Crystallizing tank for preparing dihydroartemisinin

Abstract

The invention relates to a crystallizing tank for preparing dihydroartemisinin, which comprises a tank body and a crystallizing reaction shell positioned in the tank body, a mixed solution is positioned in the crystallizing reaction shell, and the crystallizing reaction shell is connected with the tank body through a central shaft. After the crystallization reaction shell is controlled to rotate in the tank body by taking the central shaft as a central axis, a mixed solution in the crystallization reaction shell rolls, and insoluble substances in the mixed solution are filtered out by the separation and filtration assembly; compared with the prior art, the device has the beneficial effects that when the dihydroartemisinin crude product is purified and processed, the dihydroartemisinin crude product and an ethanol solvent are put into the crystallization reaction shell, and then the lower half part of the crystallization reaction shell is heated through the heating assembly, so that dihydroartemisinin is promoted to be dissolved in the ethanol solvent; in the process, the crystallization reaction shell rotates, so that the mixed solution rolls back and forth in the crystallization reaction shell, and the dissolution of the dihydroartemisinin crude product is facilitated.

Description

Technical Field

[0001] The present invention belongs to the field of crystallization equipment, and specifically relates to a crystallization tank for preparing dihydroartemisinin crystals. Background Art

[0002] During the production of dihydroartemisinin, artemisinin needs to be first reduced under the action of a reducing agent so that the peroxy bridge in its structure is reduced to a hydroxyl group, thereby converting it into a crude dihydroartemisinin product. At this time, the crude dihydroartemisinin product is further purified by methods such as column chromatography and recrystallization to finally obtain dihydroartemisinin crystals.

[0003] Especially when using the recrystallization method to purify the crude dihydroartemisinin product, a crystallization tank is required, which mainly serves to hold the crude dihydroartemisinin product and the solvent. For example, a prior art artemisinin crystallization tank with the authorization announcement number: CN206910846U is disclosed. Its structure includes a cooler, a main body of the crystallizer, a motor, a transmission, a storage tank, a thermostat, a feed inlet, etc. When in use, the thermostat is installed on the inner surface edge of the storage tank around its outer surface, the motor is powered on to drive the transmission to rotate, and the artemisinin is put into the main body of the crystallizer through the feed inlet, and the cooler drives the main body of the crystallizer to crystallize the artemisinin.

[0004] However, when using the recrystallization method to purify the crude dihydroartemisinin product, although it is also necessary to cool the solution and then precipitate the dihydroartemisinin crystals in the solution, due to the influence of the purity of the crude dihydroartemisinin product, there will be some insoluble impurities in the solution at this time. The insoluble impurities may affect the purity of the dihydroartemisinin crystals, so it is also necessary to take out the dihydroartemisinin crystals in the crystallization tank for cleaning and filtering operations, and even multiple cleaning and filtering are required, which seriously affects the processing efficiency. Summary of the Invention

[0005] The purpose of the present invention is to provide a crystallization tank that can improve the preparation efficiency of dihydroartemisinin crystals.

[0006] To achieve the above purpose, the present invention adopts the following technical scheme: A crystallization tank for preparing dihydroartemisinin, comprising a tank body and a crystallization reaction shell located inside the tank body. The mixed solution is located inside the crystallization reaction shell, and the crystallization reaction shell is connected to the tank body through a central axis. The key structure is that a filtering component is arranged inside the crystallization reaction shell. After the crystallization reaction shell is controlled to rotate inside the tank body with the central axis as the axis, the mixed solution inside it rolls, and the filtering component filters out the insoluble substances in the mixed solution. The filtering component includes a filtering shell and a filtering disc. A diversion port is arranged on the filtering shell, the filtering disc is located inside the filtering shell, and a filtering part is arranged on the filtering disc. The mixed solution can enter through the diversion port and pass through the filtering part. A conical cylinder is arranged on the filtering disc, and the conical cylinder is connected to an auxiliary disc through a transmission rod. The transmission rod passes through the filtering shell, and the auxiliary disc is located outside the crystallization reaction shell;

[0007] An arc-shaped guide rail is arranged inside the tank body. The center of the arc of the guide rail coincides with the center line of the central axis. When the guide rail meshes with the auxiliary disk and the crystallization reaction shell rotates with the central axis as the central axis, the auxiliary disk moves in a circular motion around the central axis, and the auxiliary disk drives the filter disk to rotate through a transmission rod.

[0008] Furthermore, a stirring arm is arranged inside the crystallization reaction shell. The stirring arm is connected with a transmission disk through a short shaft. The transmission disk meshes with a guide arm which is arc-shaped and located inside the tank body. The center of the arc of the guide arm coincides with the center line of the central axis.

[0009] Furthermore, a plurality of radially extending flat grooves are arranged on the filter disk. The filtering part is located in the flat grooves. The filtering part is composed of an array of a plurality of filter holes. The filtering part can be moved to correspond to the diversion port.

[0010] Furthermore, a separator is arranged in the flat groove. A central notch is arranged on the separator. The separator can translate in the flat groove.

[0011] Furthermore, a protruding shaft is arranged on the separator. A track groove is arranged on the inner surface of the sub-filter shell. The free end of the protruding shaft is located in the track groove. When the filter disk rotates, the protruding shaft on the separator moves in the track groove, so that the separator makes a linear reciprocating motion in the flat groove.

[0012] Furthermore, the track groove is a closed-loop linear groove body. The track groove includes a plurality of arc-shaped groove sections and a plurality of reciprocating track groove sections. The reciprocating groove sections are in an inverted "V" shape and are located between two adjacent arc-shaped groove sections. The ends of the reciprocating track groove sections are butted with the ends of the arc-shaped groove sections.

[0013] Furthermore, the arc-shaped groove sections are located on the radial extension line of the overflow port. The distance from the arc-shaped groove sections to the center of the filter disk is less than the distance from the overflow port to the center of the filter disk.

[0014] Furthermore, the crystallization reaction shell includes a reaction barrel and a top cover. After the top cover is connected with the reaction barrel, the top opening of the reaction barrel is sealed. The transmission rod passes through the center of the top cover. When the top cover moves away from the reaction barrel, the filter disk is taken out from the reaction barrel.

[0015] Furthermore, the sub-filter shell includes two cover bodies. The large-diameter ends of each cover body are butted with an annular extension disk. The outer circumferential surface of the extension disk is in close contact with the inner wall of the crystallization reaction shell. The overflow port is arranged on the extension disk.

[0016] Furthermore, there are a plurality of crystallization reaction shells. The plurality of crystallization reaction shells are parallel to each other and are all located inside the tank body. The top openings on the plurality of crystallization reaction shells face the same direction and can rotate simultaneously.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows: when purifying the crude dihydroartemisinin, the crude dihydroartemisinin and ethanol solvent are both put into the crystallization reaction shell, and then the lower half of the crystallization reaction shell is heated by the heating component to promote the dissolution of dihydroartemisinin in the ethanol solvent. During this process, the crystallization reaction shell rotates, causing the mixed solution to roll back and forth in the crystallization reaction shell, which helps the dissolution of the crude dihydroartemisinin.

[0018] When the mixed solution reaches the supersaturated state, the crystallization reaction shell still rotates. Since a filtering component is provided in the crystallization reaction shell, when the mixed solution rolls in the crystallization reaction shell, it will pass through the filtering component, which can filter out the insoluble impurities in the mixed solution. In this way, when dihydroartemisinin crystals precipitate in the subsequent mixed solution, the influence of insoluble impurities on the dihydroartemisinin crystals can be reduced, and the cleaning treatment of the dihydroartemisinin crystals can be reduced in the subsequent steps. Ideally, even the cleaning treatment of the dihydroartemisinin crystals can be eliminated.

[0019] When the mixed solution cools for a certain period of time, the dihydroartemisinin inside has basically precipitated. At this time, only by rotating the crystallization reaction shell by 180°, the separation of the dihydroartemisinin crystals from the ethanol solvent can be achieved, and then the filter disc in the filtering component is taken out from the crystallization reaction shell, and the dihydroartemisinin can be taken out, thereby increasing the purification efficiency as a whole. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 Schematic diagram of the connection structure between the tank body and the base of the present invention;

[0021] Figure 2 Schematic diagram of the internal structure of the tank body of the present invention;

[0022] Figure 3 Schematic diagram of the positional relationship between the crystallization reaction shell, the guide rail and the guiding arm of the present invention;

[0023] Figure 4 Schematic cross-sectional structure diagram of the crystallization reaction shell of the present invention;

[0024] Figure 5 Schematic structure diagram of the filtering shell of the present invention;

[0025] Figure 6 Schematic structure diagram of the filter disc of the present invention;

[0026] Figure 7 Top view schematic diagram of the cooperation state between the filter disc and the partition sheet of the present invention;

[0027] Figure 8 Front view cross-sectional schematic diagram of the cooperation state between the filter disc and the partition sheet of the present invention;

[0028] Figure 9 Schematic diagram of the bottom surface structure of the epitaxial disk of the present invention;

[0029] Figure 10 Schematic diagram of another embodiment structure of the present invention;

[0030] Wherein, 1 - base, 2 - tank body, 3 - support assembly, 4 - crystallization reaction shell, 41 - reaction barrel, 42 - top cover, 5 - central axis, 50 - marking disk, 6 - heating assembly, 701 - short axis, 702 - stirring arm, 703 - driving disk, 8 - guiding arm, 9 - filtering assembly, 901 - upper cover body, 902 - lower cover body, 903 - internal space, 904 - epitaxial disk, 905 - gasket, 906 - spacing space, 907 - flow - through port, 909 - storage tank, 919 - sealing block, 910 - filter disk, 911 - flat groove, 912 - filtering part, 913 - conical cylinder, 10 - transmission rod, 111 - partition piece, 112 - central notch, 113 - protruding shaft, 1101 - extension groove, 1102 - supporting piece, 122 - arc - shaped groove section, 123 - reciprocating track groove section, 13 - auxiliary disk, 14 - guide rail, 15 - lifting arm, 16 - positioning sleeve, 17 - positioning arm, 18 - holding arm, 19 - threaded locking rod, 20 - driving device, 21 - supporting arm, 30 - refrigerating fin, 60 - partition board. Detailed implementation manners

[0031] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Usually, the components of the embodiments of the present invention described and shown in the accompanying drawings here can be arranged and designed in various different configurations. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative efforts belong to the scope of protection of the present invention. In the embodiments, the components of the embodiments of the present application usually described and shown in the accompanying drawings here can be arranged and designed in various different configurations. Therefore, the following detailed description of the embodiments of the present application provided in the accompanying drawings is not intended to limit the scope of the present application required to be protected, but only represents the selected embodiments of the present application.

[0032] Refer to Figures 1 to 3As shown in the figure, a crystallization tank for preparing dihydroartemisinin includes a flat base 1. The base 1 is disc-shaped. A tank body 2 is arranged on the base 1. The tank body 2 has a cavity inside. The tank body 2 is connected to the base 1 through at least three support components 3. The three support components 3 are arranged along the length direction of the tank body 2. The central axis of the tank body 2 is in a horizontal state. The length of the tank body 2 is between 100 cm and 300 cm and can be selected according to actual needs. At this time, there is a certain distance between the tank body 2 and the base 1. A crystallization reaction shell 4 is arranged in the cavity of the tank body 2. A central shaft 5 is docked at the center of the crystallization reaction shell 4. The central shaft 5 penetrates through the tank body 2 and the central shaft 5 is in a horizontal state. The extension line of this central shaft 5 is perpendicular to the central axis of the crystallization reaction shell 4. The central shaft 5 is connected to the tank body 2 by interference fit. Two heating components 6 are arranged in the tank body 2. The heating components 6 are semi-circular heating plates. At this time, the crystallization reaction shell 4 is located between the two heating components 6. The two heating components 6 generate heat after being powered on, forming a heating area inside the tank body 2. During use, ethanol solvent and crude dihydroartemisinin are added into the crystallization reaction shell 4, and it should be noted that the volume of the mixture should be less than 1 / 2 of the internal space volume of the crystallization reaction shell 4. The lower half of the crystallization reaction shell 4 is located in the heating area. When the mixture is heated in the heating area, the crude dihydroartemisinin will dissolve in the ethanol solvent.

[0033] When dissolving the crude dihydroartemisinin, to increase the dissolution efficiency, a stirring component is arranged in the crystallization reaction shell 4. The stirring component can stir the mixture in the crystallization reaction shell 4 and cooperate with the work of the heating component at the same time, so that the crude dihydroartemisinin is dissolved in the ethanol solvent to form a mixed solution. After the crude dihydroartemisinin is dissolved, the mixed solution is continuously heated and concentrated to a certain volume to make the mixed solution reach a supersaturated state. Then, the work of the heating component 6 is stopped, and the mixed solution is cooled to 0 - 10 °C to precipitate dihydroartemisinin crystals. It should be noted that the cooling rate should be appropriate. Too fast a cooling rate may result in too small crystals, while too slow a cooling rate may affect the efficiency.

[0034] The above-mentioned stirring assembly includes a short shaft 701 passing through one end of the crystallization reaction shell 4. The inner end of the short shaft 701 is butted with a stirring arm 702, and the other end of the short shaft 701 is butted with a transmission disc 703. A sealing sleeve is connected between the short shaft 701 and the crystallization reaction shell 4. An arc-shaped guiding arm 8 is arranged in the tank body 2. Convex teeth are arranged on the guiding arm 8 along the length direction. The transmission disc 703 is a gear disc, and the transmission disc 703 meshes with the convex teeth on the guiding arm 8. The center of the arc of the arc-shaped guiding arm 8 coincides with the center line of the central axis. When the crystallization reaction shell 4 rotates with the central axis as the central axis, the transmission disc 703 makes a circular motion around the central axis. When the crystallization reaction shell 4 rotates until the transmission disc 703 enters the lower half area of the tank body 4, the transmission disc 703 contacts the guiding arm 8 and gradually forms a meshing connection state. At this time, as the crystallization reaction shell 4 continues to rotate, the transmission disc 703 will rotate on its own while making a circular motion, thereby driving the short shaft 701 and the stirring arm 702 to rotate. The stirring arm 702 stirs the mixture in the crystallization reaction shell 4. During this process, as the crystallization reaction shell 4 rotates, the mixture moves from the area at one end inside the crystallization reaction shell 4 to the area near the other end (that is, the mixture makes a reciprocating roll along the length direction of the crystallization reaction shell 4 inside the crystallization reaction shell 4). During the movement of the mixture inside the crystallization reaction shell 4, the dissolution of the crude dihydroartemisinin will be accelerated. At the same time, along with the work of the stirring arm 702, the dissolution effect can be further increased.

[0035] After the mixed solution reaches the supersaturated state, it is necessary to filter the mixed solution while it is hot before cooling it, mainly for filtering out the insoluble impurities in the mixed solution, so as to improve the purity during crystallization. Specifically, refer to Figures 4 to 6 As shown, a filtering component 9 is arranged inside the crystallization reaction shell 4. The filtering component 9 is located at the middle position inside the crystallization reaction shell 4. After the mixed solution passes through the filtering component 9, the filtering component 9 will filter out the insoluble impurities in the mixed solution.

[0036] The above-mentioned filtration component 9 includes two horn-shaped covers, namely an upper cover 901 and a lower cover 902, which are arranged longitudinally. The lower cover 902 is connected to the upper end of the stirring arm 702. For example, a cylindrical groove is provided on the lower cover 902, and the upper end of the stirring arm 702 is inserted into the groove. At this time, the stirring arm 702 can rotate, but the lower cover 902 cannot rotate. An internal space 903 is formed between the upper cover 901 and the lower cover 902. And at the edge of the large-diameter end of each cover, an annular extension disk 904 is butted. The outer circumferential surface of the extension disk 904 is in close contact with the inner wall of the crystallization reaction shell 4. An annular gasket 905 is butted at the edge of one of the extension disks 904, and an annular wire groove is provided on the plane of the other extension disk. The extension disk with the wire groove is connected to the inner wall of the crystallization reaction shell 4. When a part of the gasket 905 is located in the wire groove, the two extension disks 904 are arranged in parallel, and a spaced space 906 is formed between the two extension disks. The spaced space 906 is in communication with the internal space 903. At this time, the two covers and the two extension disks are butted to form a filtration shell. Flow-through openings 907 are provided on both extension disks 904. There are several flow-through openings 907, and several flow-through openings 907 are arranged in an array around the central axis of the extension disk. The flow-through openings 907 on the two extension disks correspond to each other. The solution can pass through the flow-through openings 907, so as not to affect the reciprocating movement of the solution in the crystallization reaction shell 4. However, at this time, the insoluble impurities in the solution cannot be filtered out. Therefore, a filter disk 910 is provided in the filtration shell. The filter disk 910 includes a circular disk body. The surface of the filter disk 910 is in contact with the surface of the extension disk. Radially extending flat grooves 911 are provided near the edge of the filter disk 910. The circumferential surface of the filter disk 910 serves as the starting end of the extension of the flat groove 911. There are several flat grooves 911, and a filtering part 912 is provided in each flat groove 911. The filtering part 912 is composed of an array of several filter holes. When the filter disk 910 rotates, the filtering part 912 can pass through the position corresponding to the flow-through opening 907 on the extension disk. When the filtering part 912 is longitudinally aligned with the flow-through opening 907, the mixed solution passes through the filtering part 912 on the filter disk 910, and the insoluble impurities are intercepted, so that the insoluble impurities are separated from the solution.

[0037] Refer to Figure 4As shown in the figure, two conical cylinders 913 are docked at the center position of the above-mentioned filter disc 910. The two conical cylinders 913 are symmetrically arranged with the filter disc 910 as the mirror plane. Each conical cylinder 913 is fixedly connected to the filter disc 910. At this time, the two conical cylinders 913 are located in the built-in space 903 formed between the upper cover 901 and the lower cover 902. One of the conical cylinders 913 is docked with a transmission rod 10. The transmission rod 10 extends along the central axis direction of the crystallization reaction shell 4 and penetrates through the upper cover 901 and the crystallization reaction shell 4. This transmission rod 10 can rotate. When the transmission rod 10 rotates, it can drive the filter disc 910 and the two conical cylinders 913 to rotate synchronously. At this time, several filtering parts 912 on the filter disc 910 can pass through the corresponding positions of a certain overflow port 907 in sequence. After the insoluble impurities are intercepted by the filtering parts 912 of the filter disc 910, as the filter disc 910 rotates, the insoluble impurities can be moved into the spacer space 906. When the next filtering part 912 on the filter disc 910 moves to the position corresponding to the overflow port 907, the mixed solution can pass through this filtering part 912, thereby realizing the interception of insoluble impurities;

[0038] Refer to Figure 7 As shown in the figure, a separating component is arranged in the planar groove 911. As the filtering part 912 moves in the spacer space 906, the separating component removes the insoluble impurities intercepted by the filtering part 912 of the filter disc 910;

[0039] The separating component includes a separating piece 111 arranged in the planar groove 911. The thickness of the separating piece 111 is equal to the depth of the planar groove 911, but the length of the separating piece 111 is less than the length of the planar groove 911. A central notch 112 is arranged on the separating piece 111. At this time, the separating piece 111 covers the filtering part 912. The area surrounded by the central notch 112 of the separating piece 111 on the filtering part 912 is the filtering area. The insoluble impurities are located in the filtering area. When the filter disc 910 rotates to the position where the filtering part 912 moves between two overflow ports 907 on the same horizontal plane, the separating piece 111 first moves in the planar groove 911 in the direction away from the center of the filter disc 910. At this time, the filtering area moves accordingly, and then the insoluble impurities in the filtering area are moved outwards from the filtering part 912. Then, as the filter disc 910 continues to rotate, the separating piece 111 moves in the planar groove 911 in the direction close to the center of the filter disc 910. This process is the reset process of the separating piece 111 until the separating piece 111 returns to its initial position. At this time, there are no insoluble impurities in the filtering area and it returns to its initial position. It should be noted that at this time, the separating piece 111 forms a tight contact with the filter disc 910 and the outer extension disc 904.

[0040] Specifically refer to 4, Figure 7 、 Figure 8 and Figure 9As shown in the figure, a protruding shaft 113 is provided on the separator plate 111, and a track groove is provided on the inner surface of the epitaxial disk 904. The free end of the protruding shaft 113 is located in this track groove and contacts the bottom plane of the track groove. When the filter disk 910 rotates, the protruding shaft 113 on the separator plate 111 will move in the track groove. In this way, the movement track of the separator plate 111 is restricted by the extending direction of the track groove. Therefore, by adjusting the extending direction of the track groove, the separator plate 111 can perform a linear reciprocating motion in the plane groove 911;

[0041] The above track groove is a closed-loop linear groove body, specifically including a plurality of arc groove segments 122. The plurality of arc groove segments 122 are distributed around the center of the epitaxial disk 904. There is a gap between two adjacent arc groove segments 122. Each arc groove segment 122 is located on the radial extension line of the corresponding flow-through port 907, and the distance from the arc groove segment 122 to the center of the filter disk 910 is less than the distance from the flow-through port 907 to the center of the filter disk 910. A reciprocating track groove segment 123 is provided between two adjacent arc groove segments 122. The two ends of the reciprocating track groove segment 123 are respectively butted with the arc groove segments 122 on the corresponding side. The reciprocating track groove segment 123 is an inverted "V" shape, but it should be noted that the corner position of the reciprocating track groove segment 123 is arc-transitioned, and the butt joint between the reciprocating track groove segment 123 and the arc groove segment 122 is also arc-transitioned, so that the protruding shaft 113 on the separator plate 111 can smoothly enter the reciprocating track groove segment 123 from the arc groove segment 122, and can also smoothly enter the arc groove segment 122 from the reciprocating track groove segment 123. The number of the arc groove segments 122 should be determined according to the number of the flow-through ports 907 on the epitaxial disk 904, and the basic requirement is that the numbers of both are equal.

[0042] In addition, it should also be noted that the filter disk 910 does not completely fill the internal space of the separation shell. There is a certain distance between the edge of the filter disk 910 and the gasket 905. The specific values of this distance and the length of the separator plate 111 can be adjusted according to the overall size parameters. The final standard is: it is allowed that the central notch 112 on the separator plate 111 is completely separated from the filter disk 910, and at this time, the inner end (the end close to the center of the filter disk 910) of the separator plate 111 is still located on the side of the flow-through port 907, that is, the flow-through port 907 is located between the two ends of the separator plate 111 at this time, and the insoluble impurities pushed out by the separator plate 111 will fall into the area between the filter disk 910 and the gasket 905. When the separator plate 111 is reset to the initial position in the central direction of the filter disk 910, the separator plate 111 seals the plane groove 911. At this time, the insoluble impurities between the filter disk 910 and the gasket 905 cannot return to the central notch 112 on the separator plate 111, so as to facilitate the continuous filtration of the remaining insoluble impurities in the mixed solution.

[0043] Refer to Figure 9As shown in the figure, in order to stably store insoluble impurities, a storage groove 909 is provided on the inner side of the epitaxial disk 904. The storage groove 909 is located in the area between the filter disk 910 and the washer 905. This storage groove 909 is composed of a flat notch and a sealing block 919. The flat notch longitudinally penetrates the epitaxial disk 904. After the sealing block is connected to the epitaxial disk 904 by screws, the sealing block plugs the outer port of the flat notch. When it is necessary to remove the accumulated insoluble impurities from the storage groove 909, the sealing block can be separated from the epitaxial disk 904, which is convenient for taking out the insoluble impurities.

[0044] Refer to Figure 8 As shown in the figure, in order to increase the contact tightness between the partition piece 111 and the epitaxial disk 904, an extension groove 1101 is provided on one side of the partition piece 111 near the inner end. The extension groove 1101 communicates with the central notch 112, that is, the extension groove 1101 extends from the central notch 112 to the inner end of the partition piece 111. The width of the extension groove 1101 is equal to the width of the flat groove 911. A supporting piece 1102 is inclined in the extension groove 1101. The supporting piece 1102 is a metal piece with certain elasticity and hardness, such as: spring steel sheet, stainless steel sheet, etc. The upper end of the supporting piece 1102 is fixedly connected to the bottom plane of the extension groove 1101, and its lower end extends to be vertically aligned with the end side edge of the central notch 112. The lower end of the supporting piece 1102 is a cutting edge and abuts against the bottom surface of the flat groove 911. And at this time, the supporting piece 1102 is in a bent state and has a certain restoring force, which can make the partition piece 111 contact the epitaxial disk 904 more tightly.

[0045] Refer to Figure 2 and Figure 3 As shown in the figure, since the rotation of the filter disk 910 needs to be driven by the transmission rod 10, an auxiliary disk 13 is docked at the outer end of the transmission rod 10. At this time, the auxiliary disk 13 is located outside the crystallization reaction shell 4. The auxiliary disk 13 is a gear disk. The auxiliary disk 13 meshes with a guide rail 14 located in the tank body 2. The guide rail 14 is also set as an arc. The side plane of the guide rail 14 is also provided with convex teeth. The convex teeth are arranged at equal intervals along the length direction of the guide rail 14. And the center of the arc of the guide rail 14 coincides with the center line of the central axis 5. However, the radius of the arc center of the guide rail 14 is greater than the radius of the arc center of the guiding arm 8. At this time, the guiding arm 8 is located in the lower half area of the tank body 2, and the opening of the bow-shaped area surrounded by the connecting line of its two end points and the arc faces upward. While the guide rail 14 is located in the upper half area of the tank body 2, and the opening of the bow-shaped area surrounded by the connecting line of its two end points and the arc faces downward. So when the crystallization reaction shell 4 rotates to the position where the auxiliary disk 13 is located in the lower half area inside the tank body 2, the auxiliary disk 13 will not contact the guiding arm 8. When the auxiliary disk 13 is located in the upper half area inside the tank body 2, it will mesh with the guide rail 14. Then, as the crystallization reaction shell 4 rotates, the auxiliary disk 13 makes a circular motion around the central axis, and then drives the transmission rod 10 to rotate;

[0046] However, since the filtration of insoluble impurities in the mixed solution needs to be carried out after the mixed solution reaches the supersaturated state, the rotation timing of the transmission rod 10 needs to be controlled. That is, when the mixed solution reaches the supersaturated solution after heating for a certain time, the guide rail 14 can be controlled to engage with the auxiliary disk 13. Specifically, the guide rail 14 is connected to a suspension arm 15 in an inclined state. The lower end of the suspension arm 15 is fixedly connected to the guide rail 14, and the upper end of the suspension arm 15 is butted with a positioning sleeve 16. A positioning arm 17 in a horizontal state is arranged in the tank body 2. The positioning arm 17 passes through the positioning sleeve 16. A positioning groove extending along the length direction is arranged on the positioning arm 17, and a positioning convex rod is arranged on the inner wall of the positioning sleeve 16. The free end of the positioning convex rod is located in the positioning groove. At this time, the positioning sleeve 16 can slide along the length direction of the positioning arm 17, but the positioning sleeve 16 cannot rotate. A holding arm 18 is fixed on the positioning sleeve 16. A strip-shaped opening is arranged on the tank body 2, and the strip-shaped opening is parallel to the positioning arm 17. The holding arm 18 passes through the strip-shaped opening on the tank body 2. The translation of the positioning sleeve 16 can be adjusted through the holding arm 18, so that the guide rail 14 engages with the auxiliary disk 13. The positioning sleeve 16 and the holding arm 18 form a pushing and controlling assembly.

[0047] After the guide rail 14 engages with the auxiliary disk 13, the position of the positioning sleeve 16 needs to be locked. The locking mechanism is arranged on the holding arm 18, and specifically includes a threaded hole channel arranged on the holding arm 18. The threaded hole channel extends from the free end of the holding arm 18 to penetrate the positioning sleeve 16. A threaded locking rod 19 is screwed in the threaded hole channel. A grip wheel is fixed at the outer end of the threaded locking rod 19. The rotation of the threaded locking rod 19 can be controlled through the grip wheel, so that the threaded locking rod 19 moves axially until the inner end of the threaded locking rod 19 abuts against the positioning arm 17. At this time, the position of the positioning sleeve 16 is locked, and further the guide rail 14 and the auxiliary disk 13 are always kept in an engaged state.

[0048] In this application, the tank body 2 is composed of a horizontal cylinder and two end covers. The two end covers seal the ends of the horizontal cylinder. At this time, the central axis of the horizontal cylinder is in a horizontal state. A feeding port is arranged on the horizontal cylinder, and the crystallization reaction shell 4 located in the tank body 2 is composed of a reaction barrel 41 and a top cover 42. After the top cover 42 is connected to the reaction barrel 41, the top opening of the reaction barrel 41 is sealed. The transmission rod 10 passes through the center of the top cover 42.

[0049] When the crystallization reaction shell 4 is in a vertical state, the feeding port is directly above the top cover 42. A hanging ring is provided on the top cover 42. Lifting equipment can be selected according to the size of the crystallization reaction shell 4. The top cover 42 is lifted by the lifting equipment, so that the top cover 42, the transmission rod 10, the upper cover body 901 and the filter disc 910 are taken out from the feeding port of the tank body 2. Then, an ethanol solvent and crude dihydroartemisinin are put into the crystallization reaction shell 4. Then, the transmission rod 10, the upper cover body 901 and the filter disc 910 are reinstalled into the reaction barrel 41. After the top cover 42 is docked with the top opening of the reaction barrel 41, the crystallization reaction shell 4 is reconstituted.

[0050] During use, refer to Figures 1 to 4 As shown, a driving device 20 and a support arm 21 are provided on the base 1. The central axis fixed to the crystallization reaction shell 4 passes through the support arm 21. The driving device 20 is connected to the central axis. The two can be connected by a transmission chain or by a coupling. The central axis is controlled to rotate by the driving device 20, driving the crystallization reaction shell 4 to rotate in the tank body 2 with the central axis as the axis. During this process, the ethanol solvent and the crude dihydroartemisinin flow from one end to the other end in the crystallization reaction shell 4 to achieve their mixing. When the preset mixing time is reached at a specified temperature, the heating component 6 is stopped from working, and at the same time, the driving device 20 is paused. Then, the guide rail 14 is controlled to move towards the crystallization reaction shell 4 by the holding arm 18 until the guide rail 14 contacts and meshes with the auxiliary disc 13. Then, the driving device 20 is started to work again, and the crystallization reaction shell 4 continues to rotate. During this process, the transmission rod 10 will rotate, thereby driving the filter disc 910 to rotate. Since the mixed solution will still flow from one end to the other end in the crystallization reaction shell as the crystallization reaction shell 4 rotates, and the mixed solution will pass through the filter disc 910 during the flow. The filter disc 910 filters out the insoluble impurities in the mixed solution and pushes the insoluble impurities to the space between the filter disc 910 and the gasket 905 through the partition piece 111. With such repeated movements, the insoluble impurities in the mixed solution are gradually reduced.

[0051] A refrigerating fin 30 is also arranged inside the tank body 2. The refrigerating fin 30 is located below the crystallization reaction shell 4. The refrigerating fin 30 is connected by a pipeline to an air-cooled chiller installed on the base 1. A marking disc 50 is also fixed on the central shaft 5. The marking disc 50 is provided with a pointing component. The pointing component can be an arrow mark, and the arrow mark points to the top cover 42 of the crystallization reaction shell 4. The pointing component can also be a marking rod arranged on the marking disc 50. The marking rod is parallel to the transmission rod 10. When the feeding port is directly above the top cover 42, the marking rod faces upward. The position state of the crystallization reaction shell can be observed by observing the orientation of the pointing component. When the pointing component faces downward, the driving device 20 is stopped, and then the air-cooled chiller is started to cool the inside of the tank body 2, thereby cooling the mixed solution in the crystallization reaction shell 4, so that dihydroartemisinin crystallizes out. Then the driving device 20 is restarted to control the crystallization reaction shell 4 to rotate and move 180°. At this time, the pointing component faces upward, and the driving device 20 is closed again. At this time, the liquid in the crystallization reaction shell 4 will flow to the lower half inside the crystallization reaction shell 4, while the dihydroartemisinin crystals will remain in the upper half. When the top cover 42, the transmission rod 10, the upper cover body 901 and the filter disc 910 are taken out from the feeding port of the tank body 2, the dihydroartemisinin crystals can be taken out. During the processing, there is no need to repeatedly filter the mixed solution in different devices, thereby improving the processing efficiency of dihydroartemisinin crystallization.

[0052] Referring to Figure 10 As shown, as another embodiment of the present invention, several crystallization reaction shells 4 can be provided. The several crystallization reaction shells 4 are all located inside the tank body 2, and the several crystallization reaction shells 4 are parallel to each other. At this time, several partition plates 60 are arranged in the internal space of the tank body 2. Each crystallization reaction shell 4 is located in the area between two adjacent partition plates 60. Adjacent two crystallization reaction shells 4 are connected by a straight shaft. When the driving device 20 controls the central shaft to rotate, several crystallization reaction shells 4 can be driven to rotate simultaneously. However, it should be noted that the top openings of the several crystallization reaction shells 4 should face the same direction, so that multiple groups of dihydroartemisinin crystallization processing can be carried out simultaneously. In this embodiment, it is not limited to the processing of dihydroartemisinin crystallization, but can also be used for other crystallization purification processing at the same time. However, it should be noted that there are not only two heating components 6 at this time, but several groups. A group of heating components 6 is arranged in the space where each crystallization reaction shell 4 is located. Two heating components 6 are a group, and each group of heating components 6 is independently regulated;

[0053] At this time, the number of control guide rails 14 and push control components also needs to be adaptively adjusted according to the number of crystallization reaction shells 4. However, it is best for the several guide rails 14 to move synchronously. Adjacent two push control components can be connected by a pull arm. The pull arm is connected to the holding arm 18 on the push control component. When one of the push control components moves, the other push control components will also move, thereby synchronously moving the several guide rails 14;

[0054] Since several guide rails 14 and the pushing and controlling components move simultaneously at this time, certain requirements are imposed on the driving force for synchronously moving and controlling them. A driving component with a telescopic structure, such as an electric push rod, a hydraulic push rod, etc., can be installed on the tank body 2. The moving end of the driving component is connected to the pushing and controlling component located at the outermost end. When the driving component extends or contracts, several guide rails 14 can be simultaneously controlled to approach the crystallization reaction shell 4, increasing the convenience of operation.

[0055] In the description of the present application, it should be noted that unless otherwise clearly specified and defined, the terms "installed", "connected", and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection; it can be an electrical connection; it can be a hydraulic oil circuit connection; it can be directly connected, or indirectly connected through an intermediate medium, and it can be the communication inside two components. For those of ordinary skill in the art, the specific meanings of the above terms in the present application can be understood according to specific situations.

[0056] The above is only the specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present invention can easily think of changes or substitutions, which should all be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A crystallization tank for preparing dihydroartemisinin, comprising a tank body (2) and a crystallization reaction shell (4) located inside the tank body (2). A mixed solution is located inside the crystallization reaction shell (4). The crystallization reaction shell (4) is connected to the tank body (2) through a central shaft (5), and is characterized in that: A filtering component (9) is arranged inside the crystallization reaction shell (4). After the crystallization reaction shell (4) is controlled to rotate inside the tank body (2) with the central axis (5) as the central axis, the mixed solution inside it rolls, and the filtering component (9) filters out the insoluble substances in the mixed solution; The filtering component (9) includes a filtering shell and a filter disc (910). An overflow port (907) is arranged on the filtering shell. The filter disc (910) is located inside the filtering shell. A filtering part (912) is arranged on the filter disc (910). The mixed solution can enter through the overflow port (907) and pass through the filtering part (912). A conical cylinder (913) is arranged on the filter disc (910). The conical cylinder (913) is connected with an auxiliary disc (13) through a transmission rod (10). The transmission rod (10) passes through the filtering shell, and the auxiliary disc (13) is located outside the crystallization reaction shell (4); An arc-shaped guide rail is arranged inside the tank body (2). The center of the arc of the guide rail coincides with the center line of the central axis. When the guide rail meshes with the auxiliary disc (13) and the crystallization reaction shell (4) rotates with the central axis as the central axis, the auxiliary disc (13) makes a circular motion around the central axis (5), and the auxiliary disc (13) drives the filter disc (910) to rotate through the transmission rod (10).

2. A crystallization tank for preparing dihydroartemisinin according to claim 1, characterized in that: A stirring arm (702) is arranged inside the crystallization reaction shell (4). The stirring arm (702) is connected with a transmission disc (703) through a short shaft (701). The transmission disc (703) meshes with a guide arm (8) which is arc-shaped and located inside the tank body (2). The center of the arc of the guide arm (8) coincides with the center line of the central axis (5).

3. A crystallization tank for preparing dihydroartemisinin according to claim 1, characterized in that: A number of radially extending flat grooves (911) are arranged on the filter disc (910). The filtering part (912) is located in the flat grooves (911). The filtering part (912) is composed of an array of a number of filter holes, and the filtering part (912) can be moved to correspond to the overflow port (907).

4. A crystallization tank for preparing dihydroartemisinin according to claim 3, characterized in that: A separating sheet (111) is arranged in the flat groove (911). A central notch (112) is arranged on the separating sheet (111), and the separating sheet (111) can translate in the flat groove (911).

5. A crystallization tank for preparing dihydroartemisinin according to claim 4, characterized in that: A protruding shaft (113) is arranged on the separating sheet (111). A track groove is arranged on the inner side surface of the filtering shell. The free end of the protruding shaft (113) is located in the track groove. When the filter disc (910) rotates, the protruding shaft (113) on the separating sheet (111) moves in the track groove, causing the separating sheet (111) to perform a linear reciprocating motion in the flat groove (911).

6. A crystallization tank for preparing dihydroartemisinin according to claim 5, characterized in that: The track groove is a closed-loop linear groove body. The track groove includes a number of arc-shaped groove segments (122) and a number of reciprocating track groove segments (123). The reciprocating groove segments are in an inverted "V" shape and are located between two adjacent arc-shaped groove segments (122). The ends of the reciprocating track groove segments (123) are butted against the ends of the arc-shaped groove segments (122).

7. A crystallization tank for preparing dihydroartemisinin according to claim 6, characterized in that: The arc-shaped groove segments (122) are located on the radial extension line of the overflow port (907), and the distance from the arc-shaped groove segments (122) to the center of the filter disc (910) is less than the distance from the overflow port (907) to the center of the filter disc (910).

8. A crystallization tank for preparing dihydroartemisinin according to claim 1, characterized in that: The described crystallization reaction shell (4) includes a reaction barrel (42) and a top cover (42). After the top cover (42) is connected to the reaction barrel (41), the top opening of the reaction barrel (41) is sealed. The transmission rod (10) passes through the center of the top cover (42). When the top cover (42) moves away from the reaction barrel (41), the filter disc (910) is taken out of the reaction barrel (41).

9. A crystallization tank for preparing dihydroartemisinin according to claim 1, characterized in that: The described sub-filter shell includes two cover bodies. The large-diameter end of each cover body is butt-connected with an annular extension disc (904). The outer circumferential surface of the extension disc (904) is in close contact with the inner wall of the crystallization reaction shell (4). The flow-through port (907) is arranged on the extension disc (904).

10. A crystallization tank for preparing dihydroartemisinin according to any one of claims 1 to 9, characterized in that: There are several described crystallization reaction shells (4). The several crystallization reaction shells (4) are parallel to each other and are all located inside the tank body (2). The top openings on the several crystallization reaction shells (4) face the same direction and can rotate simultaneously.

Images