A process for the crystallization of large particle ammonium perchlorate

By combining vacuum distillation crystallization and filtration through a specific membrane, along with flipping and tapping operations, the problems of low filtration efficiency and breakage of large-particle ammonium perchlorate crystals were solved, achieving rapid filtration and efficient cleaning, thus meeting the needs of high-efficiency production.

CN116650995BActive Publication Date: 2026-01-06DALIAN GAOJIA CHEM
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Patent Information

Application Number
CN202310677272.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-06-09
Publication Date
2026-01-06
Estimated Expiration
2043-06-09

AI Technical Summary

Technical Problem

Existing technologies for preparing large-particle ammonium perchlorate crystals suffer from low filtration efficiency and are prone to breakage, resulting in high water content after filtration, which makes it difficult to meet the requirements of high-efficiency production.

Method used

After being crystallized by vacuum distillation, the material is filtered through a filter membrane in a specific state. Combined with flipping and tapping operations, along with conveying, washing, and drying mechanisms, it achieves breakage-proof filtration and efficient cleaning.

Benefits of technology

It enables rapid filtration and efficient cleaning of large-particle ammonium perchlorate crystals, improves filtration efficiency, reduces water content, and meets the requirements of high-efficiency production.

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Abstract

The application relates to the field of ammonium perchlorate, and discloses a large-particle ammonium perchlorate crystallization treatment process, which comprises the following steps: S1: filtering a recovery solution to prepare an ammonium perchlorate solution; S2: performing vacuum distillation crystallization on the ammonium perchlorate solution; S3: continuously transferring a mixed solution containing crystals into a filtering device, and performing anti-breaking filtering treatment on the crystals by the filtering device; S4: performing drying treatment on the ammonium perchlorate crystals after filtering; and S5: performing quality inspection on the dried ammonium perchlorate, and the product is qualified if the particle size meets the requirements, and the unqualified product is recycled. The large-particle ammonium perchlorate crystallization treatment process can perform large-particle crystallization treatment on an ammonium perchlorate recovery solution, can realize rapid filtering of the crystals, and can perform efficient and rapid cleaning treatment on a filtering membrane.
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Description

Technical Field

[0001] This invention relates to the field of ammonium perchlorate, and more specifically, to a crystallization process for large-particle ammonium perchlorate. Background Technology

[0002] Ammonium perchlorate is an inorganic compound with the chemical formula NH₄ClO₄. It is a white crystalline powder and is hygroscopic. Ammonium perchlorate is a strong oxidizing agent; it can explode when mixed with reducing agents, organic matter, flammable materials such as sulfur, phosphorus, or metal powders. Contact with strong acids poses a risk of combustion and explosion. It is used in the manufacture of explosives and fireworks, and as an analytical reagent.

[0003] Depending on the requirements, different structures of ammonium perchlorate crystals are needed. Currently, when preparing large-particle, porous crystals, large-particle ammonium perchlorate crystals can be crystallized using a recycled ammonium perchlorate solution. After crystallization, the crystals need to be filtered first and then dried to avoid direct drying, which results in excessively high levels of impurities remaining in the recycled solution. However, current filtration methods use pressure or extrusion filtration, which can cause large-particle crystals to break. Direct filtration has lower filtration efficiency and higher water content. Summary of the Invention

[0004] To address the aforementioned technical problems, this invention provides a process for crystallizing large-particle ammonium perchlorate, comprising the following steps:

[0005] S1: The recovered solution is filtered to obtain ammonium perchlorate solution;

[0006] S2: Crystallize the ammonium perchlorate solution by vacuum distillation;

[0007] S3: The mixed solution containing crystals is continuously transferred into the filtration equipment, which performs anti-breakage filtration on the crystals;

[0008] S4: Dry the filtered ammonium perchlorate crystals;

[0009] S5: After drying, ammonium perchlorate is inspected. If the particle size meets the requirements, it is considered a qualified product. Unqualified products are recycled.

[0010] Furthermore: In S3, the process of the filtration equipment performing anti-breakage filtration of the solution is as follows:

[0011] S31: First, adjust the horizontally distributed filter membrane in the filtration device from a flat state to a concave state;

[0012] S32: Then, a measured amount of the solution containing the crystals is discharged into the concave part of the filter membrane;

[0013] S33: Rotate the filter membrane to ensure that the solution fully covers the surface of the filter membrane;

[0014] S34: Adjust the concave filter membrane to a flat state and rotate the filter membrane back and forth;

[0015] S35: After filtration is complete, the flat filter membrane is flipped over and tapped to cause the filtered crystals attached to the surface of the filter membrane to detach from the filter membrane, thus achieving unloading.

[0016] S36: After unloading, the filter membrane flips back, then rotates the filter membrane to transfer it to the cleaning tank. The filter membrane is continuously rotated, shaken, and tapped on the back to clean it.

[0017] S37: Remove the filter membrane from the washing tank, return it to a flat state, and then dry it.

[0018] Furthermore: the filtration equipment includes a conveying mechanism, a liquid transfer mechanism, a material transfer mechanism, a cleaning mechanism, and a drying mechanism, which are distributed at intervals along the conveying direction of the conveying mechanism;

[0019] The conveying mechanism is equipped with a filtering mechanism, which is distributed at equal intervals along the conveying mechanism. The filtering mechanism includes two parallel support rods, each with a filter membrane. One end of each support rod is mounted on a support arm, and the support rods and support arms are arranged perpendicularly. A shaft is fixedly mounted at both ends of the support arm, and the A shaft is rotatably mounted on a support base. The axial direction of the A shaft is consistent with the length direction of the support rod. The two support arms have gears at their close ends, and the two gears mesh. The support arm is connected to the A passive component. A support shaft is fixedly mounted on the support base, and the axial direction of the support shaft is consistent with the axial direction of the A shaft. The support shaft is connected to the B passive component. The conveying mechanism is equipped with an A trigger component and a B trigger component, which are arranged correspondingly to the A passive component, and the B trigger component and the B passive component are also arranged correspondingly.

[0020] Furthermore: Passive component A includes a lifting rod and a guide sleeve. The guide sleeve is fixedly installed on the support base, and the lifting rod is slidably installed inside the guide sleeve. The length direction of the lifting rod is perpendicular to the axis of A. The lower end of the lifting rod is hinged to one end of a connecting rod via a hinge shaft, and the other end of the connecting rod is hinged to a support arm via a hinge shaft. The axis of the hinge shaft is consistent with the axis of A. The lower end of the lifting rod is also equipped with rack A, which meshes with gear A. Gear A is installed at one end of drive shaft A. The support shaft is a hollow shaft, and drive shaft A is inserted inside the support shaft. The end of drive shaft A away from gear A extends out of the support shaft, and passive gear A is installed at the extended end of drive shaft A.

[0021] Furthermore: the A triggering component includes an A triggering rack, and the A triggering rack and the A driven gear are arranged accordingly. The A triggering rack is respectively arranged at the corresponding positions of the liquid transfer mechanism, the cleaning mechanism and the drying mechanism.

[0022] Furthermore, the B passive component includes a B passive gear and a counterweight. The B passive gear is installed at the end of the support shaft away from the support base, and the counterweight is installed at the end near the B passive gear. The counterweight is used to maintain the support base in a horizontal state.

[0023] Furthermore: The B triggering component includes a B triggering rack, which is arranged in the area between the liquid transfer mechanism and the material transfer mechanism, and in the corresponding arrangement with the cleaning mechanism and the drying mechanism. Several sets of B triggering racks are provided, and the B triggering racks and B driven gears are arranged correspondingly. Each set of B triggering racks is distributed at intervals along the conveying direction of the conveying mechanism.

[0024] Furthermore: a guide groove is provided on the support arm along its length direction, and a slider is slidably installed in the guide groove. The end of the support rod is installed on the slider, and the slider is connected to the C passive component. The conveying mechanism is also equipped with a C trigger component. The C passive component and the C trigger component are arranged correspondingly. The C passive component is used to drive the slider to move in the guide groove.

[0025] Furthermore: The C passive component includes a spring and a passive component, one end of which is fixedly connected to the slider, and the other end of the spring is fixedly mounted on the support arm. The spring is used to apply an elastic force away from the gear part to the slider along the length of the support arm. The passive component includes two guide wheels, a winding wheel, and a pull rope. The two guide wheels and the two sliders are arranged correspondingly. The two guide wheels and the winding wheel are rotatably mounted on the support base. The rotation axis of the two guide wheels is collinear with the axis of rotation of the A shaft. One end of the pull rope is fixedly mounted on the slider, and the other end passes through the guide wheel and is wound around the winding wheel. The rotation axis of the winding wheel is parallel to the rotation axis of the guide wheel. The C passive gear is mounted on the winding wheel.

[0026] Furthermore, the C-trigger assembly includes a C-trigger rack, which is arranged at the corresponding positions of the cleaning mechanism and the drying mechanism. The C-trigger rack and the C-driven gear are arranged correspondingly, and the C-trigger rack is distributed at intervals along the conveying direction of the conveying mechanism.

[0027] Furthermore, the support base is also equipped with a toggle assembly, which includes a lever. The lever is arranged along the length of the support rod, and one end of the lever is connected to a rotating shaft through a support rod. The rotating shaft is rotatably mounted on the support base, and a D driven gear is installed on the rotating shaft. The D driven gear and the D trigger rack are arranged correspondingly, and the D trigger rack is arranged in positions corresponding to the material transfer mechanism, the cleaning mechanism, and the drying mechanism.

[0028] Furthermore: the middle of the support shaft is rotatably mounted on the movable seat, and both ends of the movable seat are rotatably mounted in the bearing housing via the horizontal shaft. The horizontal shaft and the support shaft are arranged perpendicularly, and the horizontal shaft is arranged along the conveying direction of the conveying mechanism. The bearing housing is mounted on the conveying mechanism, which is used to drive the bearing housing to move. A passive rod is mounted on the horizontal shaft, and the passive rod, the support shaft, and the horizontal shaft are all vertically distributed. A ball head is mounted on the upper end of the passive rod. The conveying mechanism is also equipped with a limit guide rail, and the passive rod is installed in the limit guide rail. The passive rod and the ball head abut against the limit guide rail, and the passive rod and the ball head slide and guide with it along the track of the limit guide rail. The limit guide rail includes a limit section A, a transition section, and a limit section B. The limit section A is used to keep the passive rod upright, the limit section B is used to keep the passive rod horizontal, the transition section is used to connect the limit section A and the limit section B, and the limit section B is arranged at the corresponding position of the cleaning mechanism.

[0029] The beneficial effects of this invention are as follows: the large-particle ammonium perchlorate crystallization process proposed in this invention can perform large-particle crystallization treatment on ammonium perchlorate recovery solution, achieve rapid filtration of the crystals, and perform efficient and rapid cleaning of the filter membrane. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the process steps for crystallizing large-particle ammonium perchlorate proposed in this invention;

[0031] Figure 2 This is a schematic diagram of the filtration equipment in the large particle ammonium perchlorate crystallization process proposed in this invention;

[0032] Figure 3 This is a schematic diagram of the filtration mechanism inside the filtration equipment in the large particle ammonium perchlorate crystallization process proposed in this invention;

[0033] Figure 4 This is a schematic diagram of the structure of passive component A in the filtration equipment of a large-particle ammonium perchlorate crystallization process proposed in this invention;

[0034] Figure 5 This is a schematic diagram of the structure of passive component C in the filtration equipment of a large-particle ammonium perchlorate crystallization process proposed in this invention;

[0035] Figure 6 This is a schematic diagram of the structure of the A trigger rack inside the filtration equipment in the large particle ammonium perchlorate crystallization process proposed in this invention;

[0036] Figure 7 This is a schematic diagram of the structure of the B trigger rack in the filtration equipment of a large-particle ammonium perchlorate crystallization process proposed in this invention;

[0037] Figure 8This is a schematic diagram of the A trigger rack and B trigger rack corresponding to the cleaning mechanism and drying mechanism in the filtration equipment of the large particle ammonium perchlorate crystallization process proposed in this invention.

[0038] Figure 9 This is a schematic diagram of the structure of the C-trigger gear, D-trigger gear, C-trigger rack, and C-trigger rack passive assembly in the filtration equipment of a large-particle ammonium perchlorate crystallization process proposed in this invention.

[0039] In the diagram: 100, Conveying mechanism; 110, A trigger gear; 120, B trigger gear; 130, C trigger gear; 140, D trigger gear; 150, Limiting guide rail; 200, Filtering mechanism; 210, Support rod; 220, Filter membrane; 230, Support arm; 231, Guide sleeve; 232, Lifting rod; 233, A gear; 234, A rack; 235, A drive shaft; 236, A driven gear; 237, Connecting rod; 240, Support base; 250, Support shaft; 251, B driven gear. 252. Counterweight; 260. C Passive Component; 261. Guide Groove; 262. Slider; 263. Spring; 264. Pull Rope; 265. Guide Wheel; 266. Winding Wheel; 267. C Passive Gear; 270. Actuating Component; 271. Lever; 272. Rotating Shaft; 273. D Passive Gear; 280. Movable Seat; 281. Horizontal Shaft; 282. Passive Rod; 283. Ball Head; 284. Bearing Seat; 300. Liquid Transfer Mechanism; 400. Material Transfer Mechanism; 500. Cleaning Mechanism; 600. Drying Mechanism. Detailed Implementation

[0040] The subject matter described herein will now be discussed with reference to exemplary embodiments. It should be understood that these embodiments are discussed to enable those skilled in the art to better understand and implement the subject matter described herein. Changes may be made to the function and arrangement of the elements discussed without departing from the scope of this specification. Various processes or components may be omitted, substituted, or added as needed in the examples. Furthermore, features described in some examples may be combined in other examples. Example

[0041] Reference Appendix Figure 1 This embodiment proposes a crystallization process for large-particle ammonium perchlorate, including the following steps:

[0042] S1: The recovered solution is filtered to obtain ammonium perchlorate solution;

[0043] S2: Crystallize the ammonium perchlorate solution by vacuum distillation;

[0044] S3: The mixed solution containing crystals is continuously transferred into the filtration equipment, which performs anti-breakage filtration on the crystals;

[0045] S4: Dry the filtered ammonium perchlorate crystals;

[0046] S5: After drying, ammonium perchlorate is inspected. If the particle size meets the requirements, it is considered a qualified product. Unqualified products are recycled.

[0047] In S3, the process of the filtration equipment performing anti-breakage filtration of the solution is as follows:

[0048] S31: First, adjust the horizontally distributed filter membrane in the filtration device from a flat state to a concave state;

[0049] S32: Then, a measured amount of the solution containing the crystals is discharged into the concave part of the filter membrane;

[0050] S33: Rotate the filter membrane to ensure that the solution fully covers the surface of the filter membrane;

[0051] S34: Adjust the concave filter membrane to a flat state and rotate the filter membrane back and forth;

[0052] S35: After filtration is complete, the flat filter membrane is flipped over and tapped to cause the filtered crystals attached to the surface of the filter membrane to detach from the filter membrane, thus achieving unloading.

[0053] S36: After unloading, the filter membrane flips back, then rotates the filter membrane to transfer it to the cleaning tank. The filter membrane is continuously rotated, shaken, and tapped on the back to clean it.

[0054] S37: Remove the filter membrane from the washing tank, return it to a flat state, and then dry it. Example

[0055] Reference Appendix Figures 2-9 In this embodiment, a filtration device applied in Embodiment 1 is proposed. The filtration device includes a conveying mechanism 100, a liquid transfer mechanism 300, a material transfer mechanism 400, a cleaning mechanism 500, and a drying mechanism 600. The liquid transfer mechanism 300, the material transfer mechanism 400, the cleaning mechanism 500, and the drying mechanism 600 are distributed at intervals along the conveying direction of the conveying mechanism 100.

[0056] A filter mechanism 200 is mounted on the conveying mechanism 100. The filter mechanisms 200 are distributed at equal intervals along the conveying mechanism 100. The filter mechanism 200 includes two parallel support rods 210. A filter membrane 220 is mounted on the two support rods 210. One end of each support rod 210 is mounted on a support arm 230. The support rods 210 and the support arms 230 are vertically distributed. An A-axis is fixedly mounted at both ends of the support arm 230. The A-axis is rotatably mounted on a support seat 240. The axial direction of the A-axis is consistent with the length direction of the support rods 210. The two support arms 230 have gears at their close ends. The two gears mesh. The support arm 230 is connected to the A passive component. A support shaft 250 is fixedly mounted on the support seat 240. The axial direction of the support shaft 250 is consistent with the axial direction of the A-axis. The support shaft 250 is connected to the B passive component. An A trigger component and a B trigger component are mounted on the conveying mechanism 100. The A trigger component and the A passive component are arranged correspondingly. The B trigger component and the B passive component are arranged correspondingly.

[0057] Passive component A includes a lifting rod 232 and a guide sleeve 231. The guide sleeve 231 is fixedly mounted on the support base 240. The lifting rod 232 is slidably mounted inside the guide sleeve 231. The length direction of the lifting rod 232 is perpendicular to the axis of A. The lower end of the lifting rod 232 is hinged to one end of a connecting rod 237 via a hinge shaft. The other end of the connecting rod 237 is hinged to a support arm 230 via a hinge shaft. The axis of the hinge shaft is consistent with the axis of A. The lower end of the lifting rod 232 is also equipped with an A rack 234. The A rack 234 meshes with an A gear 233. The A gear 233 is mounted on one end of the A drive shaft 235. The support shaft 250 is a hollow shaft. The A drive shaft 235 is inserted inside the support shaft 250. The end of the A drive shaft 235 away from the A gear 233 extends out of the support shaft 250. The extended end of the A drive shaft 235 is equipped with an A passive gear 236.

[0058] The A trigger assembly includes an A trigger rack 110, which is arranged in correspondence with the A driven gear 236. The A trigger rack 110 is arranged at positions corresponding to the liquid transfer mechanism 300, the cleaning mechanism 500, and the drying mechanism 600.

[0059] The passive component B includes a passive gear 251 and a counterweight 252. The passive gear 251 is mounted on the end of the support shaft 250 away from the support base 240, and the counterweight 252 is mounted on the end near the passive gear 251. The counterweight 252 is used to maintain the support base 240 in a horizontal state.

[0060] The B trigger assembly includes a B trigger rack 120, which is arranged in the area between the liquid transfer mechanism 300 and the material transfer mechanism 400, and in a corresponding arrangement with the cleaning mechanism 500 and the drying mechanism 600. Several sets of B trigger racks 120 are provided, and the B trigger racks 120 and the B driven gear 251 are arranged correspondingly. Each set of B trigger racks 120 is distributed at intervals along the conveying direction of the conveying mechanism 100.

[0061] A guide groove 261 is provided on the support arm 230 along its arm length direction. A slider 262 is slidably installed in the guide groove 261. The end of the support rod 210 is installed on the slider 262. The slider 262 is connected to the C passive component 260. A C trigger component is also installed on the conveying mechanism 100. The C passive component 260 and the C trigger component are arranged correspondingly. The C passive component 260 is used to drive the slider 262 to move in the guide groove 261.

[0062] The passive component 260 includes a spring 263 and a passive component. One end of the spring 263 is fixedly connected to the slider 262, and the other end of the spring 263 is fixedly mounted on the support arm 230. The spring 263 is used to apply an elastic force away from the gear part to the slider 262 along the arm length direction of the support arm 230. The passive component includes two guide wheels 265, a winding wheel 266, and a pull rope 264. The two guide wheels 265 and the two sliders 262 are arranged correspondingly. The two guide wheels 265 and the winding wheel 266 are rotatably mounted on the support base 240. The rotation axis of the two guide wheels 265 is collinear with the axis of A. One end of the pull rope 264 is fixedly mounted on the slider 262, and the other end passes through the guide wheel 265 and is wound around the winding wheel 266. The rotation axis of the winding wheel 266 is parallel to the rotation axis of the guide wheel 265. The passive gear 267 is mounted on the winding wheel 266.

[0063] The C-trigger assembly includes a C-trigger rack 130, which is arranged at positions corresponding to the cleaning mechanism 500 and the drying mechanism 600. The C-trigger rack 130 and the C-driven gear 267 are arranged correspondingly, and the C-trigger rack 130 is distributed at intervals along the conveying direction of the conveying mechanism 100.

[0064] The support base 240 is also equipped with a toggle assembly 270, which includes a lever 271. The lever 271 is arranged along the length of the support rod 210. One end of the lever 271 is connected to the rotating shaft 272 through a support rod. The rotating shaft 272 is rotatably mounted on the support base 240. A D driven gear 273 is installed on the rotating shaft 272. The D driven gear 273 and the D trigger rack 140 are arranged correspondingly. The D trigger rack 140 is arranged at a position corresponding to the material transfer mechanism 400, the cleaning mechanism 500, and the drying mechanism 600.

[0065] The support shaft 250 is rotatably mounted on the movable seat 280 at its center. Both ends of the movable seat 280 are rotatably mounted in the bearing seats 284 via the horizontal shaft 281. The horizontal shaft 281 is perpendicular to the support shaft 250 and is arranged along the conveying direction of the conveying mechanism 100. The bearing seats 284 are mounted on the conveying mechanism 100, which drives the bearing seats 284 to move. A driven rod 282 is mounted on the horizontal shaft 281, perpendicular to both the support shaft 250 and the horizontal shaft 281. A ball head 283 is mounted on the upper end of the driven rod 282. The conveying mechanism 100... The 0 is also equipped with a limiting guide rail 150. The passive rod 282 is slidably installed in the limiting guide rail 150. The passive rod 282 and the ball head 283 abut against the limiting guide rail 150. The passive rod 282 and the ball head 283 slide and guide along the track of the limiting guide rail 150. The limiting guide rail 150 includes a limiting section A, a transition section and a limiting section B. The limiting section A is used to keep the passive rod 282 in an upright position. The limiting section B is used to keep the passive rod 282 in a horizontal position. The transition section is used to connect the limiting section A and the limiting section B. The limiting section B is arranged at the corresponding position of the cleaning mechanism 500.

[0066] The working process of the filtration device in this embodiment is as follows:

[0067] First, the conveying mechanism 100 transfers the filtration mechanism 200 to below the liquid transfer mechanism 300. During this process, the A driven gear 236 meshes with the A trigger rack 110. The A driven gear 236 drives the A gear 233 to rotate synchronously through the A drive shaft 235. The A gear 233 meshes with the A rack 234, driving the A rack 234 to rise. The A rack 234 drives the lifting rod 232 to rise. The lifting rod 232 drives a support arm 230 to rotate around the A axis through the connecting rod 237. Through the meshing of the gears, the two support arms 230 rotate synchronously around the corresponding A axis. The rotation of the support arms 230 drives the two support rods 210 to rotate. During the upward rotation, the distance between the two support rods 210 decreases. The filter membrane 220 on the two support rods 210 changes from a flat state to a concave state under the action of gravity.

[0068] At this time, the conveying mechanism 100 pauses, and the liquid transfer mechanism 300 discharges an appropriate amount of mixed solution into the center of the filter membrane. It should be noted that the ends and sides of the filter membrane 220, where the support rods 210 are connected, are all bent upwards to prevent the mixed solution from flowing out from the ends or sides.

[0069] After the mixed solution is discharged onto the filter membrane 220, it will first flow to both ends, and the liquid in the mixed solution will permeate through the filter membrane 220.

[0070] At this time, the conveying mechanism 100 is started, the A passive gear 236 disengages from the A trigger rack 110, and the support rod 210 and support arm 230 descend and return to their original positions under the action of gravity, and the filter membrane 220 becomes flat.

[0071] As the conveying mechanism 100 moves at a constant speed, the B driven gear 251 and the B trigger rack 120 mesh. The B trigger racks 120 in the first two groups are respectively arranged above and below the B driven gear 251. The B driven gear 251 first meshes with the first group of B trigger racks 120, thereby driving the support shaft 250 to rotate to the left, adjusting the filter membrane 220 to swing to the left, and causing the mixed solution to flow to the left. Then, the B driven gear 251 meshes with the second group of B trigger racks 120, thereby driving the support shaft 250 to rotate to the right, adjusting the filter membrane 220 to swing to the right, and causing the mixed solution to flow to the right, so that the mixed solution can flow and cover the surface of the filter membrane 220.

[0072] Then, the conveying mechanism 100 continues to move forward, and the B driven gear 251 intermittently meshes with the B trigger rack 120. During meshing, the filter membrane 220 swings left and right, and can return to a horizontal state through the action of the counterweight 252. During the left and right swinging of the filter membrane, firstly, the mixed solution on its surface can flow, improving the filtration efficiency; secondly, after the liquid in the mixed solution has permeated through the filter, the crystals can also roll on the paper surface, allowing the liquid in the gaps between the crystals to be poured out, improving the filtration efficiency.

[0073] Then, the conveying mechanism 100 continues to move forward, and after transferring to above the transfer mechanism 400, the conveying mechanism pauses. During this process, the B driven gear 251 intermittently meshes with the B trigger rack 120, adjusting the filter membrane 220 to flip, pouring the crystals on it onto the flexible belt of the transfer mechanism 400. Furthermore, the transfer mechanism 400 has a trigger gear that matches the D driven gear 273. At this time, the trigger gear descends and meshes with the D driven gear 273, and the adjusting lever 271 rotates. The lever 271 continuously moves the back of the filter membrane 220, allowing the attached crystals to fall off completely.

[0074] Then, as the conveying mechanism 100 continues to move, the B driven gear 251 disengages from the B trigger rack 120, and the filter membrane 220 rotates back to its original position. As the conveying mechanism 100 continues to move, the filter mechanism rotates to above the cleaning mechanism 500, which includes a cleaning tank. The driven rod 282 moves from the A limit section through the conversion section to the B limit section. The horizontal shaft 281 is adjusted to rotate 90 degrees, causing the filter membrane 220 to rotate into an upright position, so that the filter membrane 220 is inserted into the cleaning water in the cleaning tank.

[0075] As the conveying mechanism 100 continues to move forward, the A driven gear 236, B driven gear 251, C driven gear 267, and D driven gear 273 engage with their corresponding racks, adjusting the filter membrane 220 to continuously swing back and forth and left and right in the cleaning water, as well as causing the two ends of the filter membrane 220 to move closer or further apart. During this process, the lever 271 continuously moves the back of the filter membrane 220, achieving efficient and rapid cleaning of the filter membrane 220 and discharging the impurities adsorbed and permeated into the filter membrane 220. When the C driven gear 267 engages with the C trigger rack 130, the reel 266 winds up the pull rope 261, driving the slider 262 to move, thus adjusting the two support rods 210 to move closer together. After the C driven gear 267 disengages from the C trigger rack 130, the two sliders 262 return to their original positions under the restoring force of the spring 263.

[0076] As the conveying mechanism 100 continues to move, the passive rod 282 moves from the B limit section through the conversion section to the A limit section, and the horizontal shaft 281 rotates 90 degrees. Then, the filtration mechanism 200 is transferred through the drying mechanism 600, and the hot air blown out by the drying mechanism 600 achieves the drying treatment of the filter membrane 220.

[0077] The large-particle ammonium perchlorate crystallization process proposed in this invention can crystallize large particles of ammonium perchlorate recovery solution, achieve rapid filtration of the crystals, and perform efficient and rapid cleaning of the filter membrane.

[0078] The embodiments of this embodiment have been described above with reference to the accompanying drawings. However, this embodiment is not limited to the specific implementation methods described above. The specific implementation methods described above are merely illustrative and not restrictive. Those skilled in the art can make many other forms under the guidance of this embodiment without departing from the spirit of this embodiment and the scope of protection of the claims, and all of these forms are within the protection scope of this embodiment.

Claims

1. A large particle ammonium perchlorate crystallization process characterized by, It comprises the following steps: S1: filtering the recovery solution to obtain an ammonium perchlorate solution; S2: performing vacuum distillation crystallization on the ammonium perchlorate solution; S3: continuously transferring the mixed solution containing the crystals into a filtering device, and the filtering device performs anti-breaking filtering treatment on the crystals; S4: drying the ammonium perchlorate crystals after filtering; S5: performing quality inspection on the dried ammonium perchlorate, and the particle size meets the requirements, that is, it is a qualified product, and the unqualified product is recycled; The filtering device comprises a conveying mechanism (100), a liquid transferring mechanism (300), a material transferring mechanism (400), a cleaning mechanism (500) and a drying mechanism (600), and the liquid transferring mechanism (300), the material transferring mechanism (400), the cleaning mechanism (500) and the drying mechanism (600) are spaced apart along the conveying direction of the conveying mechanism (100); The conveying mechanism (100) is provided with filtering mechanisms (200) which are equidistantly spaced apart along the conveying mechanism (100), and each filtering mechanism (200) comprises two parallel support rods (210) provided with filtering membranes (220), and one end of each support rod (210) is mounted on a support arm (230), the support rod (210) and the support arm (230) are vertically arranged, the support arm (230) is fixedly provided with an A shaft at both ends, the A shaft is rotatably mounted on a support base (240), the axial direction of the A shaft is consistent with the length direction of the support rod (210), the ends of the two support arms (230) are provided with gear portions which are engaged with each other, the support arm (230) is connected with an A passive component, the support base (240) is fixedly provided with a support shaft (250) whose axial direction is consistent with that of the A shaft, the support shaft (250) is connected with a B passive component, and the conveying mechanism (100) is provided with an A trigger component and a B trigger component, the A trigger component and the A passive component are arranged correspondingly, and the B trigger component and the B passive component are arranged correspondingly.

2. A large particle ammonium perchlorate crystallization process according to claim 1, wherein In S3, the filtering device performs anti-breaking filtering treatment on the solution as follows: S31: first, adjust the horizontally arranged filtering membranes in the filtering device from a flat state to a concave state; S32: then, pour a certain amount of solution containing crystals into the concave part of the filtering membrane; S33: rotate the filtering membrane so that the solution covers the surface of the filtering membrane; S34: adjust the concave filtering membrane to a flat state and rotate the filtering membrane back and forth; S35: after the filtering is completed, turn over the flat filtering membrane, knock the filtering membrane, make the crystals attached to the surface of the filtering membrane fall off the filtering membrane, and realize the unloading treatment; S36: after the unloading, turn over the filtering membrane back, then rotate the filtering membrane, transfer the filtering membrane to a cleaning pool, continuously rotate and shake the filtering membrane, and knock the back of the filtering membrane to clean the filtering membrane; S37: separate the filtering membrane from the cleaning pool and return it to a flat state, and then dry it.

3. A large particle ammonium perchlorate crystallization process according to claim 2, wherein The A passive component includes a lifting rod (232) and a guide sleeve (231), the guide sleeve (231) is fixedly installed on the support seat (240), the lifting rod (232) is slidingly installed in the guide sleeve (231), the rod length direction of the lifting rod (232) is perpendicular to the axial direction of the A shaft, the lower end of the lifting rod (232) is hingedly connected with one end of a connecting rod (237) through a hinge shaft, the other end of the connecting rod (237) is hingedly connected to a support arm (230) through a hinge shaft, the axial direction of the hinge shaft is consistent with the axial direction of the A shaft, the lower end of the lifting rod (232) is also provided with an A rack (234), the A rack (234) is engaged with an A gear (233), the A gear (233) is installed at one end of an A transmission shaft (235), the support shaft (250) is a hollow shaft, the A transmission shaft (235) is inserted into the support shaft (250), the end of the A transmission shaft (235) away from the A gear (233) extends out of the support shaft (250), and the extending end of the A transmission shaft (235) is provided with an A passive gear (236).

4. A process for the crystallization of large particle size ammonium perchlorate according to claim 3, characterized in that, The A trigger component includes an A trigger rack (110), the A trigger rack (110) is arranged corresponding to the A passive gear (236), and the A trigger rack (110) is arranged at positions corresponding to the liquid rotating mechanism (300), the cleaning mechanism (500) and the drying mechanism (600) respectively.

5. A process for the crystallization of large particle size ammonium perchlorate according to claim 4, characterized in that, The B passive component includes a B passive gear (251) and a counterweight (252), the B passive gear (251) is installed at one end of the support shaft (250) away from the support seat (240), and the counterweight (252) is installed at the end close to the B passive gear (251), the counterweight (252) is used for maintaining the support seat (240) in a horizontal state.

6. A large particle ammonium perchlorate crystallization process according to claim 5 wherein, The B trigger component includes a B trigger rack (120), the B trigger rack (120) is arranged in a region between the liquid rotating mechanism (300) and the material rotating mechanism (400), and is arranged corresponding to the cleaning mechanism (500) and the drying mechanism (600), the B trigger rack (120) is provided in a plurality of groups, the B trigger rack (120) is arranged corresponding to the B passive gear (251), and the B trigger racks (120) in each group are distributed along the conveying direction of the conveying mechanism (100) at intervals.

7. A large particle ammonium perchlorate crystallization process according to claim 6 wherein, A guide groove (261) is formed in the support arm (230) along the arm length direction of the support arm (230), a sliding block (262) is slidingly installed in the guide groove (261), the end of the support rod (210) is installed on the sliding block (262), the sliding block (262) is connected with a C passive component (260), the conveying mechanism (100) is also provided with a C trigger component, the C passive component (260) and the C trigger component are arranged corresponding to each other, and the C passive component (260) is used for driving the sliding block (262) to move in the guide groove (261).

8. A large particle ammonium perchlorate crystallization process according to claim 7, wherein, The C passive assembly (260) comprises a spring (263) and a passive assembly. One end of the spring (263) is fixedly connected with the sliding block (262), and the other end of the spring (263) is fixedly installed on the support arm (230). The spring (263) is used for applying an elastic force to the sliding block (262) away from the gear part along the length direction of the support arm (230). The passive assembly comprises two guide wheels (265), a winding wheel (266) and a pull rope (264). The two guide wheels (265) are correspondingly arranged with the two sliding blocks (262). The two guide wheels (265) and the winding wheel (266) are rotatably installed on the support seat (240). The rotation axes of the two guide wheels (265) are collinear with the axis of the A shaft. One end of the pull rope (264) is fixedly installed on the sliding block (262), and the other end of the pull rope (264) passes through the guide wheel (265) and is wound on the winding wheel (266). The rotation axis of the winding wheel (266) is parallel to the rotation axis of the guide wheel (265). The winding wheel (266) is installed with the C passive gear (267).

9. A large particle ammonium perchlorate crystallization process according to claim 8 wherein, The C trigger assembly comprises a C trigger rack (130). The C trigger rack (130) is arranged at a position corresponding to the cleaning mechanism (500) and the drying mechanism (600). The C trigger rack (130) is correspondingly arranged with the C passive gear (267). The C trigger rack (130) is spaced apart along the conveying direction of the conveying mechanism (100).

Citation Information

Patent Citations

  • Continuous cooling crystallization process capable of regulating and controlling granularity of ammonium perchlorate

    CN115121002A