A method and equipment for purifying calcium dobesilate

Abstract

The present application relates to a purification method and purification equipment for calcium dobesilate, which includes a kettle body, in which are provided: a partition; a filter screen; an activated carbon layer; a central shaft, the central shaft and the partition being arranged to move and rise in tandem in the axial direction of the central shaft; an upper stirring blade and a lower stirring blade being arranged to rotate in tandem with the central shaft; a plurality of disturbance rods, which are arranged and pass through the partition, and the plurality of disturbance rods are arranged to surround the outer periphery of the stirring area of ​​the upper stirring blade; a driving mechanism for driving the central shaft to drive the upper stirring blade to rotate synchronously, and a lifting mechanism for driving the central shaft to drive the partition to move and rise synchronously. The present application can realize the dissolution, adsorption, filtration, crystallization and discharge processes in the calcium dobesilate purification process in only one kettle body, without the need to transfer the intermediate product during the connection between the various processes, thereby improving the purification efficiency, and by controlling the uniform temperature drop in the crystallization process, the particle size consistency of the precipitated calcium dobesilate crystals can be improved, thereby improving the purification quality.

Description

Technical Field

[0001] The present application relates to the technical field of biopharmaceuticals, and in particular to a purification method and purification equipment for calcium dobesilate. Background Art

[0002] Calcium dobesilate is a vascular protective agent primarily used to treat diabetic microvascular complications, such as diabetic retinopathy and diabetic nephropathy. It exhibits anti-inflammatory, antioxidant, and anti-angiogenic properties. However, crude calcium dobesilate may contain raw material impurities, unreacted raw materials, by-products, catalysts, or other impure substances. Therefore, purification is required during production to remove these unwanted components, improve the purity of the drug, and ensure its quality and efficacy.

[0003] In the related art, a Chinese patent application with application number CN202210245007.4 proposes a method for preparing a crystalline form of benzenesulfonate, comprising the following steps: step (1): weighing a certain mass of (S)-2-(1-(9H-purine-6-ylamino)propyl)-3-(3-fluorophenyl)-4H-chromen-4-one free base compound, adding it to a certain volume of isopropanol solvent and dissolving it in a water bath to obtain solution 1; step (2): weighing a certain mass of benzenesulfonic acid ligand, dissolving it in a certain volume of isopropanol solvent by ultrasonic heating; A certain volume of isopropanol is added to obtain solution 2; step (3): the solution 2 obtained in step (2) is added dropwise to the stirred solution 1 obtained in step (1) to obtain solution 3; step (4): the solution 3 obtained in step (3) is stirred until no solid is precipitated, a certain volume of antisolvent is added to the solution to precipitate solid, and stirring is continued to obtain a suspension; step (5): the suspension obtained in step (4) is filtered under reduced pressure, the surface of the filter cake is rinsed with isopropanol, and the obtained solid is vacuum dried at room temperature to obtain the crystalline form 1.

[0004] The above-mentioned related technologies have the following defects: during the purification process of calcium dobesilate, crude calcium dobesilate is usually first dissolved in hot water, then impurities are adsorbed with activated carbon, and then cooled and crystallized. After the crystals are completely precipitated, they are filtered, and the filtered crystals are washed with low-temperature water. Finally, the finished calcium dobesilate obtained by drying can meet the needs of use. However, in actual production, the cooling and crystallization time is generally 2 to 4 hours, which is much longer than the dissolution and adsorption process of calcium dobesilate. This causes the front-end equipment in the production line to be shut down for a long time and fails to effectively improve production efficiency. In addition, the traditional water-jacketed kettle cooling and crystallization method causes a temperature gradient from the edge to the center of the solution, resulting in the crystal particle size near the water jacket being larger than the crystal particle size at the center of the kettle, which is not conducive to controlling the consistency of the crystal particle size. Summary of the Invention

[0005] In order to improve the problems of low production efficiency and weak crystal particle size control in existing calcium dobesilate purification equipment, the present application provides a purification method and purification equipment for calcium dobesilate.

[0006] The first aspect of the present application provides a calcium dobesilate purification device that adopts the following technical solution:

[0007] A purification device for calcium dobesilate comprises a kettle body, a water jacket is provided on the kettle body, a feeding port is provided at the upper portion of the kettle body, a discharge port is provided at the lower portion of the kettle body, and the kettle body is provided with:

[0008] A partition is sealingly and slidably disposed in the kettle body, and has a plurality of hollow portions thereon, and the partition divides the interior of the kettle body into an upper area and a lower area;

[0009] A filter screen is fixed to the partition plate and covers all the hollow portions;

[0010] An activated carbon layer is filled between the partition and the top wall of the kettle body;

[0011] A central shaft passes through the upper and lower sides of the partition and is rotatably mounted on the partition, wherein the central shaft and the partition are simultaneously raised and lowered along the axis of the central shaft;

[0012] There are multiple upper stirring blades and lower stirring blades, which are sleeved on the central shaft and rotated together with the central shaft. The upper stirring blades and the lower stirring blades are respectively arranged above and below the partition; and

[0013] A plurality of agitation rods are provided and fixedly connected to the kettle body, the agitation rods are arranged through the partition and are sealed and slidably connected to the partition, and the plurality of agitation rods surround the outer periphery of the stirring area of ​​the upper stirring blade;

[0014] The kettle body is provided with a driving mechanism for driving the middle shaft to drive the upper stirring blade to rotate synchronously, and a lifting mechanism for driving the middle shaft to drive the partition to rise and fall synchronously;

[0015] The driving mechanism is configured to drive the central shaft to rotate at a first speed during the dissolution process and at a second speed during the crystallization process, wherein the second speed is less than the first speed;

[0016] The lifting mechanism is configured to drive the central shaft to rise after the dissolution process is completed and to drive the central shaft to descend after the crystallization process is completed.

[0017] Furthermore, the upper stirring blade and the lower stirring blade each include a ring and a plurality of blades fixed to the ring, the cross-section of the central axis corresponding to the upper area and the lower area is non-circular, the ring is slidably adapted to the central axis, and a first permanent magnet and a second permanent magnet that magnetically repel each other are respectively provided on adjacent two side edges of two adjacent rings.

[0018] Furthermore, a lower limit ring is fixed to the bottom end of the central shaft, and an upper limit ring is provided on the top sliding sleeve. The upper limit ring and the lower limit ring are both provided with a third permanent magnet on one side close to the partition that magnetically repels the adjacent first permanent magnet or second permanent magnet.

[0019] Furthermore, the lower part of the kettle body is connected to a backwash pipe connected to a cold water source, and a backwash control valve is provided on the backwash pipe. The backwash control valve is configured to open after the crystallization process is completed to allow cold water to flush the crystallized crystals.

[0020] Furthermore, a discharge pipe is connected to the peripheral side of the lower part of the kettle body. When the partition moves down to the maximum stroke, the discharge pipe is located above the partition. A discharge control valve is provided on the discharge pipe. The discharge control valve is configured to open synchronously or delayed when the backflush control valve is opened to discharge the flushing water or the activated carbon layer.

[0021] Furthermore, the driving mechanism includes:

[0022] A transmission sleeve is rotatably mounted on the top of the kettle body, and the top end of the central shaft passes through the top end of the kettle body and is inserted into the transmission sleeve;

[0023] A transmission ring gear is coaxially arranged with the central shaft and fixedly connected to the outer peripheral wall of the transmission sleeve;

[0024] A transmission gear is rotatably mounted on the kettle body and meshed with the transmission gear ring;

[0025] The driving motor is used to drive the transmission gear to rotate.

[0026] Furthermore, the lifting mechanism includes:

[0027] A balance plate is arranged above the central axis, and the top end of the central axis is anti-slip and rotatably mounted on the middle part of the lower end surface of the balance plate;

[0028] Two linear drive members are provided and are respectively fixed to two opposite side walls of the kettle body, and the output ends of the linear drive members are fixed to the end of the balance plate.

[0029] Furthermore, a circulation channel is provided in the disturbance rod, the inlet of the circulation channel is connected to the cold water source, and the outlet is connected to the circulating water source.

[0030] The second aspect of the present application provides a method for purifying calcium dobesilate using the following technical solution:

[0031] A method for purifying calcium dobesilate, based on the above-mentioned calcium dobesilate purification device, comprises the following steps:

[0032] S1. Dissolving, driving the partition downward to its maximum stroke via the lifting mechanism, mixing the crude calcium dobesilate with hot water and feeding the mixture into the upper region of the kettle through the feeding port, driving the central shaft via the driving mechanism to rotate the plurality of upper stirring blades at the first speed, and utilizing the plurality of disturbance rods to enhance the stirring effect and accelerate dissolution;

[0033] S2 adsorption, the feed port into the kettle into the activated carbon balls to form the activated carbon layer, maintaining the upper stirring blade rotating stirring state to ensure uniform adsorption effect;

[0034] S3 filtering, the lifting mechanism drives the partition to move up to the maximum stroke to filter the activated carbon balls in the solution so that the filtrate after the adsorbed impurities enter the lower zone;

[0035] S4. Crystallization, circulating cold water is passed into the water jacket and the disturbance rod, and the central shaft is driven by the drive mechanism to drive the plurality of lower stirring blades to rotate at the second speed to maintain a uniform temperature drop of the filtrate in the lower zone;

[0036] S5. Discharge, after complete crystallization, the partition is driven downward by the lifting mechanism, and the discharge port is opened to discharge the calcium dobesilate crystal mixture;

[0037] S6. Centrifuge and dry, centrifuge and sieve out calcium dobesilate crystals, and dry them to obtain finished calcium dobesilate.

[0038] Furthermore, in step S5, a discharge pipe is provided on the side wall of the lower part of the kettle body, and a backwash pipe is provided at the lower part of the kettle body. When the lifting mechanism drives the partition to move down and over the discharge pipe, cold water is introduced into the lower area through the backwash pipe to flush the calcium p-hydroxybenzenesulfonate crystals. Part of the flushing water passes through the filter and is discharged from the discharge pipe. After flushing is completed, the discharge port is opened again.

[0039] In summary, the beneficial technical effects of this application are:

[0040] 1. The purification equipment of the present application allows the dissolution, adsorption, filtration, crystallization, rinsing, and discharging steps in the calcium dobesilate purification process to be completed in a single kettle, eliminating the need to transfer intermediate products during the transition between steps. This simplifies production equipment and reduces floor space. Furthermore, the purification efficiency can be improved by significantly reducing the time required for the dissolution, adsorption, and filtration steps. Furthermore, by controlling the uniform temperature drop during the crystallization step, the particle size consistency of the precipitated calcium dobesilate crystals can be increased, thereby improving the purification quality.

[0041] 2. The magnetic repulsion between the two adjacent rings on the upper and lower stirring blades can ensure the effective stirring effect of the upper and lower zones during the corresponding process, and can also make full use of the kettle space, keeping the actual available range of the required upper or lower zone as large as possible, so as to ensure the single purification amount of the purification equipment of the present application, and be suitable for industrial mass production;

[0042] 3. The arrangement of multiple disturbance bars can not only improve the stirring effect of the upper and lower stirring blades during rotation, but also allow cold water to be introduced into the circulation channel during the crystallization process to cooperate with the water jacket to form a dual cooling effect in the inner and outer zones, which can greatly improve the efficiency of crystal precipitation.

[0043] 4. By setting up the discharge pipe, not only the filtrate after the crystals are precipitated can be discharged in time, but also the backwash water can be discharged. After the filter plate is set, the activated carbon balls in the activated carbon layer can be selectively replaced, which can ensure the purification efficiency of the purification equipment of this application after continuous production and is more convenient to maintain. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 is a cross-sectional view of the overall structure of an embodiment of the present application;

[0045] Figure 2 yes Figure 1 A partial enlarged schematic diagram of part A;

[0046] Figure 3 yes Figure 1 A partial enlarged schematic diagram of part B;

[0047] Figure 4 yes Figure 1 A partial enlarged schematic diagram of part C in the middle;

[0048] Figure 5 This is a schematic cross-sectional view of the disturbance rod of the embodiment of the present application.

[0049] Description of reference numerals:

[0050] 1. Kettle body; 11. Feeding port; 12. Discharge port; 13. Upper zone; 14. Lower zone; 15. Discharge pipe;

[0051] 21. Water jacket; 22. Disturbance rod; 221. Circulation channel; 222. Separation cylinder; 223. Water inlet pipe; 224. Water outlet pipe;

[0052] 31. Partition plate; 311. First perforation; 312. Second perforation; 313. Polytetrafluoroethylene ring; 32. Filter screen; 33. Activated carbon layer;

[0053] 41. Central axis; 411. Lower limiting ring; 412. Upper limiting ring; 413. Third permanent magnet; 414. Limiting plate; 42. Upper stirring blade; 43. Lower stirring blade; 441. Collar; 442. Blade; 443. First permanent magnet; 444. Second permanent magnet;

[0054] 51. Recoil pipe; 52. Recoil control valve;

[0055] 61. Discharge pipe; 62. Discharge control valve;

[0056] 71. Transmission sleeve; 72. Transmission ring gear; 73. Transmission gear; 74. Drive motor;

[0057] 81. Balance board; 82. Linear drive component. DETAILED DESCRIPTION

[0058] The following will clearly and completely describe the technical solution of this application in conjunction with the accompanying drawings. Obviously, the embodiments described are only part of the embodiments of this application, not all of them. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of this application.

[0059] The present application embodiment discloses a purification device for calcium dobesilate. Figure 1 、 Figure 2 and Figure 3 The kettle body 1 includes a water jacket 21 provided outside the kettle body 1. The water jacket 21 is connected to a cold water source and is only connected to the cold water source during the crystallization process. The kettle body 1 is provided with a feeding port 11 at the top and a discharging port 12 at the bottom. The kettle body 1 is provided with:

[0060] The partition 31 is sealingly and slidably disposed in the kettle body 1 and has a plurality of hollow portions thereon. The partition 31 divides the interior of the kettle body 1 into an upper area 13 and a lower area 14;

[0061] The filter 32 is fixed to the partition 31 and covers all hollow parts;

[0062] The activated carbon layer 33 is filled between the partition 31 and the top wall of the kettle body 1, specifically in the upper area 13. The activated carbon layer 33 is specifically composed of activated carbon balls, and the particle size of the activated carbon balls is larger than the pore size of the filter 32;

[0063] The central axis 41 passes through the upper and lower sides of the partition 31 and is rotatably installed on the partition 31. The central axis 41 and the partition 31 are arranged to move up and down synchronously in the axial direction of the central axis 41. Specifically, a first through-hole 311 is opened in the middle of the partition 31 for the central axis 41 to pass through. A polytetrafluoroethylene ring 313 is fixedly connected to the inner wall of the first through-hole 311. The central axis 41 forms a sealed and rotatable connection with the partition 31 through the polytetrafluoroethylene ring 313; and the central axis 41 is fixedly connected to the upper and lower sides of the partition 31 with limit plates 414, so as to realize the synchronous lifting and lowering setting and rotatable connection between the central axis 41 and the partition 31.

[0064] Furthermore, a plurality of upper stirring blades 42 and lower stirring blades 43 are provided and are sleeved on the central shaft 41 and rotated together with the central shaft 41. The upper stirring blades 42 and the lower stirring blades 43 are arranged above and below the partition 31 respectively.

[0065] Multiple agitation rods 22 are provided and fixedly attached to the kettle body 1. The agitation rods 22 penetrate the partition 31 and are sealed and slidingly connected to the partition 31. The multiple agitation rods 22 surround the outer periphery of the stirring area of ​​the upper stirring blade 42. Specifically, the multiple agitation rods 22 are distributed in an evenly spaced circular array about the central axis 41 of the kettle body 1. The partition 31 is penetrated by a plurality of second through-holes 312 corresponding to the multiple agitation rods 22. The walls of the second through-holes 312 are also fixedly attached to the walls of the polytetrafluoroethylene rings 313. The agitation rods 22 are sealed and slidingly connected to the partition 31 through the polytetrafluoroethylene rings 313. The lower ends of the agitation rods 22 are fixedly attached to the inner wall of the kettle body 1, and the upper ends are fixedly attached to the inner wall of the kettle body 1 through peripheral brackets so as not to interfere with the movement of the upper stirring blade 42.

[0066] The outside of the kettle body 1 is provided with a driving mechanism for driving the middle shaft 41 to drive the upper stirring blade 42 to rotate synchronously, and a lifting mechanism for driving the middle shaft 41 to drive the partition 31 to rise and fall synchronously;

[0067] The driving mechanism is configured to drive the central shaft 41 to rotate at a first speed during the dissolution process and at a second speed during the crystallization process, the second speed being lower than the first speed;

[0068] The lifting mechanism is configured to drive the central shaft 41 upward after the dissolution process is completed and to drive the central shaft 41 downward after the crystallization process is completed.

[0069] Therefore, when purifying calcium dobesilate, the lifting mechanism can be used to drive the central shaft 41 to move the partition 31 downward to its maximum stroke. At this time, the space in the upper zone 13 reaches its maximum. The crude calcium dobesilate is mixed with hot water and fed into the upper zone 13 of the kettle body 1 through the feeding port 11. The driving mechanism drives the central shaft 41 to drive the multiple upper stirring blades 42 to rotate at a first speed. At this time, the multiple upper stirring blades 42 can mix and stir the solution in the upper zone 13 while rotating with the central shaft 41, thereby promoting the dissolution efficiency of the crude calcium dobesilate in the hot water. In addition, the provision of the multiple disturbance rods 22 further enhances the mixing degree of the crude calcium dobesilate and the hot water, which can further shorten the time consumption of the dissolution process and thereby improve production efficiency.

[0070] After the dissolution process is completed, activated carbon balls are added into the kettle body 1 through the feeding port 11 to form an activated carbon layer 33, and the upper stirring blade 42 is kept in a rotating stirring state so that the activated carbon balls can be evenly suspended in the dissolving liquid to ensure a uniform adsorption effect on impurities in the crude calcium hydroxybenzenesulfonate. Similarly, the provision of multiple disturbance rods 22 can also promote this uniform adsorption process and shorten the time consumption of the adsorption process.

[0071] When the adsorption process is completed, the lifting mechanism drives the central shaft 41 to move the partition 31 up to its maximum stroke. At this time, the activated carbon balls in the mixed liquid are filtered and intercepted in the upper area 13, while the filtrate after the impurities are adsorbed passes through the filter 32 on the partition 31 and enters the lower area 14, so that the activated carbon layer 33 can be separated from the filtrate to avoid affecting the subsequent crystallization yield.

[0072] After the filtration process is completed, circulating cold water is introduced into the water jacket 21 to cool the filtrate in the lower zone 14 of the kettle body 1 until the crystallization temperature is reached. During this process, the central shaft 41 is continuously driven by the driving mechanism to drive the multiple lower stirring blades 43 to rotate at the second speed to maintain a uniform temperature drop of the filtrate in the lower zone 14; similarly, with the help of the setting of multiple disturbance rods 22, the temperature uniformity of the filtrate in the lower zone 14 can be greatly promoted without significantly increasing the rotation speed of the lower stirring blades 43 to avoid damaging the precipitated crystals, thereby ensuring the consistency of the particle size of the crystal particles in the crystallization process.

[0073] After the crystallization process is completed, the lifting mechanism drives the partition 31 downward, allowing the filtrate from the precipitated crystals to pass through the filter screen 32 and enter the upper zone 13, while the crystallized crystals remain in the lower zone 14. Furthermore, the PTFE ring 313 provided in the second perforation 312 allows the partition 31 to scrape off any crystals adhering to the agitation rod 22 during its downward movement. Simultaneously, the circumference of the partition 31 can also scrape off any crystals adhering to the inner wall of the kettle 1, thereby preventing interference with the purification of the next batch of calcium dobesilate. To this end, the PTFE ring 313 can be secured to the circumference of the partition 31 to achieve a sealed, sliding connection with the inner wall of the kettle 1, while ensuring that any remaining crystals on the inner wall of the kettle 1 are effectively scraped and cleaned. The discharge port 12 is then opened to discharge the calcium dobesilate crystals. The calcium dobesilate crystals are then subjected to low-temperature water washing, centrifugation, and drying to obtain a high-purity finished calcium dobesilate.

[0074] It can be seen that, through the configuration of the purification equipment of the present application, the dissolution, adsorption, filtration, crystallization and discharging steps in the purification process of calcium dobesilate can be achieved in only one kettle body 1, without the need to transfer the intermediate product during the connection of each step, thereby simplifying the production equipment and reducing the floor space. In addition, the purification efficiency can be improved by significantly reducing the time consumption of the dissolution, adsorption and filtration processes, and by controlling the uniform temperature drop in the crystallization process, the particle size consistency of the precipitated calcium dobesilate crystals can be improved, thereby improving the purification quality.

[0075] Specifically, refer to Figure 1 and Figure 4 In order to expand the actual application area of ​​the upper zone 13 and the lower zone 14 as much as possible, the upper stirring blade 42 and the lower stirring blade 43 both include a collar 441 and a plurality of blades 442 fixed to the collar 441. The cross-section of the central axis 41 corresponding to the upper zone 13 and the lower zone 14 is non-circular, such as a square, while the cross-section of the central axis 41 corresponding to the first through-hole 311 on the partition 31 is circular to meet the requirements of the rotation connection; the collar 441 is slidably adapted to the central axis 41, and the adjacent two sides of the two adjacent collars 441 are respectively provided with a first permanent magnet 443 and a second permanent magnet 444 that repel magnetically.

[0076] The bottom end of the central shaft 41 is fixedly connected to a lower limiting ring 411, and the top end is slidably sleeved with an upper limiting ring 412. Both the upper limiting ring 412 and the lower limiting ring 411 are provided with a third permanent magnet 413 on the side near the partition 31, which magnetically repels the adjacent first permanent magnet 443 or second permanent magnet 444. Furthermore, the kettle body 1 is provided with a discharge pipe 15 at the discharge port 12. The discharge pipe 15 is arranged directly opposite the central shaft 41. When the partition 31 moves downward to its maximum stroke, the bottom end of the central shaft 41 and the lower limiting ring 411 extend into the discharge pipe 15.

[0077] In this way, when the lifting mechanism drives the central shaft 41 to drive the partition 31 to move down to the maximum stroke, the bottom end of the central shaft 41 and the lower limit ring 411 extend into the discharge pipe 15, and the multiple lower stirring blades 43 slide and stack on the central shaft 41 under the squeezing of the partition 31; for the multiple upper stirring blades 42, since there is a magnetic repulsion between the two adjacent rings 441, a certain distance is maintained between the two adjacent upper stirring blades 42, which can ensure the stirring effect of the central shaft 41 on the solution in the upper zone 13 when driving the multiple upper stirring blades 42 to rotate.

[0078] When the lifting mechanism drives the central shaft 41 to drive the partition 31 to move up to the maximum stroke, the multiple upper stirring blades 42 slide and overlap on the central shaft 41 under the pressure of the partition 31; as for the multiple lower stirring blades 43, a certain distance is maintained under the action of magnetic repulsion, which can also ensure the stirring effect of the central shaft 41 on the filtrate in the lower area 14 when driving the multiple lower stirring blades 43.

[0079] In this way, it is possible to ensure that the upper stirring blades 42 and the lower stirring blades 43 have an effective stirring effect on the upper zone 13 and the lower zone 14 during the corresponding process, and to make full use of the space of the kettle body 1, and to keep the actual available range of the required upper zone 13 or lower zone 14 as large as possible, so as to ensure the single purification amount of the purification equipment of the present application, which is suitable for industrial mass production.

[0080] In addition, refer to Figure 1 To further optimize the calcium dobesilate purification process, a backwash pipe 51 connected to a cold water source is located at the bottom of the kettle 1. A backwash control valve 52 is provided on the backwash pipe 51. Backwash control valve 52 is configured to open after the crystallization process is complete to flush the crystals with cold water. It should be noted that the pore size of the filter 32 is also smaller than the particle size of the precipitated calcium dobesilate crystals to prevent loss of calcium dobesilate crystals during the flushing process.

[0081] In addition, a discharge pipe 61 is connected to the peripheral side of the lower part of the kettle body 1. When the partition 31 moves down to the maximum stroke, the discharge pipe 61 is located above the partition 31. A discharge control valve 62 is provided on the discharge pipe 61. The discharge control valve 62 is configured to open synchronously or delayed when the backflush control valve 52 is opened to discharge the flushing water or the activated carbon layer 33.

[0082] Thus, after the crystallization process is completed, when the partition 31 is driven downward to its maximum stroke by the lifting mechanism, most of the filtrate after the crystals are precipitated is accumulated in the upper zone 13. At this time, the discharge control valve 62 can be directly opened to discharge the filtrate from the discharge pipe 61. At the same time, the backwash control valve 52 is also in the open state, and cold water enters the lower zone 14 through the backwash pipe 51 to perform low-temperature flushing on the calcium dobesilate crystals in the lower zone 14, which can further improve the purity of the calcium dobesilate crystals. The flushing water can also pass through the filter 32 and be discharged from the discharge pipe 61, which can greatly reduce the impurities contained in the calcium dobesilate crystals discharged from the discharge port 12.

[0083] Furthermore, if a detachable filter plate is provided on the discharge pipe 61, the filter plate can be placed on the discharge pipe 61 when the discharge pipe 61 is draining, thereby preventing the activated carbon balls in the upper zone 13 from being discharged along with the activated carbon balls. Furthermore, if, after multiple purification operations, the activated carbon layer 33 has become substantially inactivated and fails to achieve the desired adsorption effect, the filter plate can be removed and the activated carbon balls in the upper zone 13 can be discharged with backwash water for activation, or a new activated carbon layer 33 can be directly added to the upper zone 13. This ensures the purification efficiency of the purification equipment of the present application after continuous production, and makes maintenance more convenient.

[0084] In order to further promote the uniformity of the temperature drop of the filtrate during the crystallization process, refer to Figure 1 and Figure 5 A circulation channel 221 is also provided in the disturbance rod 22, and the inlet of the circulation channel 221 is connected to the cold water source, and the outlet is connected to the circulating water source; specifically, the interior of the disturbance rod 22 is hollow and a separation tube 222 is fixed inside the disturbance rod 22, the upper end of the separation tube 222 is fixed to the upper end of the disturbance rod 22, and the lower end is spaced apart from the disturbance rod 22, so that the separation tube 222 can separate the inner cavity of the disturbance rod 22 into an outer flow channel and an inner flow channel, and the outer flow channel and the inner flow channel are connected at the bottom end of the disturbance rod 22 to form a complete circulation channel 221.

[0085] A water inlet pipe 223 connected to the outer flow channel and a water outlet pipe 224 connected to the inner flow channel are provided on the top of the disturbance rod 22. After the water inlet pipe 223 is connected to the cold water source and the water outlet pipe 224 is connected to the circulating water source, in the crystallization process, cold water is introduced into the water jacket 21 while cold water is also introduced into the water inlet pipe 223. At this time, the cold water flows from top to bottom in the outer flow channel and flows from bottom to top in the inner flow channel and is discharged through the water outlet pipe 224. The filtrate on the side of the disturbance rod 22 can be cooled in the inner zone. With the help of the stirring of the filtrate by the rotation of the multiple lower stirring blades 43 and the outer zone cooling effect of the water jacket 21 outside the kettle body 1, a double cooling effect of the outer zone and the inner zone is formed, which can further promote the uniformity of the temperature drop of the filtrate in the lower zone 14, thereby ensuring the uniformity of the particle size of the calcium hydroxybenzenesulfonate crystals precipitated in the filtrate.

[0086] In addition, refer to Figure 1, the above-mentioned driving mechanism includes:

[0087] The transmission sleeve 71 is rotatably mounted on the top of the kettle body 1. The top of the central shaft 41 passes through the top of the kettle body 1 and is inserted into the transmission sleeve 71. Specifically, the inner hole cross section of the transmission sleeve 71 is adapted to the non-circular cross section of the top of the central shaft 41.

[0088] The transmission ring gear 72 is coaxially arranged with the central shaft 41 and fixedly connected to the outer peripheral wall of the transmission sleeve 71;

[0089] The transmission gear 73 is rotatably mounted on the kettle body 1 and meshes with the transmission ring gear 72;

[0090] The driving motor 74 is used to drive the transmission gear 73 to rotate.

[0091] The above-mentioned lifting mechanism includes:

[0092] The balance plate 81 is arranged above the central shaft 41. The top end of the central shaft 41 is anti-slip and rotationally mounted on the middle part of the lower end surface of the balance plate 81. For example, the central shaft 41 can be rotatably connected to the balance plate 81 by a bearing that can withstand axial loads, such as a bidirectional thrust bearing, a tapered roller bearing, or an angular contact ball bearing.

[0093] There are two linear drive members 82 , which are fixed to two opposite side walls of the kettle body 1 , respectively. The output end of the linear drive member 82 is fixed to the end of the balance plate 81 , and the linear drive member 82 is specifically provided with a hydraulic cylinder.

[0094] In this way, when the driving motor 74 drives the transmission gear 73 to rotate, it can drive the transmission ring gear 72 and the transmission sleeve 71 to rotate, and the transmission sleeve 71 and the central shaft 41 are configured to move synchronously, so it can drive the central shaft 41 to rotate; and when the linear drive member 82 drives the balance plate 81 to rise and fall, it can drive the central shaft 41 to rise and fall without interfering with the rotation state of the central shaft 41.

[0095] The present application embodiment discloses a method for purifying calcium dobesilate, based on the above-mentioned calcium dobesilate purification device, referring to Figure 1 , which includes the following steps:

[0096] S1. Dissolution, the partition 31 is driven downward to its maximum stroke by the lifting mechanism, the crude calcium dobesilate is mixed with hot water and fed into the upper zone 13 of the kettle body 1 from the feeding port 11, the central shaft 41 is driven by the driving mechanism to drive the plurality of upper stirring blades 42 to rotate at a first speed, and the stirring effect is enhanced by means of the plurality of disturbance rods 22 to accelerate the dissolution;

[0097] S2 adsorption, the feed port 11 into the kettle 1 into the activated carbon balls to form an activated carbon layer 33, keep the stirring blade 42 rotating stirring state to ensure uniform adsorption effect;

[0098] S3 filtration, the partition 31 is driven by the lifting mechanism to move up to the maximum stroke to filter the activated carbon balls in the solution so that the filtrate after the adsorbed impurities enter the lower zone 14;

[0099] S4 crystallization, circulating cold water is passed into the water jacket 21 and the disturbance rod 22, and the central shaft 41 is driven by the drive mechanism to drive the plurality of lower stirring blades 43 to rotate at a second speed to maintain a uniform temperature drop of the filtrate in the lower zone 14;

[0100] S5 discharge, after complete crystallization, the partition 31 is driven downward by the lifting mechanism, and the discharge port 12 is opened to discharge the calcium dobesilate crystal mixture;

[0101] S6. Centrifuge and dry, centrifuge and sieve out calcium dobesilate crystals, and dry them to obtain finished calcium dobesilate.

[0102] In step S5, a discharge pipe 61 is provided on the lower side wall of the kettle body 1, and a backwash pipe 51 is provided at the lower part of the kettle body 1. When the lifting mechanism drives the partition 31 to move down and over the discharge pipe 61, cold water is introduced into the lower zone 14 through the backwash pipe 51 to flush the calcium p-hydroxybenzenesulfonate crystals. Part of the flushing water passes through the filter 32 and is discharged from the discharge pipe 61. After the flushing is completed, the discharge port 12 is opened.

[0103] The implementation principle of a purification device for calcium dobesilate in the embodiment of the present application is as follows:

[0104] During the purification of calcium dobesilate, crude calcium dobesilate is first mixed with hot water and fed into the upper region 13 of the kettle 1 through the feed port 11. The central shaft 41 is driven by a driving mechanism to rotate the plurality of upper stirring blades 42 at a first speed, thereby promoting the dissolution efficiency of the crude calcium dobesilate in the hot water. Furthermore, the provision of the plurality of agitation rods 22 further enhances the mixing of the crude calcium dobesilate and the hot water, thereby further shortening the dissolution process and thereby improving production efficiency.

[0105] After the dissolution process is completed, activated carbon balls are added into the kettle body 1 through the feeding port 11 to form an activated carbon layer 33, and the upper stirring blade 42 is kept in a rotating stirring state so that the activated carbon balls can be evenly suspended in the dissolving liquid to ensure a uniform adsorption effect on impurities in the crude calcium hydroxybenzenesulfonate. Similarly, the provision of multiple disturbance rods 22 can also promote this uniform adsorption process and shorten the time consumption of the adsorption process.

[0106] When the adsorption process is completed, the lifting mechanism drives the central shaft 41 to move the partition 31 up to its maximum stroke. At this time, the activated carbon balls in the mixed liquid are filtered and intercepted in the upper area 13, while the filtrate after the impurities are adsorbed passes through the filter 32 on the partition 31 and enters the lower area 14, so that the activated carbon layer 33 can be separated from the filtrate to avoid affecting the subsequent crystallization yield.

[0107] When the filtration process is completed, circulating cold water is simultaneously introduced into the water jacket 21 and the disturbance rod 22, and the filtrate in the lower zone 14 of the kettle body 1 is cooled by the dual cooling effect of the outer zone and the inner zone until the crystallization temperature is reached. During this process, the central shaft 41 is continuously driven by the driving mechanism to drive the multiple lower stirring blades 43 to rotate at the second speed to maintain a uniform temperature drop of the filtrate in the lower zone 14; similarly, with the help of the setting of multiple disturbance rods 22, the temperature uniformity of the filtrate in the lower zone 14 can be greatly promoted without significantly increasing the rotation speed of the lower stirring blades 43 to avoid damaging the precipitated crystals, thereby ensuring the consistency of the particle size of the crystal particles in the crystallization process.

[0108] After the crystallization process is completed, the partition 31 is driven downward by the lifting mechanism, allowing the filtrate from which the crystals have precipitated to pass through the filter screen 32 and enter the upper zone 13, while the crystallized crystals remain in the lower zone 14. Furthermore, due to the provision of the polytetrafluoroethylene ring 313 in the second through-hole 312, the partition 31 can scrape off some of the crystals attached to the agitation rod 22 through the polytetrafluoroethylene ring 313 as it moves downward. Simultaneously, the peripheral side of the partition 31 can also scrape off crystals attached to the inner wall of the kettle body 1, thereby avoiding interference with the purification of the next batch of calcium dobesilate.

[0109] Then, the discharge control valve 62 and the backwash control valve 52 are opened to allow cold water to backwash the calcium dobesilate crystals in the lower zone 14 to rinse. After the rinsing is completed, the discharge port 12 is opened to discharge the calcium dobesilate crystals. The calcium dobesilate crystals are then washed with low-temperature water, centrifuged, and dried to obtain high-purity finished calcium dobesilate.

[0110] Thus, by setting up the purification equipment of the present application, the dissolution, adsorption, filtration, crystallization, rinsing and discharging steps in the purification process of calcium dobesilate can be achieved in only one kettle body 1, without the need to transfer the intermediate product during the connection between the various steps, thereby simplifying the production equipment and reducing the floor space. In addition, the purification efficiency can be improved by significantly reducing the time consumption of the dissolution, adsorption and filtration processes, and by controlling the uniform temperature drop in the crystallization process, the particle size consistency of the precipitated calcium dobesilate crystals can be improved, thereby improving the purification quality.

[0111] Unless otherwise defined, the technical or scientific terms used in this application shall have the usual meanings understood by persons of ordinary skill in the field to which this application belongs. The words "first", "second", "third" and similar terms used in the specification and claims of this application do not indicate any order, quantity or importance, but are only used to distinguish different components. Words such as "one" or "a" do not indicate a quantity limitation, but rather indicate the existence of at least one. Words such as "include" or "comprise" mean that the elements or objects appearing before "include" or "comprises" cover the elements or objects listed after "include" or "comprises" and their equivalents, and do not exclude other elements or objects. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0112] The above are all preferred embodiments of the present application, and are not intended to limit the scope of protection of the present application. Therefore, any equivalent changes made based on the structure, shape, and principle of the present application should be included in the scope of protection of the present application.

Claims

1. A purification device for calcium dobesilate, characterized in that, The invention comprises a kettle body (1), wherein a water jacket (21) is provided on the outside of the kettle body (1), a feeding port (11) is provided on the upper part of the kettle body (1), and a discharge port (12) is provided on the lower part of the kettle body (1), and the kettle body (1) is provided with: A partition (31) is sealingly and slidably disposed in the kettle body (1), and has a plurality of hollow portions thereon. The partition (31) divides the interior of the kettle body (1) into an upper area (13) and a lower area (14); A filter (32) is fixed to the partition (31) and covers all the hollow portions; An activated carbon layer (33) is filled between the partition (31) and the top wall of the kettle body (1); A central shaft (41) passes through the upper and lower sides of the partition (31) and is rotatably mounted on the partition (31), wherein the central shaft (41) and the partition (31) are simultaneously moved up and down in the axial direction of the central shaft (41); The upper stirring blades (42) and the lower stirring blades (43) are provided in plurality and are sleeved on the central shaft (41) and rotated together with the central shaft (41). The upper stirring blades (42) and the lower stirring blades (43) are arranged above and below the partition (31). as well as A plurality of disturbance rods (22) are provided and fixedly connected to the kettle body (1); the disturbance rods (22) are provided through the partition (31) and are sealed and slidably connected to the partition (31); and the plurality of disturbance rods (22) surround the outer periphery of the stirring area of ​​the upper stirring blade (42); The kettle body (1) is provided with a driving mechanism for driving the central shaft (41) to drive the upper stirring blade (42) to rotate synchronously, and a lifting mechanism for driving the central shaft (41) to drive the partition (31) to rise and fall synchronously; The driving mechanism is configured to drive the central shaft (41) to rotate at a first speed during the dissolution process and at a second speed during the crystallization process, wherein the second speed is less than the first speed; The lifting mechanism is configured to drive the central shaft (41) to rise after the dissolution process is completed and to drive the central shaft (41) to descend after the crystallization process is completed.

2. A purification device for calcium dobesilate according to claim 1, characterized in that, The upper stirring blade (42) and the lower stirring blade (43) both include a collar (441) and a plurality of blades (442) fixed to the collar (441); the cross-section of the central axis (41) corresponding to the upper area (13) and the lower area (14) is non-circular; the collar (441) is slidably fitted with the central axis (41); and a first permanent magnet (443) and a second permanent magnet (444) with magnetic repulsion are respectively provided on adjacent side edges of two adjacent collars (441).

3. A purification device for calcium dobesilate according to claim 2, characterized in that, The bottom end of the central shaft (41) is fixedly connected to a lower limiting ring (411), and the top sliding sleeve is provided with an upper limiting ring (412). The upper limiting ring (412) and the lower limiting ring (411) are both provided with a third permanent magnet (413) on one side close to the partition (31) that magnetically repels the adjacent first permanent magnet (443) or second permanent magnet (444).

4. A purification device for calcium dobesilate according to claim 1, characterized in that, The lower part of the kettle body (1) is connected to a backwash pipe (51) connected to a cold water source. A backwash control valve (52) is provided on the backwash pipe (51). The backwash control valve (52) is configured to be opened after the crystallization process is completed so that cold water can flush the crystallized crystals.

5. A purification device for calcium dobesilate according to claim 4, characterized in that, A discharge pipe (61) is connected to the peripheral side of the lower portion of the kettle body (1). When the partition (31) moves downward to the maximum stroke, the discharge pipe (61) is located above the partition (31). A discharge control valve (62) is provided on the discharge pipe (61). The discharge control valve (62) is configured to open synchronously or with delay when the backflush control valve (52) is opened to discharge flushing water or the activated carbon layer (33).

6. A purification device for calcium dobesilate according to claim 1, characterized in that, The driving mechanism comprises: A transmission sleeve (71) is rotatably mounted on the top of the kettle body (1); the top end of the central shaft (41) passes through the top end of the kettle body (1) and is inserted into the transmission sleeve (71); A transmission ring gear (72) is coaxially arranged with the central shaft (41) and fixedly connected to the outer peripheral wall of the transmission sleeve (71); A transmission gear (73) is rotatably mounted on the kettle body (1) and meshedly connected with the transmission ring gear (72); The driving motor (74) is used to drive the transmission gear (73) to rotate.

7. A purification device for calcium dobesilate according to claim 1, characterized in that, The lifting mechanism comprises: A balancing plate (81) is arranged above the central shaft (41), and the top end of the central shaft (41) is anti-slip and rotationally mounted on the middle portion of the lower end surface of the balancing plate (81); Two linear drive members (82) are provided and are respectively fixed to two opposite side walls of the kettle body (1); the output end of the linear drive member (82) is fixed to the end of the balance plate (81).

8. A purification device for calcium dobesilate according to any one of claims 1 to 7, characterized in that: A circulating flow channel (221) is provided in the disturbance rod (22), and the inlet of the circulating flow channel (221) is connected to a cold water source, and the outlet is connected to a circulating water source.

9. A method for purifying calcium dobesilate, based on the calcium dobesilate purification device according to any one of claims 1 to 8, characterized in that: The following steps are involved: S1. Dissolving, driving the partition (31) downward to the maximum stroke by the lifting mechanism, mixing the crude calcium hydroxybenzenesulfonate with hot water and feeding the mixture into the upper area (13) of the kettle (1) from the feeding port (11), driving the central shaft (41) by the driving mechanism to drive the plurality of upper stirring blades (42) to rotate at the first speed, and using the plurality of disturbance rods (22) to enhance the stirring effect to accelerate the dissolution; S2. Adsorption, adding activated carbon balls into the kettle (1) through the feeding port (11) to form the activated carbon layer (33), and keeping the upper stirring blade (42) in a rotating stirring state to ensure a uniform adsorption effect; S3. Filtration, driving the partition (31) to move up to the maximum stroke by the lifting mechanism to filter the activated carbon balls in the solution so that the filtrate after the impurities are adsorbed enters the lower zone (14); S4. Crystallization, circulating cold water is introduced into the water jacket (21) and the disturbance rod (22), and the driving mechanism drives the central shaft (41) to drive the plurality of lower stirring blades (43) to rotate at the second speed to maintain a uniform temperature drop of the filtrate in the lower zone (14); S5. Discharging: After crystallization is complete, the partition (31) is driven downward by the lifting mechanism, and the discharge port (12) is opened to discharge the calcium hydroxybenzenesulfonate crystal mixture; S6. Centrifuge and dry, centrifuge and sieve out calcium dobesilate crystals, and dry them to obtain finished calcium dobesilate.

10. The method for purifying calcium dobesilate according to claim 9, wherein: In step S5, a discharge pipe (61) is provided on the side wall of the lower part of the kettle body (1), and a backwash pipe (51) is provided at the lower part of the kettle body (1). When the lifting mechanism drives the partition (31) to move downward to pass over the discharge pipe (61), cold water is introduced into the lower area (14) through the backwash pipe (51) to flush the calcium p-hydroxybenzenesulfonate crystals. Part of the flushing water passes through the filter (32) and is discharged from the discharge pipe (61). After the flushing is completed, the discharge port (12) is opened again.

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