Purification method and purification equipment of calcium dobesilate

Abstract

The invention relates to a purification method and purification equipment for calcium dobesilate, and the purification equipment comprises a kettle body, a filter screen; an activated carbon layer; the middle shaft and the partition plate are arranged in a synchronous lifting mode in the axial direction of the middle shaft; the upper stirring blade and the lower stirring blade are rotationally arranged together with the middle shaft; the multiple disturbance rods penetrate through the partition plate, and the multiple disturbance rods surround the periphery of the stirring area of the upper stirring blade; a driving mechanism for driving the middle shaft to drive the upper stirring blades to synchronously rotate and a lifting mechanism for driving the middle shaft to drive the partition plate to synchronously lift are arranged outside the kettle body. Dissolution, adsorption, filtration, crystallization and discharging procedures in a calcium dobesilate purification process can be realized in only one kettle body, an intermediate product does not need to be transferred in the process of joining all the procedures, the purification efficiency can be improved, and by means of control over uniform temperature drop in the crystallization procedure, the purification efficiency can be improved. The particle size consistency of precipitated calcium dobesilate crystals can be improved, so that the purification quality is improved.

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, mainly used to treat microvascular complications caused by diabetes, such as diabetic retinopathy, diabetic nephropathy, etc. It has anti-inflammatory, antioxidant and anti-angiogenesis effects. However, crude calcium dobesilate may contain raw material impurities, unreacted raw materials, by-products, catalysts or other impure substances. Therefore, it needs to be purified during production to remove these unnecessary 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): solution 2 obtained in step (2) is added dropwise to the stirred solution 1 obtained in step (1) to obtain solution 3; step (4): solution 3 obtained in step (3) is stirred until no solid is precipitated, a certain volume of anti-solvent 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 dried under vacuum at room temperature to obtain the crystalline form 1.

[0004] The above-mentioned related technologies have the following defects: in the purification process of calcium dobesilate, the crude calcium dobesilate is usually first dissolved in hot water, then impurities are adsorbed by activated carbon, and then cooled and crystallized. After the crystals are completely precipitated, they are filtered, and then the filtered crystals are washed with low-temperature water. Finally, the finished calcium dobesilate obtained by drying can meet the use needs. 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, resulting in long-term shutdown of the front-end equipment in the production line, and the production efficiency cannot be effectively improved; and the traditional water-jacketed kettle cooling and crystallization method will cause a temperature gradient from the edge to the center of the solution, so that the crystal particle size close to the water jacket is larger than the crystal particle size in 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 of 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 purification device for calcium dobesilate using the following technical solution: A purification device for calcium dobesilate comprises a kettle body, a water jacket is arranged outside the kettle body, a feeding port is arranged at the upper part of the kettle body, a discharge port is arranged at the lower part of the kettle body, and the kettle body is provided with: A partition plate is sealingly and slidably disposed in the kettle body, and has a plurality of hollow parts thereon, and the partition plate divides the interior of the kettle body into an upper area and a lower area; A filter screen, fixedly connected to the partition plate and covering all the hollow portions; An activated carbon layer is filled between the partition and the top wall of the kettle body; A central shaft passes through the upper and lower sides of the partition and is rotatably mounted on the partition. The central shaft and the partition are simultaneously raised and lowered in the axial direction of the central shaft; The upper stirring blades and the lower stirring blades are provided in plurality and are sleeved on the central axis and are rotated together with the central axis. The upper stirring blades and the lower stirring blades are arranged above and below the partition respectively; and A plurality of disturbance rods are provided and fixedly connected to the kettle body, the disturbance rods penetrate the partition and are sealed and slidably connected to the partition, and the plurality of disturbance rods surround the outer periphery of the stirring area of ​​the upper stirring blade; 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; The driving mechanism is configured to drive the central shaft to rotate at a first speed in the dissolution process and at a second speed in the crystallization process, wherein the second speed is less than the first speed; The lifting mechanism is configured to drive the central axis to rise after the dissolution process is completed and to drive the central axis to descend after the crystallization process is completed.

[0007] 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 fitted with 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.

[0008] Furthermore, a lower limit ring is fixedly connected 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.

[0009] Furthermore, the lower part of the kettle body is connected to a recoil pipe connected to a cold water source, and a recoil control valve is provided on the recoil pipe. The recoil control valve is configured to be opened after the crystallization process is completed to allow cold water to flush the crystallized crystals.

[0010] 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 with delay when the recoil control valve is opened to discharge flushing water or the activated carbon layer.

[0011] Furthermore, the driving mechanism comprises: A transmission sleeve is rotatably mounted on the top of the kettle body, and the top end of the central axis passes through the top end of the kettle body and is inserted into the transmission sleeve; A transmission gear ring, which is coaxially arranged with the central axis and fixedly connected to the outer peripheral wall of the transmission sleeve; A transmission gear is rotatably mounted on the kettle body and meshedly connected with the transmission gear ring; The driving motor is used to drive the transmission gear to rotate.

[0012] Furthermore, the lifting mechanism comprises: 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; Two linear drive members are provided and are respectively fixed to two opposite side walls of the kettle body, and the output end of the linear drive member is fixed to the end of the balance plate.

[0013] Furthermore, a circulation channel is arranged in the disturbance rod, and the inlet of the circulation channel is connected to the cold water source, and the outlet is connected to the circulating water source.

[0014] The second aspect of the present application provides a method for purifying calcium dobesilate using the following technical solution: A method for purifying calcium dobesilate, based on the above-mentioned calcium dobesilate purification device, comprises the following steps: S1. dissolving, driving the partition to move down to the maximum stroke through the lifting mechanism, mixing the crude calcium dobesilate with hot water and feeding it into the upper area of ​​the kettle from the feeding port, driving the central shaft to drive the plurality of upper stirring blades to rotate at the first speed through the driving mechanism, and using the plurality of disturbance rods to improve the stirring effect to accelerate the dissolution; S2. adsorption, adding activated carbon balls into the kettle through the feeding port to form the activated carbon layer, and keeping the upper stirring blade in a rotating stirring state to ensure uniform adsorption effect; S3. Filtration, driving the partition to move up to the maximum stroke through the lifting mechanism to filter the activated carbon balls in the solution so that the filtrate after the adsorbed impurities enters the lower zone; S4. Crystallization, circulating cold water is introduced into the water jacket and the disturbance rod, and the central shaft drives the plurality of lower stirring blades to rotate at the second speed through the driving mechanism to maintain a uniform temperature drop of the filtrate in the lower zone; S5. Discharging, after crystallization is complete, the partition is driven downward by the lifting mechanism, and the discharge port is opened to discharge the calcium dobesilate crystal mixture; S6. Centrifuge and dry, centrifuge and screen out calcium dobesilate crystals, and dry to obtain finished calcium dobesilate.

[0015] Furthermore, in step S5, a discharge pipe is provided on the lower side wall of the kettle body, and a recoil 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 recoil 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.

[0016] In summary, the beneficial technical effects of this application are: 1. Through the setting of the purification equipment of the present application, the dissolution, adsorption, filtration, crystallization, rinsing and discharging processes in the purification process of calcium dobesilate can be realized in only one kettle, without the need to transfer the intermediate products during the connection of each process, thereby simplifying the production equipment and reducing the floor space; and the purification efficiency can be improved by greatly 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; 2. Through the magnetic repulsion between the two adjacent rings on the upper stirring blade and the lower stirring blade, it can ensure the effective stirring effect of the upper and lower zones of the upper and lower zones during the corresponding process, and make full use of the kettle space to keep 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, which is suitable for industrial mass production; 3. The arrangement of multiple disturbance bars can not only improve the stirring effect of the upper stirring blade and the lower stirring blade 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 double cooling effect in the inner and outer zones, which can greatly improve the crystal precipitation efficiency; 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

[0017] Figure 1 is a cross-sectional view of the overall structure of an embodiment of the present application; Figure 2 yes Figure 1 A partial enlarged schematic diagram of part A; Figure 3 yes Figure 1 A partial enlarged schematic diagram of part B; Figure 4 yes Figure 1 A partial enlarged schematic diagram of part C in the middle; Figure 5 Schematic diagram of the cross-sectional structure of the disturbance rod of the embodiment of the present application Description of reference numerals: 1. Kettle body; 11. Feeding port; 12. Discharging port; 13. Upper zone; 14. Lower zone; 15. Discharging pipe; 21. Water jacket; 22. Disturbance rod; 221. Circulation channel; 222. Separation cylinder; 223. Water inlet pipe; 224. Water outlet pipe; 31. partition; 311. first perforation; 312. second perforation; 313. polytetrafluoroethylene ring; 32. filter screen; 33. activated carbon layer; 41, middle 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; 51. Recoil pipe; 52. Recoil control valve; 61. Discharge pipe; 62. Discharge control valve; 71. Transmission sleeve; 72. Transmission ring gear; 73. Transmission gear; 74. Driving motor; 81. Balance board; 82. Linear drive component. DETAILED DESCRIPTION

[0018] The technical solution of the present application will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present application.

[0019] 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 disposed 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, and the kettle body 1 is provided with a feed port 11 at the top and a discharge port 12 at the bottom. The kettle body 1 is provided with: 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; The filter screen 32 is fixed to the partition plate 31 and covers all hollow parts; 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 screen 32; 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 together 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 rotation 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 rotation connection between the central axis 41 and the partition 31.

[0020] Also, the upper stirring blades 42 and the lower stirring blades 43 are provided in plurality and are sleeved on the central shaft 41 and are 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; A plurality of disturbance rods 22 are provided and fixedly connected in the kettle body 1. The disturbance rods 22 penetrate the partition 31 and are sealed and slidably connected with the partition 31. The plurality of disturbance rods 22 surround the outer periphery of the stirring area of ​​the upper stirring blade 42. Specifically, the plurality of disturbance rods 22 are distributed in an equidistant circular array along the axis 41 of the kettle body 1, and the partition 31 is provided with a plurality of second through holes 312 corresponding to the plurality of disturbance rods 22. A polytetrafluoroethylene ring 313 is also fixedly connected to the hole wall of the second through hole 312. The disturbance rods 22 are sealed and slidably connected with the partition 31 through the polytetrafluoroethylene ring 313. The lower end of the disturbance rod 22 is fixedly connected to the inner wall of the kettle body 1, and the upper end is fixedly connected to the inner wall of the kettle body 1 through a peripheral bracket so as not to interfere with the movement of the upper stirring blade 42.

[0021] 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 plate 31 to rise and fall synchronously; The driving mechanism is configured to drive the central shaft 41 to rotate at a first speed in the dissolution process and at a second speed in the crystallization process, wherein the second speed is lower than the first speed; 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.

[0022] Therefore, when purifying calcium dobesilate, the lifting mechanism can be used to drive the central axis 41 to drive the partition 31 to move downward to the maximum stroke. At this time, the space of the upper zone 13 reaches the maximum, and 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 driving mechanism drives the central axis 41 to drive the plurality of upper stirring blades 42 to rotate at a first speed. At this time, the plurality of upper stirring blades 42 can mix and stir the solution in the upper zone 13 while rotating with the central axis 41, so as to promote the dissolution efficiency of the crude calcium dobesilate in the hot water. In addition, due to the provision of the plurality of disturbance rods 22, the mixing degree of the crude calcium dobesilate and the hot water is further aggravated, which can further shorten the time consumption of the dissolution process, thereby improving the production efficiency.

[0023] 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 rotating and stirring so that the activated carbon balls can be evenly suspended in the dissolved 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.

[0024] When the adsorption process is completed, the lifting mechanism drives the central axis 41 to drive the partition 31 to move up to the maximum stroke. At this time, the activated carbon balls in the mixed liquid are filtered and intercepted in the upper area 13, and the filtrate after the impurities are adsorbed passes through the filter screen 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 rate.

[0025] 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 axis 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.

[0026] After the crystallization process is completed, the partition 31 is driven downward by the lifting mechanism, so that the filtrate of the precipitated crystals passes through the filter screen 32 and enters the upper area 13, and the crystals of the crystals are left in the lower area 14. In addition, by means of the setting of the polytetrafluoroethylene ring 313 in the second perforation 312, the partition 31 can scrape off the crystals partially attached to the disturbance rod 22 through the polytetrafluoroethylene ring 313 when it moves downward, and at the same time, the side of the partition 31 can also scrape off the crystals attached to the inner wall of the kettle body 1 to avoid interference with the purification of the next batch of calcium hydroxybenzenesulfonate. For this reason, the polytetrafluoroethylene ring 313 can be fixed on the side of the partition 31 to achieve a sealed sliding connection with the inner wall of the kettle body 1, while ensuring the scraping and cleaning effect of the residual crystals on the inner wall of the kettle body 1. Then, the discharge port 12 is opened to discharge the calcium hydroxybenzenesulfonate crystals, and then the calcium hydroxybenzenesulfonate crystals are washed with low-temperature water, centrifuged, and dried to obtain high-purity finished calcium hydroxybenzenesulfonate.

[0027] It can be seen that, through the setting 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 realized in only one kettle body 1, and there is no need to transfer the intermediate product during the connection of each step, which simplifies the production equipment and reduces the floor space; and the purification efficiency can be improved by greatly 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.

[0028] 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, and 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 rotational 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 each other magnetically.

[0029] The bottom end of the central axis 41 is fixedly connected with a lower limit ring 411, and the top sliding sleeve is provided with an upper limit ring 412. The upper limit ring 412 and the lower limit ring 411 are both provided with a third permanent magnet 413 that magnetically repels the adjacent first permanent magnet 443 or second permanent magnet 444 on one side of the partition 31. Further, the kettle body 1 is provided with a discharge pipe 15 at the discharge port 12, and the discharge pipe 15 is arranged opposite to the central axis 41, and when the partition 31 moves down to the maximum stroke, the bottom end of the central axis 41 and the lower limit ring 411 extend into the discharge pipe 15.

[0030] In this way, when the lifting mechanism drives the central axis 41 to drive the partition 31 to move down to the maximum stroke, the bottom end of the central axis 41 and the lower limit ring 411 extend into the discharge pipe 15, and the multiple lower stirring blades 43 slide and overlap on the central axis 41 under the pressure of the partition 31; for the multiple upper stirring blades 42, since there is a magnetic repulsion between two adjacent rings 441, a certain distance is maintained between two adjacent upper stirring blades 42, which can ensure the stirring effect of the central axis 41 on the solution in the upper zone 13 when driving the multiple upper stirring blades 42 to rotate.

[0031] When the lifting mechanism drives the central axis 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 axis 41 under the pressure of the partition 31; 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 axis 41 on the filtrate in the lower zone 14 when driving the multiple lower stirring blades 43.

[0032] 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 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.

[0033] In addition, refer to Figure 1 In order to further optimize the purification process of calcium dobesilate, a backwash pipe 51 connected to a cold water source is connected to the lower part of the kettle body 1, and 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 the cold water can flush the crystallized crystals. It should be clearly stated here that the pore size of the filter screen 32 is also smaller than the particle size of the precipitated calcium dobesilate crystals to avoid the loss of calcium dobesilate crystals during the flushing process.

[0034] 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 with delay when the recoil control valve 52 is opened to discharge the flushing water or the activated carbon layer 33.

[0035] Thus, after the crystallization process is completed, when the partition 31 is driven downward to the maximum stroke by the lifting mechanism, most of the filtrate after the crystals are precipitated is stored 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 an open state, and cold water enters the lower zone 14 through the backwash pipe 51, and the calcium hydroxybenzenesulfonate crystals in the lower zone 14 can be low-temperature washed, which can further improve the purity of the calcium hydroxybenzenesulfonate crystals. The washing water can also pass through the filter screen 32 and be discharged from the discharge pipe 61, which can greatly reduce the impurities contained in the calcium hydroxybenzenesulfonate crystals discharged from the discharge port 12.

[0036] Moreover, 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 drained to prevent the activated carbon balls in the upper zone 13 from being discharged; and if the activated carbon layer 33 has been basically deactivated after multiple purification productions and fails to achieve the expected adsorption effect, the filter plate is removed, and the activated carbon balls in the upper zone 13 are discharged with the help of backwash water for activation treatment or a new activated carbon layer 33 is directly placed in the upper zone 13. In this way, the purification efficiency of the purification equipment of the present application can still be ensured after continuous production, and maintenance is more convenient.

[0037] 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 arranged 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 fixedly connected in the disturbance rod 22, the upper end of the separation tube 222 is fixedly connected 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.

[0038] A water inlet pipe 223 connected to the outer flow channel and a water outlet pipe 224 connected to the inner flow channel are arranged 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 and the water inlet pipe 223 at the same time. 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.

[0039] In addition, refer to Figure 1, the above-mentioned driving mechanism includes: The transmission sleeve 71 is rotatably mounted on the top of the kettle body 1, and the top of the central axis 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 axis 41; The transmission gear ring 72 is coaxially arranged with the central shaft 41 and fixedly connected to the outer peripheral wall of the transmission sleeve 71; The transmission gear 73 is rotatably mounted on the kettle body 1 and meshedly connected with the transmission gear ring 72; The driving motor 74 is used to drive the transmission gear 73 to rotate.

[0040] The above-mentioned lifting mechanism comprises: The balance plate 81 is arranged above the middle shaft 41, and the top end of the middle shaft 41 is anti-slip and rotatably mounted on the middle part of the lower end surface of the balance plate 81. For example, the middle 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, an angular contact ball bearing, etc.; There are two linear drive members 82 which 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 , and the linear drive member 82 is specifically provided with a hydraulic cylinder.

[0041] 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 axis 41 are configured to move synchronously, so the central axis 41 can be driven to rotate; and when the linear driving member 82 drives the balance plate 81 to rise and fall, it can drive the central axis 41 to rise and fall, and will not interfere with the rotation state of the central axis 41.

[0042] 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 comprises the following steps: S1. Dissolving, the partition 31 is driven down to the 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 improved by means of the plurality of disturbance rods 22 to accelerate the dissolution; S2 adsorption, activated carbon balls are added to the kettle body 1 through the feed port 11 to form an activated carbon layer 33, and the upper stirring blade 42 is kept rotating and stirring to ensure uniform adsorption effect; S3. Filtration, the partition 31 is moved up to the maximum stroke by the lifting mechanism to filter the activated carbon balls in the solution so that the filtrate after the adsorbed impurities enters the lower zone 14; S4. Crystallization, circulating cold water is introduced into the water jacket 21 and the disturbance rod 22, and the central shaft 41 is driven by the driving 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; 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; S6. Centrifuge and dry, centrifuge and screen out calcium dobesilate crystals, and dry to obtain finished calcium dobesilate.

[0043] Among them, in step S5, a discharge pipe 61 is arranged on the lower side wall of the kettle body 1, and a recoil pipe 51 is arranged 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 recoil pipe 51 to flush the calcium p-hydroxybenzenesulfonate crystals, and part of the flushing water passes through the filter screen 32 and is discharged from the discharge pipe 61. After the flushing is completed, the discharge port 12 is opened.

[0044] The implementation principle of a purification device for calcium dobesilate in the embodiment of the present application is: When purifying calcium dobesilate, the crude calcium dobesilate is first mixed with hot water and fed into the upper area 13 of the kettle body 1 from the feed 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, which can promote the dissolution efficiency of the crude calcium dobesilate in the hot water. In addition, due to the provision of the plurality of disturbance rods 22, the mixing degree of the crude calcium dobesilate and the hot water is further intensified, which can further shorten the time consumption of the dissolution process, thereby improving the production efficiency.

[0045] 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 rotating and stirring so that the activated carbon balls can be evenly suspended in the dissolved 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.

[0046] When the adsorption process is completed, the lifting mechanism drives the central axis 41 to drive the partition 31 to move up to the maximum stroke. At this time, the activated carbon balls in the mixed liquid are filtered and intercepted in the upper area 13, and the filtrate after the impurities are adsorbed passes through the filter screen 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 rate.

[0047] 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 effects of the outer zone and the inner zone until the crystallization temperature is reached. In this process, the central axis 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.

[0048] When the crystallization process is completed, the partition 31 is driven downward by the lifting mechanism, so that the filtrate with precipitated crystals passes through the filter screen 32 and enters the upper area 13, and the crystallized crystals remain in the lower area 14. In addition, with the arrangement of the polytetrafluoroethylene ring 313 in the second through hole 312, the partition 31 can scrape off part of the crystals attached to the disturbance rod 22 through the polytetrafluoroethylene ring 313 when moving downward. At the same time, the side of the partition 31 can also scrape off the crystals attached to the inner wall of the kettle body 1, so as to avoid interference with the purification of the next batch of calcium dobesilate.

[0049] 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 wash; after the washing is completed, the discharge port 12 is opened to discharge the calcium dobesilate crystals, and then the calcium dobesilate crystals are washed with low-temperature water, centrifuged, and dried to obtain high-purity finished calcium dobesilate.

[0050] Therefore, by setting 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 realized in only one kettle body 1, and there is no need to transfer the intermediate product during the connection of each step, which simplifies the production equipment and reduces the floor space; and the purification efficiency can be improved by greatly 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.

[0051] Unless otherwise defined, the technical terms or scientific terms used in this application should be understood by people with ordinary skills in the field to which this application belongs. The words "first", "second", "third" and similar words 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. "One" or "one" and similar words do not indicate a quantitative limit, but indicate that there is at least one. "Include" or "comprise" and similar words mean that the elements or objects appearing before "include" or "comprise" include the elements or objects listed after "include" or "comprise" 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.

[0052] The above are all preferred embodiments of the present application, and the protection scope of the present application is not limited thereto. Therefore, any equivalent changes made according to the structure, shape, and principle of the present application should be included in the protection scope 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 arranged outside the kettle body (1), a feeding port (11) is arranged at the top of the kettle body (1), and a discharging port (12) is arranged at the bottom 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, wherein the partition (31) divides the interior of the kettle body (1) into an upper area (13) and a lower area (14); A filter screen (32) fixedly connected to the partition plate (31) and covering all the hollow portions; An activated carbon layer (33) is filled between the partition plate (31) and the top wall of the kettle body (1); A central axis (41) passes through upper and lower sides of the partition (31) and is rotatably mounted on the partition (31); the central axis (41) and the partition (31) are simultaneously raised and lowered in the axial direction of the central axis (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 are arranged to rotate 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. as well as A plurality of disturbance rods (22) are provided and fixedly connected to the kettle body (1); the disturbance rods (22) penetrate the partition plate (31) and are sealingly and slidably connected to the partition plate (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 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 plate (31) to rise and fall synchronously; The driving mechanism is configured to drive the central shaft (41) to rotate at a first speed in the dissolution process and at a second speed in the crystallization process, wherein the second speed is less than the first speed; The lifting mechanism is configured to drive the central axis (41) to rise after the dissolution process is completed, and to drive the central axis (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 comprise a collar (441) and a plurality of blades (442) fixedly connected 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 matched with the central axis (41); and a first permanent magnet (443) and a second permanent magnet (444) that repel each other magnetically are respectively arranged on adjacent two side edges of two adjacent collars (441).

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

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 be used to 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 circumferential side of the lower part 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 recoil 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), and 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 gear ring (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 meshingly connected with the transmission gear ring (72); A 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 balance plate (81) is arranged above the middle shaft (41), and the top end of the middle shaft (41) is anti-slip and rotatably mounted on the middle part of the lower end surface of the balance 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), wherein the inlet of the circulating flow channel (221) is connected to a cold water source, and the outlet of the circulating flow channel (221) 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) to move downward to the maximum stroke through the lifting mechanism, mixing the crude calcium hydroxybenzenesulfonate with hot water and feeding the mixture into the upper area (13) of the kettle body (1) from the feeding port (11), driving the central shaft (41) to drive the plurality of upper stirring blades (42) to rotate at the first speed through the driving mechanism, and using the plurality of disturbance rods (22) to improve 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 through 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 central shaft (41) is driven by the driving mechanism 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 the crystallization is complete, the partition (31) is driven downward by the lifting mechanism, and the discharge port (12) is opened to discharge the calcium dobesilate crystal mixture; S6. Centrifuge and dry, centrifuge and screen out calcium dobesilate crystals, and dry to obtain finished calcium dobesilate.

10. A method for purifying calcium dobesilate according to claim 9, characterized in that: In step S5, a discharge pipe (61) is provided on the side wall of the lower part of the kettle body (1), and a recoil 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 recoil pipe (51) to flush the calcium p-hydroxybenzenesulfonate crystals. Part of the flushing water passes through the filter screen (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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