A mother liquor circulation treatment device and method for producing calcium dobesilate

Abstract

The present application relates to a mother liquor circulation treatment device and method for producing calcium dobesilate, and relates to the technical field of calcium dobesilate production. The device comprises a tank body, the tank body being provided with a liquid inlet for mother liquor to enter and a liquid outlet for mother liquor to flow out; the tank body being provided with a constant temperature assembly, the constant temperature assembly comprising a coil, the coil comprising three groups, which are sequentially installed in the upper, middle, and lower parts of the tank body; the tank body being provided with a rehydration assembly, the rehydration assembly comprising a rehydration main pipe and a bottom diffusion pipe. The present application can recycle and store mother liquor, so that the stored mother liquor can be fed back into the subsequent or next batch of recrystallization process for reuse, significantly reducing the waste of mother liquor; secondly, each production does not require the same strict quantity control as before, significantly improving production continuity and efficiency.

Description

Technical Field

[0001] The present application relates to the field of calcium dobesilate production, and in particular to a mother liquor circulation treatment device and method for producing calcium dobesilate. Background Art

[0002] Calcium dobesilate is a vascular protective agent that can prevent thrombosis by regulating the physiological function of the microvascular wall, reducing resistance, lowering plasma viscosity and platelet aggregation; at the same time, it can improve the flexibility of red blood cells, indirectly increase lymphatic drainage and reduce edema.

[0003] At present, the main production process of calcium dobesilate is to first synthesize the crude product and then generate high-purity calcium dobesilate through recrystallization.

[0004] The crude product is synthesized by first sulfonating hydroquinone with concentrated sulfuric acid, then neutralizing it with calcium carbonate to form calcium hydroxybenzenesulfonate hydrate, and then filtering to remove calcium sulfate. The filtrate is concentrated under reduced pressure in a concentration tank, cooled, and crystallized to obtain a white solid crude product.

[0005] Recrystallization is to mix the white solid crude product with water, stir, heat to dissolve, and then filter hot to remove insoluble matter. The filtrate is pumped into a crystallization tank, crystallized, centrifuged to obtain a wet product, and then dried to obtain high-purity calcium hydroxybenzenesulfonate.

[0006] The aforementioned production process for calcium dobesilate features relatively mild reaction conditions, no toxic reagents are used during the intermediate process, and a high-purity product. However, in current production, there is a lack of a suitable method for utilizing the mother liquor after centrifugation during recrystallization, leading to waste of the mother liquor. Furthermore, this requires strict quantity control and intermittent production for each production run, significantly impacting production efficiency. Summary of the Invention

[0007] In order to improve the problem of mother liquor recycling, the present application provides a mother liquor recycling treatment device and method for producing calcium dobesilate.

[0008] First, the present application provides a mother liquor circulation treatment device for producing calcium dobesilate, which adopts the following technical solution: a mother liquor circulation treatment device for producing calcium dobesilate, comprising a tank body, wherein the upper portion of the tank body is provided with a liquid inlet for mother liquor to enter and the lower portion of the tank body is provided with a liquid outlet for mother liquor to flow out;

[0009] The tank body is also provided with a constant temperature component, which includes a coil. There are three groups of coils, which are installed in the upper, middle and lower parts of the tank body in sequence.

[0010] The tank body is also provided with a fluid replenishment assembly, which includes a fluid replenishment main pipe and a bottom liquid dispersion pipe. The upper end of the fluid replenishment main pipe is located outside the tank body and the lower end extends to a position close to the bottom of the tank body; the bottom liquid dispersion pipe is connected to the lower end of the fluid replenishment main pipe and is horizontally arranged in the central area of the bottom of the tank body. The bottom liquid dispersion pipe is evenly provided with liquid dispersion holes.

[0011] Preferably, the fluid infusion assembly further includes a top liquid diffusion pipe, which includes a fluid infusion branch pipe and an annular liquid diffusion pipe, one end of the fluid infusion branch pipe is connected to the upper side of the fluid infusion main pipe and the other end is connected to the annular liquid diffusion pipe; the annular liquid diffusion pipe is annular and has nozzles evenly installed thereon, and the annular liquid diffusion pipe is located in the middle area of the upper inner part of the tank body.

[0012] Preferably, the fluid infusion component also includes a avoidance bracket laterally fixed on the fluid infusion main pipe, and the position of the avoidance bracket is lower than the end of the fluid infusion branch pipe connected to the fluid infusion main pipe; the avoidance bracket includes a strut and a fixed pulley, one end of the strut is fixedly connected to the fluid infusion main pipe, the fixed pulley is installed at the other end of the strut, and the fluid infusion branch pipe is embedded in the wheel groove of the fixed pulley.

[0013] Preferably, the fluid replenishment component also includes a liquid level controller, which includes a float and an annular liquid level switch. The annular liquid level switch is mounted on the fluid replenishment branch pipe and can control the opening and closing of the fluid replenishment branch pipe; the float is installed on the annular liquid level switch, and the float is located below the annular liquid level switch.

[0014] Preferably, a stirring assembly is also provided in the tank body, and the stirring assembly includes a drive motor, a stirring shaft, and stirring blades. The drive motor is installed on the top of the tank body and the output end extends into the interior of the tank body. The stirring shaft is vertically arranged on the central axis of the tank body and the upper end is fixedly connected to the output end of the drive motor; the stirring blades are installed on the stirring shaft, and there are two groups of stirring blades in the upper and lower groups.

[0015] Preferably, the stirring shaft is slidably connected to a base, the base includes an outer frame, an inner cylinder and a rib plate, the inner cylinder is slidably sleeved on the stirring shaft, a slide groove is vertically opened on the stirring shaft within the range for adjusting the stirring blade up and down, and a slider is protruding at the position of the inner cylinder corresponding to the slide groove; the outer frame is sleeved and fixed to the outside of the inner cylinder through the rib plate, and the stirring blade is fixed to the outer frame; the base is also provided with a vertical driving member for driving the inner cylinder to slide along the stirring shaft and a vertical positioning member for positioning the position of the inner cylinder after sliding; the vertical driving member includes an outer shell, a rotating power member and a gear, the outer shell is fixed to the outer wall of the inner cylinder, the rotating power member is installed in the outer shell, the gear is installed at the output end of the rotating power member, the inner cylinder and the slider are provided with a clearance window at the position corresponding to the gear, and a part of the gear extends into the inner cylinder through the clearance window; the bottom of the slide groove of the stirring shaft is provided with a tooth groove adapted to the gear along the length direction.

[0016] Preferably, the vertical positioning member is installed on the outer wall of the inner cylinder, and the vertical positioning member includes a shell, a piston, a contact, a tension spring and an electromagnet. The shell is a cylindrical structure with an open end, and the shell is fixedly connected to the inner cylinder; the piston is slidably connected to the shell; the contact is connected to the end of the piston close to the shell opening; the tension spring is wound around the outside of the piston, one end of the tension spring is fixed to the open end of the shell and the other end is fixed to the end of the piston close to the closed end of the shell. Under the elastic force of the tension spring, the piston has a tendency to slide outside the shell opening, and the contact extends out of the shell opening; the electromagnet is installed on one side of the shell close to the closed end, and the electromagnet includes a fixed magnet fixedly connected to the closed end of the shell and a movable magnet fixedly connected to the end of the piston; when the electromagnet is energized, the adsorption force of the fixed magnet and the movable magnet is greater than the elastic force of the tension spring.

[0017] Preferably, the vertical positioning member also includes a damping member, which includes an elastic member, a curved column, and a damping ball. A movable cavity is opened in the horizontal direction at one end of the piston connecting contact, one end of the contact is located in the movable cavity and the other end is located outside the movable cavity. The length of the part of the contact located in the movable cavity is longer than the length of the part located outside the movable cavity. A rotating shaft is installed in the movable cavity, and the contact is rotatably installed on the rotating shaft and has a certain swing space in the up and down directions; one end of the contact located in the movable cavity is opened in the horizontal direction A damping chamber is provided; an elastic member is installed at the bottom of the damping chamber, and the elastic member can be a butterfly spring; the curved column is slidably connected in the damping chamber and is located on the side of the elastic member away from the bottom of the damping chamber, and a damping groove with an inward concave cone is provided on the end face of the curved column away from the elastic member; a part of the damping ball is located in the damping groove; a hemispherical spherical groove is provided on the side of the active cavity of the piston corresponding to the damping groove, and the other part of the damping ball is located in the spherical groove, and the damping ball is tightly clamped between the damping groove of the curved column 5562 and the spherical groove of the active cavity.

[0018] Preferably, a quick installation component is provided on the base, and the quick installation component includes a plate clamp and a plug connector. The plate clamp is fixed to the outer frame of the base, and the plate clamp includes a bottom plate, a top plate and two side plates. The bottom plate, the top plate and the two side plates form a clamping space for the end of the stirring blade to be inserted; three limiting holes are provided at intervals on the top plate, and three through holes are provided correspondingly at the end of the stirring blade; the plug connector includes a hand-held part and three insertion rods fixed at intervals below the hand-held part.

[0019] Furthermore, the present application provides a mother liquor recycling treatment method for producing calcium dobesilate, comprising the following steps: first, when the calcium dobesilate recrystallization process production line is running, the mother liquor centrifuged during the recrystallization is recovered and stored; at the same time, a constant temperature component is turned on to stabilize the temperature of the mother liquor in the tank body within the range of 40°C-60°C; then, a stirring component is turned on continuously or intermittently to stir the mother liquor in the tank body; then, based on the storage time or the requirements of the subsequent recrystallization process, liquid substances such as additives, catalysts or water are added to the mother liquor in the tank body through the liquid replenishing component; finally, the stored mother liquor is sent back to the subsequent or next batch of recrystallization process flow for reuse.

[0020] In summary, this application includes at least one of the following beneficial technical effects:

[0021] 1. First, by setting up tanks and constant temperature components, the mother liquor can be recovered and stored. After storage, the mother liquor can be sent back into the subsequent or next batch of recrystallization process for reuse. The waste of mother liquor is significantly reduced, and the strict quantity control is no longer required for each production. The production continuity and production efficiency are significantly improved.

[0022] 2. Secondly, by setting up a liquid replenishment component, liquid substances such as additives, catalysts, or water can be added to the tank. Adding additives can extend the storage time of the mother liquor or better maintain the mother liquor in a liquid state. When adding catalysts or water, production conditions can be prepared in advance, which significantly increases the heating and dissolution rate of the white solid crude product.

[0023] 3. Furthermore, by setting up a stirring component, the replenishing liquid and the mother liquor can be mixed more quickly. Continuous or intermittent stirring can also be used to reduce sedimentation or abnormal crystallization, so that the mother liquor can be better maintained in a liquid state and better fed into the subsequent recrystallization process. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a process flow chart of Example 1 of the present application;

[0025] Figure 2 This is a schematic diagram of the main structure of Example 1 of the present application;

[0026] Figure 3 Schematic diagram of the structure of the top liquid diffusion pipe of Example 1 of the present application;

[0027] Figure 4 Schematic diagram of the structure of the avoidance bracket of Example 1 of the present application;

[0028] Figure 5 yes Figure 2 Enlarged view of part A in the middle;

[0029] Figure 6This is a schematic diagram of the structure of the base, stirring shaft and stirring blades in the second embodiment of the present application;

[0030] Figure 7 is a top view of the base of Example 2 of the present application;

[0031] Figure 8 is a cross-sectional view of the vertical positioning member of the second embodiment of the present application;

[0032] Figure 9 This is a schematic diagram of the structure of the base and the stirring blade in the third embodiment of the present application;

[0033] Figure 10 This is a schematic diagram of the structure of the base and the stirring blade in the fourth embodiment of the present application;

[0034] Figure 11 is a cross-sectional view of a lateral limiter according to a fourth embodiment of the present application;

[0035] Figure 12 This is a schematic diagram of the coordination between the scrubbing assembly and the base in the fifth embodiment of the present application.

[0036] In the figure, 1, tank body; 11, liquid inlet; 12, liquid outlet; 13, manhole; 14, safety vent pipe; 2, constant temperature assembly; 21, coil; 22, mounting bracket; 23, clamp; 3, liquid replenishment assembly; 31, liquid replenishment main pipe; 32, bottom liquid dispersion pipe; 321, liquid dispersion hole; 322, height limit bracket; 33, top liquid dispersion pipe; 331, liquid replenishment branch pipe; 332, annular liquid dispersion pipe; 3321, nozzle; 34, avoidance bracket; 341, support rod; 342, fixed pulley; 35, liquid level controller; 3 51. Float; 352. Annular level switch; 4. Stirring assembly; 41. Drive motor; 42. Stirring shaft; 421. Slide; 422. Tooth groove; 423. Positioning hole; 43. Stirring blade; 431. Plug hole; 44. Support frame; 5. Base; 51. Outer frame; 52. Inner cylinder; 521. Slider; 53. Rib; 54. Vertical drive member; 541. Housing; 542. Rotating power member; 543. Gear; 55. Vertical positioning member; 551. Housing; 552. Piston; 5521. Movable cavity; 553, contact; 5531, rotating shaft; 5532, damping cavity; 554, tension spring; 555, electromagnet; 5551, fixed magnet; 5552, movable magnet; 556, damping element; 5561, elastic element; 5562, curved column; 55621, damping groove; 5563, damping ball; 56, quick installation assembly; 561, plate clamp; 5611, bottom plate; 5612, top plate; 5613, side plate; 5614, limiting hole; 562, plug connector; 5621, handheld Part; 5622, plug rod; 563, lateral limiter; 5631, base shell; 56311, strip hole; 5632, push rod; 56321, rotating support; 56322, clearance hole; 5633, plug; 5634, compression spring; 5635, guide column; 57, brush assembly; 571, fixing clamp; 572, ring brush; 5721, column; 5722, positioning ring; 5723, bristle 1; 573, groove brush; 5731, vertical plate; 5732, rotating cylinder; 5733, bristle 2. DETAILED DESCRIPTION

[0037] The following is combined with Figure 1 -Attached Figure 12 , further details of this application are given. Example 1

[0038] A mother liquor circulation treatment device for producing calcium dobesilate, referring to Figure 1 、 Figure 2The mother liquor recycling and treatment device is installed in the calcium dobesilate recrystallization production line. By recovering and storing the mother liquor after centrifugation during recrystallization, it can be fed back into the recrystallization production line for reuse. Specifically, the mother liquor can be fed into a decolorization tank or heated for dissolution. After the improvement, the separated mother liquor can be used in the production of the next batch of products, significantly reducing the waste of mother liquor. Secondly, because the mother liquor can be recovered and stored, there is no need to strictly control the amount of mother liquor in each production, which significantly improves production continuity and production efficiency.

[0039] The mother liquor circulation treatment device includes a tank body 1, and a liquid inlet 11 for the mother liquor to enter is provided on the side of the upper part of the tank body 1 corresponding to the separation process; a liquid outlet 12 for the mother liquor (a mixed liquid formed by mixing pure water or other substances again) to flow out is provided on the side of the lower part of the tank body 1 corresponding to the decolorization tank or the heating and dissolution process; a manhole 13 is provided at a position above the liquid outlet 12 in the lower part of the tank body 1; a safety vent pipe 14 is provided on the top of the tank body 1, one end of the safety vent pipe 14 is located in the tank body 1, and the other end is located outside the tank body 1, and an air pressure valve is provided on the safety vent pipe 14, which can be opened when the pressure in the tank body 1 reaches a threshold value to release the pressure in the tank body 1; a circulation pump is provided on the pipeline from the liquid outlet 12 of the tank body 1 to the decolorization tank or the heating and dissolution process, and the mother liquor is extracted from the tank body 1 and sent to the decolorization tank or the heating and dissolution process through the circulation pump.

[0040] The mother liquor circulation treatment device also includes a constant temperature component 2 arranged in the tank body 1, which can provide heat in the range of 40℃-60℃ for the mother liquor in the tank body 1, especially during the period of low external ambient temperature, so that the mother liquor can be kept in a liquid state for a long time.

[0041] The thermostatic component 2 can be electrically heated. Considering the chemical composition of the mother liquor and the utilization of the plant's production capacity, the thermostatic component 2 in this embodiment preferably uses a coil 21. The process steam in the plant can be introduced into the coil 21 to fully utilize the waste heat of the process steam. The inlet and outlet of the coil 21 are located outside the tank body 1, and the remaining part is distributed in a ring shape inside the tank body 1. The central axis of the annular part of the coil 21 coincides with the central axis of the tank body 1, and a gap is left between the edge of the coil 21 and the inner wall of the tank body 1. A mounting bracket 22 is fixed in a circumferential array at the position corresponding to the coil 21 on the inner wall of the tank body 1, and the coil 21 is fixed to the mounting bracket 22 by a clamp 23.

[0042] Preferably, there are three groups of coils 21, which are sequentially installed in the upper, middle, and lower parts of the tank body 1. This arrangement allows for more uniform heating of the mother liquor. Furthermore, depending on the amount of mother liquor, it is possible to choose to open only the lower coil 21, the lower coil 21 and the middle coil 21, or all three groups of coils 21, thereby increasing energy efficiency and simplifying temperature control.

[0043] In order to facilitate the storage of the mother liquor and the subsequent recrystallization process, a liquid replenishing component 3 is further provided in the tank body 1, which can replenish liquid substances such as additives, catalysts or water into the tank body 1. If additives are added, the storage time of the mother liquor can be extended or the mother liquor can be better maintained in a liquid state; if catalysts or water are added, production conditions can be prepared in advance. For example, in the recrystallization process, the white solid crude product must first be mixed with water. If water is added in advance in the tank body 1, the water temperature can reach a range of 40°C-60°C under the action of the constant temperature component 2. In this way, when the mother liquor enters the decolorization tank or the heating and dissolution link, the heating and dissolution rate of the white solid crude product can be significantly improved.

[0044] Specifically, the liquid infusion assembly 3 includes a liquid infusion main pipe 31 and a bottom liquid distribution pipe 32. The liquid infusion main pipe 31 is vertically fixed in the tank body 1, with the upper end of the liquid infusion main pipe 31 located outside the tank body 1 and the lower end extending to a position close to the bottom of the tank body 1; the bottom liquid distribution pipe 32 is connected to the lower end of the liquid infusion main pipe 31 and is horizontally arranged in the central area of the bottom of the tank body 1. Liquid distribution holes 321 are evenly opened on the bottom liquid distribution pipe 32, and a gap of 15 cm to 20 cm is left between the bottom liquid distribution pipe 32 and the bottom of the tank body 1. At least one height limiting bracket 322 is fixed at the position of the bottom liquid distribution pipe 32 on the bottom of the tank body 1, and the upper end of the height limiting bracket 322 is fixedly connected to the bottom liquid distribution pipe 32.

[0045] Through the above arrangement, the replenished liquid can be uniformly dispersed into the mother liquid through the liquid replenishing main pipe 31, the bottom liquid dispersion pipe 32, and the liquid dispersion hole 321 in sequence, and uniformly mixed with the mother liquid.

[0046] Reference Figure 2 、 Figure 3 The liquid infusion assembly 3 also includes a top liquid diffusion pipe 33, which includes a liquid infusion branch pipe 331 and an annular liquid diffusion pipe 332. One end of the liquid infusion branch pipe 331 is connected to the upper side of the liquid infusion main pipe 31 and the other end is connected to the annular liquid diffusion pipe 332; the annular liquid diffusion pipe 332 is annular and has nozzles 3321 evenly installed on it. The annular liquid diffusion pipe 332 is located in the middle area of the upper part of the tank body 1.

[0047] Through the above arrangement, the replenished liquid can be added from the bottom and the top of the mother liquor at the same time, making it easier to mix evenly.

[0048] Reference Figure 2 、 Figure 4The fluid infusion assembly 3 also includes a relief bracket 34 transversely fixed to the fluid infusion main pipe 31. The relief bracket 34 is positioned lower than the end of the fluid infusion branch pipe 331 that connects to the fluid infusion main pipe 31. It supports the fluid infusion branch pipe 331 and prevents it from bending too much, which could affect fluid flow. Specifically, the relief bracket 34 includes a strut 341 and a fixed pulley 342. One end of the strut 341 is fixedly connected to the fluid infusion main pipe 31, and the fixed pulley 342 is mounted on the other end of the strut 341. The groove depth of the fixed pulley 342 allows the fluid infusion branch pipe 331 to be fully embedded.

[0049] Reference Figure 2 、 Figure 5 The rehydration component 3 also includes a liquid level controller 35, which includes a float 351 and an annular liquid level switch 352. The annular liquid level switch 352 is mounted on the rehydration branch pipe 331 and can control the opening and closing of the rehydration branch pipe 331; the float 351 is installed on the annular liquid level switch 352, and the float 351 is located below the annular liquid level switch 352.

[0050] The liquid level controller 35 is installed at a pre-set position on the liquid replenishment branch 331, that is, at a relatively fixed height within the tank body 1. When the float 351 detects the liquid level, the annular liquid level switch 352 closes the liquid replenishment branch 331. At this time, liquid replenishment is mainly carried out through the bottom liquid diffusion pipe 32, and the mother liquid can be sent to the subsequent recrystallization process at any time through the liquid outlet 12 at the bottom of the tank body 1. Because the replenishment liquid is located at the bottom of the tank body 1, and the liquid outlet 12 is also located at the bottom of the tank body 1 near the liquid replenishment area, the circulating pump will create a disturbance in this area when it draws out the mother liquid. Therefore, the replenishment liquid and mother liquid can be evenly mixed, and the evenly mixed replenishment liquid and mother liquid can be sent to the subsequent recrystallization process. At the same time, when the annular liquid level switch 352 is closed, an electrical signal is generated. After receiving the electrical signal, the external control system can decide to reduce or stop the operation of the liquid replenishment component 3 based on system or manual control. Example 2

[0051] A mother liquor circulation treatment device for producing calcium dobesilate, referring to Figure 2 、 Figure 6 The difference between this embodiment and the first embodiment is that a stirring component 4 for stirring the mother liquor is further installed in the tank body 1. The stirring component 4 can mix the replenishing liquid and the mother liquor more quickly, and can also reduce sedimentation or abnormal crystallization through continuous or intermittent stirring, so that the mother liquor can be better maintained in a liquid state and can be better fed into the subsequent recrystallization process.

[0052] The stirring assembly 4 includes a drive motor 41, a stirring shaft 42, and stirring blades 43. The drive motor 41 is mounted on the top of the tank body 1, with its output end extending into the interior of the tank body 1. The stirring shaft 42 is vertically arranged on the central axis of the tank body 1, and its upper end is fixedly connected to the output end of the drive motor 41. The stirring blades 43 are mounted on the stirring shaft 42 and can be plate-shaped, spiral-shaped, or other shapes. There are two groups of stirring blades 43, each with at least two blades. The blades in the same group are symmetrically arranged to fully stir the upper and lower mother liquors, ensuring uniform mixing of the mother liquors.

[0053] Because the demand for calcium dobesilate varies weekly or quarterly due to market demand during actual production, the amount of mother liquor in tank 1 may also vary. To ensure adequate stirring of the mother liquor regardless of whether the amount is large or small, the mounting structure of the upper set of stirring blades 43 has been improved so that the position of the upper set of stirring blades 43 can be adaptively adjusted up and down.

[0054] Specifically, refer to Figure 6 、 Figure 7 A base 5 is slidably connected to the stirring shaft 42. The base 5 includes an outer frame 51, an inner cylinder 52 and ribs 53. The inner cylinder 52 is slidably sleeved on the stirring shaft 42. A slide groove 421 is provided on the stirring shaft 42 along the vertical direction within the range for the stirring blade 43 to adjust up and down. A slider 521 is protrudingly provided at the position of the inner cylinder 52 corresponding to the slide groove 421; the outer frame 51 is a square frame structure and is sleeved on the outside of the inner cylinder 52, and the stirring blade 43 is fixed on the outer frame 51; there are four ribs 53, which are fixed between the outer frame 51 and the inner cylinder 52 in the direction of the diagonal of the outer frame 51 to fix the outer frame 51 and the inner cylinder 52.

[0055] The base 5 is also provided with a vertical drive member 54 for driving the inner cylinder 52 to slide along the stirring shaft 42, and a vertical positioning member 55 for positioning the inner cylinder 52 after sliding. The vertical drive member 54 includes a housing 541, a rotating power member 542, and a gear 543. The housing 541 is fixed to the outer wall of the inner cylinder 52, and the rotating power member 542 is installed in the housing 541. The rotating power member 542 can use a servo motor. The gear 543 is installed at the output end of the rotating power member 542. The inner cylinder 52 and the slider 521 have a clearance window at the position corresponding to the gear 543. A portion of the gear 543 extends into the inner cylinder 52 through the clearance window. The bottom of the chute 421 of the stirring shaft 42 has a tooth groove 422 along the length direction that is compatible with the gear 543. The rotating power member 542 can drive the gear 543 to rotate, and the gear 543 engages with the tooth groove 422, thereby driving the base 5 to slide up and down, and then driving the stirring blade 43 to adjust its position up and down.

[0056] The vertical positioning member 55 is mounted on the outer wall of the inner cylinder 52. The vertical positioning member 55 includes a contact 553 that elastically extends into the interior of the inner cylinder 52. Positioning holes 423 for the contact 553 to insert are spaced apart vertically on the stirring shaft 42. When the vertical drive member 54 drives the stirring blade 43 to the adjustment position, the contact 553 of the vertical positioning member 55 can be inserted into the positioning hole 423, thereby maintaining the stirring blade 43 in that position, and the vertical drive member 54 no longer needs to be energized. When the position of the stirring blade 43 is to be adjusted, the vertical positioning member 55 and the vertical drive member 54 are energized, the vertical positioning member 55 retracts the contact 553 away from the positioning hole 423, and the vertical drive member 54 drives the stirring blade 43 to adjust its position.

[0057] Specifically, refer to Figure 7 、 Figure 8 The vertical positioning member 55 includes a shell 551, a piston 552, a contact 553, a tension spring 554 and an electromagnet 555. The shell 551 is a cylindrical structure with one end open, and the shell 551 is fixedly connected to the inner cylinder 52; the piston 552 is slidably connected to the shell 551; the contact 553 is connected to the end of the piston 552 close to the opening of the shell 551; the tension spring 554 is wound around the outside of the piston 552, one end of the tension spring 554 is fixed to the open end of the shell 551 and the other end is fixed to the end of the piston 552 close to the closed end of the shell 551. Under the elastic force of the tension spring 554, the movable The plug 552 has a tendency to slide out of the opening of the shell 551, and the contact 553 extends out of the opening of the shell 551; the electromagnet 555 is installed on the side of the shell 551 close to the closed end, and the electromagnet 555 includes a fixed magnet 5551 fixedly connected to the closed end of the shell 551 and a movable magnet 5552 fixedly connected to the end of the piston 552; when the electromagnet 555 is energized, the adsorption force of the fixed magnet 5551 and the movable magnet 5552 is greater than the elastic force of the tension spring 554, which can make the piston 552 slide toward the inside of the shell 551 and the contact 553 retract into the inside of the shell 551.

[0058] In actual use, because there will be a small deviation in the position movement of the base 5 driven by the vertical drive member 54, this deviation will make it difficult for the contact 553 and the positioning hole 423 on the stirring shaft 42 to be completely aligned. Therefore, generally when the vertical drive member 54 is about to reach the adjustment position, the electromagnet 555 will be closed in advance, so that the contact 553 will elastically abut against the stirring shaft 42 under the action of the tension spring 554. When encountering the positioning hole 423, the contact 553 enters the positioning hole 423, and the vertical drive member 54 stops running to achieve positioning. The above positioning form is relatively convenient to operate, but there are two shortcomings in actual use. The first is that due to the elastic abutment, the contact 553 and the positioning hole 423 are worn out quickly; the second is that when the contact 553 enters the positioning hole 423, the vertical drive member 54 stops again, so that the contact 553 will have a delayed small displacement, and this displacement will cause the contact 553 and the positioning hole 423 to produce a shear impact, which will have an adverse effect on the contact 553 and the positioning hole 423 as well as the corresponding vertical drive member 54 and the vertical positioning member 55.

[0059] To this end, the vertical positioning member 55 is improved. The vertical positioning member 55 also includes a damping member 556. The damping member 556 includes an elastic member 5561, a curved column 5562, and a damping ball 5563. A movable cavity 5521 is opened in the horizontal direction at one end of the piston 552 connected to the contact 553. One end of the contact 553 is located in the movable cavity 5521 and the other end is located outside the movable cavity 5521. The length of the part of the contact 553 located in the movable cavity 5521 is longer than the length of the part located outside the movable cavity 5521. A rotating shaft 5531 is installed in the movable cavity 5521. The contact 553 is rotatably installed on the rotating shaft 5531 and has a certain swing space in the up and down directions. The end of the contact 553 located in the movable cavity 5521 is opened in the horizontal direction. A damping chamber 5532 is provided; an elastic member 5561 is installed at the bottom of the damping chamber 5532, and the elastic member 5561 can be a butterfly spring; the curved column 5562 is slidably connected in the damping chamber 5532 and is located on the side of the elastic member 5561 away from the bottom of the damping chamber 5532, and a damping groove 55621 with an inwardly concave cone surface is provided on the end surface of the curved column 5562 away from the elastic member 5561; a part of the damping ball 5563 is located in the damping groove 55621; a hemispherical spherical groove is provided on the side of the active cavity 5521 of the piston 552 corresponding to the damping groove 55621, and the other part of the damping ball 5563 is located in the spherical groove, and the damping ball 5563 is tightly clamped between the damping groove 55621 of the curved column 5562 and the spherical groove of the active cavity 5521.

[0060] When the contact 553 slides on the stirring shaft 42 or enters the positioning hole 423 and generates a shear impact, the contact 553 can perform a small elastic swing based on the damping member 556, thereby reducing the impact between the contact 553 and the positioning hole 423. Specifically, when the contact 553 swings, the contact point between the damping ball 5563 and the damping groove 55621 and the spherical groove changes. As a result, the damping ball 5563 generates a normal force acting on the damping groove 55621 at the contact point between its spherical surface and the damping groove 55621. The axial component of this force further compresses the pre-stressed elastic member 5561, thereby allowing the contact 553 to swing to a certain angle but be subject to a damping effect, thereby providing a certain elastic buffer space while maintaining positioning capability. Example 3

[0061] A mother liquor circulation treatment device for producing calcium dobesilate, referring to Figure 2 、 Figure 9 Because the mother liquor of calcium hydroxybenzenesulfonate contains calcium sulfate and other components, the interior of the tank body 1 and the stirring blade 43 need to be flushed regularly. The difference between this embodiment and the second embodiment is that the stirring blade 43 can be disassembled and assembled with the base 5 through the quick installation component 56. In this way, when flushing, the operator first enters the interior of the tank body 1 through the manhole 13, then removes the stirring blade 43 and takes it out of the tank body 1 for flushing. At the same time, without the obstruction of the stirring blade 43, flushing the interior of the tank body 1 is also more convenient.

[0062] The two sets of stirring blades 43 above and below are both installed on the stirring shaft 42 through the base 5, wherein the base 5 of the lower stirring blade 43 only needs to include an outer frame 51, an inner tube 52 and ribs 53. Because the lower stirring blade 43 does not need to be adjusted up and down, the inner tube 52 and the stirring shaft 42 can be fixedly connected by bolts.

[0063] Specifically, the quick installation assembly 56 includes a plate clamp 561 and a plug connector 562. The plate clamp 561 is fixed on the outer frame 51 of the base 5. The plate clamp 561 includes a bottom plate 5611, a top plate 5612 and two side plates 5613. The bottom plate 5611, the top plate 5612 and the two side plates 5613 form a clamping space for the end of the stirring blade 43 to be inserted. The area of the bottom plate 5611 is larger than the area of the top plate 5612 to provide better support. Three limiting holes 5614 are spaced apart on the top plate 5612, and three through holes are correspondingly opened at the end of the stirring blade 43. The plug connector 562 includes a hand-held portion 5621 and three insertion rods 5622 fixed at intervals below the hand-held portion 5621.

[0064] When in use, the stirring blade 43 can be fixed by inserting the three insertion rods 5622 of the plug connector 562 through the limiting hole 5614 into the through hole of the stirring blade 43; the stirring blade 43 can be disassembled by pulling out the plug connector 562; both installation and disassembly are relatively convenient. Example 4

[0065] A mother liquor circulation treatment device for producing calcium dobesilate, referring to Figure 10 、 Figure 11 The difference between this embodiment and the third embodiment is that a lateral limiter 563 is installed on one of the side plates 5613 of the plate clamp 561, and a plug hole 431 adapted to the lateral limiter 563 is opened on the side surface of the end of the stirring blade 43; the lateral limiter 563 can fix the stirring blade 43 at one more position point, making the stirring blade 43 more stable during the stirring process.

[0066] Specifically, the lateral limiter 563 includes a base shell 5631, a lever 5632, a plug 5633, a compression spring 5634, and a guide post 5635. The base shell 5631 is a rectangular box structure fixed to the side plate 5613, and has an opening on the side facing the side plate 5613; the lever 5632 is V-shaped, horizontally arranged, and the opening is facing the side away from the side plate 5613; with the inflection point of the V-shaped lever 5632 as the reference, the lever 5633 is 2. Half of it is located inside the base shell 5631 and the other half is located outside the base shell 5631. A rotating support 56321 is installed on the side plate 5613 at a position corresponding to the inflection point of the shift lever 5632. The inflection point of the shift lever 5632 is installed on the rotating support 56321, and can swing a certain range based on the rotating support 56321. A pin is installed on the end of the shift lever 5632 located inside the base shell 5631. A strip-shaped clearance hole 56322 is opened along the length direction of the shift lever 5632 at a position corresponding to the pin. The pin passes through the clearance hole 56322 and has a certain sliding space in the clearance hole 56322 along the direction of the clearance hole 56322. The plug 5633 is rotatably connected to the pin. The axis of the plug 5633 is perpendicular to the side plate 5613. A sliding hole for the plug 5633 to slide is opened on the side plate 5613. The position of the sliding hole is consistent with the plug hole 4 31; a guide post 5635 is fixed to the end of the plug 5633 away from the side plate, the axis of the guide post 5635 coincides with the axis of the plug 5633, and a strip hole 56311 for the guide post 5635 to extend and move is opened at the position of the base shell 5631 corresponding to the guide post 5635; a compression spring 5634 is sleeved on the guide post 5635, and both ends of the compression spring 5634 respectively abut the end of the plug 5633 and the side wall of the base shell 5631.

[0067] By adopting the above arrangement, when the stirring blade 43 is to be removed, the plug connector 562 is first pulled out, and then the lever 5632 is pressed to compress the compression spring 5634 to drive the plug 5633 out of the plug hole 431, thereby releasing the restriction on the stirring blade 43. The stirring blade 43 can then be removed. When the stirring blade 43 is to be installed, the lever 5632 is first pressed to drive the plug 5633 out of position, and then the stirring blade 43 is put into place. The lever 5632 is then released, and the plug 5633 can enter the plug hole 431 under the action of the compression spring 5634 to restrict the up and down movement of the stirring blade 43. The plug connector 562 is then inserted to restrict the forward and backward and up and down movement of the stirring blade 43, and finally the installation of the stirring blade 43 is completed. In summary, the removal and installation of the stirring blade 43 are both relatively convenient, and the stirring blade 43 can be easily flushed, and the stability after installation is also relatively good. Example 5

[0068] A mother liquor circulation treatment device for producing calcium dobesilate, referring to Figure 2 、 Figure 12 The difference between this embodiment and the fourth embodiment is that a brushing assembly 57 for brushing the stirring shaft 42 is further provided on the upper base 5. The brushing assembly 57 includes a fixed clamp 571, a ring brush 572 and a groove brush 573. The fixed clamp 571 is annular and clamped on the outer wall of the inner cylinder 52. The central axis of the fixed clamp 571 coincides with the central axis of the inner cylinder 52; the ring brush 572 includes a column 5721, a positioning ring 5722 and a brush 5723. The column 5721 has multiple columns and is fixed on the fixed clamp 571 in a circular array at equal intervals. The central axis of the positioning ring 5722 coincides with the central axis of the fixed clamp 571. The positioning ring 5722 is fixed to the column 5721. The brush 5723 723 is evenly fixed on the inner edge of the positioning ring 5722 and the end of the bristle 1 5723 elastically abuts against the stirring shaft 42; the groove brush 573 includes a vertical plate 5731, a rotating cylinder 5732 and bristles 2 5733, the vertical plate 5731 is fixed on the fixed clamp 571, the rotating cylinder 5732 is horizontally rotated and connected to the vertical plate 5731, the position of the rotating cylinder 5732 corresponds to the position of the slide groove 421 on the stirring shaft 42, the bristles 2 5733 are evenly fixed on the outer surface of the rotating cylinder 5732 and the end of the bristles 2 5733 elastically abuts against the slide groove 421.

[0069] Through the above arrangement, the upper area of the stirring shaft 42 can open the vertical driving member 54 to drive the base 5 to move up and down, so that the annular brush 572 and the groove brush 573 can brush the stirring shaft 42 and the slide groove 421; at the same time, the annular liquid dispersion tube 332 is placed on the positioning ring 5722 of the annular brush 572, and the rotation of the stirring shaft 42 does not interfere with the annular liquid dispersion tube 332. The nozzle 3321 of the annular liquid dispersion tube 332 can spray the flushing liquid onto the stirring shaft 42. Of course, the flushing liquid can also be sprayed manually with a handheld high-pole spray gun, which is more convenient. As for the lower area of the stirring shaft 42, because it is located at a lower position, it can be brushed quickly and conveniently by hand.

[0070] The implementation principle of the embodiment of the present application is as follows: specifically, a mother liquor circulation treatment method combined with a mother liquor circulation treatment device, first, when the process production line of calcium dobesilate recrystallization is running, the mother liquor centrifuged during the recrystallization is recovered and stored; at the same time, the constant temperature component 2 is turned on to stabilize the temperature of the mother liquor in the tank body 1 in the range of 40°C-60°C; then, the stirring component 4 is turned on continuously or intermittently to stir the mother liquor in the tank body 1 so that the mother liquor is well maintained in a liquid state; then, based on the storage time or the requirements of the subsequent recrystallization process, additives, catalysts, water or other liquid substances are added to the mother liquor in the tank body 1 through the liquid replenishing component 3. If the additives are added, the storage time of the mother liquor can be extended or the mother liquor can be better kept in a liquid state. solid state; if the catalyst or water is added, the production conditions can be prepared in advance. For example, in the recrystallization process, the white solid crude product must first be mixed with water. If water is added in advance in the tank body 1, the water temperature can reach 40°C-60°C under the action of the constant temperature component 2. In this way, when the mother liquor enters the decolorization tank or the heating and dissolution link, the heating and dissolution speed of the white solid crude product can be significantly improved; the mother liquor finally stored can be sent to the subsequent or next batch of recrystallization process for reuse, and the waste of mother liquor is significantly reduced; secondly, because the mother liquor can be recovered and stored, there is no need to worry about waste, so each production does not need to be strictly controlled like before, and the production continuity and production efficiency are significantly improved.

[0071] The examples of this specific embodiment are all preferred embodiments of this application and are not intended to limit the scope of protection of this application. Identical components are represented by the same reference numerals. Therefore, any equivalent changes made based on the structure, shape, and principle of this application should be included in the scope of protection of this application.

Claims

1. A mother liquor circulation treatment device for producing calcium dobesilate, which is installed in a process line for recrystallization of calcium dobesilate, comprising a tank body (1), characterized in that: The tank body (1) is provided with a liquid inlet (11) for the mother liquid to enter at the upper portion and a liquid outlet (12) for the mother liquid to flow out at the lower portion; A constant temperature component (2) is further provided in the tank body (1), and the constant temperature component (2) includes a coil (21). There are three groups of coils (21) installed in the upper, middle and lower parts of the tank body (1) in sequence. A fluid replenishment assembly (3) is further provided in the tank body (1), the fluid replenishment assembly (3) comprising a fluid replenishment main pipe (31) and a bottom fluid distribution pipe (32), the upper end of the fluid replenishment main pipe (31) being located outside the tank body (1) and the lower end extending to a position close to the bottom of the tank body (1); the bottom fluid distribution pipe (32) being connected to the lower end of the fluid replenishment main pipe (31) and being horizontally provided in the center area of the bottom of the tank body (1); and fluid distribution holes (321) being uniformly provided on the bottom fluid distribution pipe (32); The rehydration assembly (3) further comprises a top liquid dispersion pipe (33), the top liquid dispersion pipe (33) comprising a liquid dispersion branch pipe (331) and an annular liquid dispersion pipe (332), one end of the liquid dispersion branch pipe (331) being connected to the upper side of the liquid dispersion main pipe (31) and the other end being connected to the annular liquid dispersion pipe (332); the annular liquid dispersion pipe (332) being annular in shape and having nozzles (3321) evenly mounted thereon, the annular liquid dispersion pipe (332) being located in the middle region of the upper inner portion of the tank body (1); A stirring assembly (4) is further provided in the tank body (1), the stirring assembly (4) comprising a stirring shaft (42), the stirring shaft (42) being provided with a chute (421); the stirring shaft (42) being slidably connected to a base (5) at the position of the chute (421), the base (5) being provided with a vertical driving member (54) for driving the base (5) to slide; A brushing assembly (57) for brushing the stirring shaft (42) is also provided on the base (5). The brushing assembly (57) includes a fixing clamp (571), a ring brush (572) and a groove brush (573). The ring brush (572) includes a column (5721), a positioning ring (5722) and a brush bristle (5723). In the upper area of the stirring shaft (42), the vertical driving member (54) can be opened to drive the base (5) to move up and down, so that the ring brush (572) and the groove brush (573) brush the stirring shaft (42) and the chute (421); The annular liquid dispersion pipe (332) is placed on the positioning ring (5722) of the annular brush (572), and the flushing liquid can be sprayed onto the stirring shaft (42) through the nozzle (3321) of the annular liquid dispersion pipe (332).

2. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 1, characterized in that: The fluid infusion assembly (3) further comprises a position-avoiding bracket (34) transversely fixed on the fluid infusion main pipe (31), the position of the position-avoiding bracket (34) being lower than one end of the fluid infusion branch pipe (331) connected to the fluid infusion main pipe (31); the position-avoiding bracket (34) comprises a support rod (341) and a fixed pulley (342), one end of the support rod (341) being fixedly connected to the fluid infusion main pipe (31), the fixed pulley (342) being mounted on the other end of the support rod (341), and the fluid infusion branch pipe (331) being embedded in a wheel groove of the fixed pulley (342).

3. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 1, characterized in that: The liquid replenishing assembly (3) further comprises a liquid level controller (35), the liquid level controller (35) comprising a float (351) and an annular liquid level switch (352), the annular liquid level switch (352) being mounted on the liquid replenishing branch pipe (331) to control the opening and closing of the liquid replenishing branch pipe (331); the float (351) being mounted on the annular liquid level switch (352), and the float (351) being located below the annular liquid level switch (352).

4. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 1, characterized in that: The stirring assembly (4) comprises a driving motor (41) and stirring blades (43); the driving motor (41) is mounted on the top of the tank body (1) and the output end thereof extends into the interior of the tank body (1); the stirring shaft (42) is vertically arranged on the central axis of the tank body (1) and the upper end thereof is fixedly connected to the output end of the driving motor (41); the stirring blades (43) are mounted on the stirring shaft (42), and there are two upper and lower groups of stirring blades (43).

5. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 4, characterized in that: The base (5) comprises an outer frame (51), an inner cylinder (52) and a rib plate (53); the inner cylinder (52) is slidably sleeved on the stirring shaft (42); a chute (421) is provided on the stirring shaft (42) within a range for vertical adjustment of the stirring blade (43); a slider (521) is protrudingly provided at a position of the inner cylinder (52) corresponding to the chute (421); the outer frame (51) is sleeved and fixed to the outside of the inner cylinder (52) through the rib plate (53); the stirring blade (43) is fixed to the outer frame (51); a vertical driving member (54) The invention is used to drive the inner cylinder (52) to slide along the stirring shaft (42); a vertical positioning member (55) is also provided on the base (5) for positioning the position of the inner cylinder (52) after sliding; the vertical driving member (54) comprises a shell (541), a rotating power member (542) and a gear (543); the shell (541) is fixed on the outer wall of the inner cylinder (52); the rotating power member (542) is installed in the shell (541); the gear (543) is installed at the output end of the rotating power member (542); the inner cylinder (52) and the slider (521) are provided with a clearance window at a position corresponding to the gear (543); a part of the gear (543) extends into the inner cylinder (52) through the clearance window; the bottom of the slide groove (421) of the stirring shaft (42) is provided with a tooth groove (422) adapted to the gear (543) along the length direction.

6. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 5, characterized in that: The vertical positioning member (55) is installed on the outer wall of the inner cylinder (52). The vertical positioning member (55) includes a shell (551), a piston (552), a contact (553), a tension spring (554) and an electromagnet (555). The shell (551) is a cylindrical structure with one end open. The shell (551) is fixedly connected to the inner cylinder (52); the piston (552) is slidably connected to the shell (551); the contact (553) is connected to the end of the piston (552) close to the opening of the shell (551); the tension spring (554) is wound around the outside of the piston (552), one end of the tension spring (554) is fixed to the open end of the shell (551) and the other end is fixed to the piston (552). ) is fixed at one end close to the closed end of the housing (551), and under the elastic force of the tension spring (554), the piston (552) has a tendency to slide out of the opening of the housing (551), and the contact (553) extends out of the opening of the housing (551); the electromagnet (555) is installed on one side close to the closed end in the housing (551), and the electromagnet (555) includes a fixed magnet (5551) fixedly connected to the closed end of the housing (551) and a movable magnet (5552) fixedly connected to the end of the piston (552); when the electromagnet (555) is energized, the adsorption force of the fixed magnet (5551) and the movable magnet (5552) is greater than the elastic force of the tension spring (554).

7. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 6, characterized in that: The vertical positioning member (55) further includes a damping member (556), which includes an elastic member (5561), a curved column (5562), and a damping ball (5563). A movable cavity (5521) is provided in the horizontal direction at one end of the piston (552) connected to the contact (553). One end of the contact (553) is located in the movable cavity (5521) and the other end is located outside the movable cavity (5521). The length of the portion of the contact (553) located in the movable cavity (5521) is longer than the length of the portion located outside the movable cavity (5521). A rotating shaft (5531) is installed in the movable cavity (5521). The contact (553) is rotatably installed on the rotating shaft (5531) and has a certain swing space in the up and down directions. The end of the contact (553) located in the movable cavity (5521) is horizontally opened. A damping chamber (5532) is provided in the direction of the spring; an elastic member (5561) is installed at the bottom of the damping chamber (5532); a curved column (5562) is slidably connected in the damping chamber (5532) and is located on the side of the elastic member (5561) away from the bottom of the damping chamber (5532); a damping groove (55621) with an inward concave conical surface is provided on the end surface of the curved column (5562) away from the elastic member (5561); a damping ball A portion of the damping ball (5563) is located in the damping groove (55621); a hemispherical spherical groove is provided on one side of the movable cavity (5521) of the piston (552) corresponding to the damping groove (55621), and the other portion of the damping ball (5563) is located in the spherical groove. The damping ball (5563) is tightly clamped between the damping groove (55621) of the curved column (5562) and the spherical groove of the movable cavity (5521).

8. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 7, characterized in that: The elastic member (5561) is a butterfly spring.

9. A mother liquor circulation treatment device for producing calcium dobesilate according to claim 5, characterized in that: The base (5) is provided with a quick installation component (56), which includes a plate clamp (561) and a plug connector (562). The plate clamp (561) is fixed to the outer frame (51) of the base (5). The plate clamp (561) includes a bottom plate, a top plate and two side plates, which form a clamping space for the end of the stirring blade (43) to be inserted. Three limiting holes (5611) are spaced apart on the top plate, and three through holes are correspondingly opened at the end of the stirring blade (43). The plug connector (562) includes a handheld portion (5621) and three plug rods (5622) fixed at intervals below the handheld portion (5621).

10. A method for circulating and treating mother liquor for producing calcium dobesilate, suitable for the mother liquor circulating and treating device for producing calcium dobesilate according to any one of claims 1 to 9, characterized in that: The following steps are included: First, when the calcium dobesilate recrystallization production line is running, the mother liquor after centrifugation in the recrystallization is recovered and stored; At the same time, the constant temperature component (2) is turned on to stabilize the temperature of the mother liquid in the tank (1) in the range of 40°C to 60°C; Afterwards, the stirring component (4) is continuously or intermittently turned on to stir the mother liquid in the tank (1); Afterwards, based on the storage time or the requirements of the subsequent recrystallization process, liquid substances such as additives, catalysts or water are added to the mother liquid in the tank body (1) through the liquid replenishing component (3); Finally, the stored mother liquor is sent back to the subsequent or next batch of recrystallization process for reuse.

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