting, and the lower end of swing motor (331) is connected with a short connecting rod (332), and the part of short connecting rod (332) outside crystallization tank (31) is provided with a simple pendulum limiting part (333), the utility model relates to a simple pendulum limiting part (333) setting outside short connecting rod (332) simple pendulum limiting rod (3331), and the outside of simple pendulum limiting rod (3331) is provided with a limiting cylinder (3332), and the inside of limiting cylinder (3332) is provided with two one-way limiting seats (3333), the utility model relates to a swingable cooling structure (34), and the swingable cooling structure (34) includes a separation membrane (341) disposed within the coil pipe, the separation membrane (341) divides the interior of the coil pipe into a refrigerant zone (342) and a temperature control zone (343), the lower end of the swing assembly (33) is provided with a nested cylinder (344), the input section (381) is inserted into the nested cylinder (344), and the bottom of the backflow section (383) extends to the center of the crystallization tank (31) and extends into the nested cylinder (344), the inner side of the convolution section (382) is attached to the outer side of the backflow section (383) by an inner support (345), the lower half of the interior of the crystallization tank (31) is connected to a plurality of threaded channels (311), the lower rotating fixing structure (35) includes a lower rotating plate (351) disposed within the threaded channel (311), a plurality of lower clamping pieces (352) are disposed on the lower rotating plate (351), the outer peripheral surface of the convolution section (382) is attached to the lower clamping pieces (352), and the lower clamping pieces (352) are spaced apart from each other. The nested cylinder (344) is connected to the part of the short connecting rod (332) inside the crystallization tank (31), the nested cylinder (344) includes a sleeve (3441) fixed to the short connecting rod (332), the bottom of the nested cylinder (344) extends outwardly to a hanging bracket (3442), the hanging bracket (3442) is connected to the convolution section (382), and the input section (381) and the backflow section (383) are connected to the short connecting rod (332) through the sleeve (3441). ​ ​ ​ ​ ​ 2. The low-temperature crystallization device for regenerating electrolyte solution for electrolysis of fluorine according to claim 1, characterized in that, ​ 3. The low-temperature crystallization device for regenerating electrolyte solution for electrolysis of fluorine according to claim 1, characterized in that, The inner support (345) comprises an inner support cylinder (3451) sleeved outside the return flow section (383), and an outer wall of the inner support cylinder (3451) is provided with a plurality of inner support rods (3452) which are pressed on the lower clamping piece (352).

4. The low-temperature crystallization apparatus for regenerating electrolyte solution for electrolysis of fluorine according to claim 1, characterized by The lower rotating plate (351) comprises a hollow frame (3511) for supporting a bottom surface of the return flow section (383), an outer side of the hollow frame (3511) is connected with an extrusion frame (3512) for supporting the return flow section (382), the extrusion frame (3512) is fixed on a rotating frame (3513), and the rotating frame (3513) is matched with the screw thread channel (311).

5. The low temperature crystallization apparatus for regenerating electrolyte solution for electrolysis of fluorspar according to claim 1, wherein The lower clamping piece (352) comprises a clamping piece (3521) vertically arranged on the extrusion frame (3512), an inner side of the clamping piece (3521) is provided with a plurality of clamping hoops (3522), and the clamping hoops (3522) are attached to the return flow section (382).

6. The low-temperature crystallization apparatus for regenerating electrolyte solution for electrolysis of fluorspar according to claim 1, wherein The cold medium area (342) and the temperature control area (343) are both extended to the outside of the short connecting rod (332) through pipelines at the head and tail ends.

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