Crystallization treatment device for imidazole processing and process thereof

Abstract

The invention relates to the related technical field of drug synthesis, and discloses a crystallization treatment device for imidazole processing and a process thereof.The device comprises a crystallizer body, a water bath is arranged in the inner wall of the crystallizer body, a feeding pipe is arranged on the upper side of the crystallizer body, and a discharging pipe is arranged on the lower side of the crystallizer body; two sowing assemblies are arranged at the two ends of the interior of the crystallizer body. The reciprocating frequency of the piston plate in the cylinder can be controlled by controlling the rotating speed of the rotating shaft, so that a solvating-out agent in an external solvating-out agent box is controlled to be pumped into the hydraulic cavity through the feeding valve according to the reciprocating frequency of the piston plate in the cylinder; therefore, a solution in the crystallizer body is stirred at a proper speed by the sowing assembly, a solventing-out agent is dropwise added into the crystallizer body at a certain speed, and the phenomenon of poor crystal form is avoided.

Description

Technical Field

[0001] The invention belongs to the technical field related to drug synthesis, and more specifically, particularly relates to a crystallization treatment device for imidazole processing and a process thereof. Background Art

[0002] Imidazole is an important chemical raw material and pharmaceutical intermediate. Its derivatives are downstream products of imidazole, mainly including monomethylimidazole, dimethylimidazole and dozens of other series of products. They are used as curing agents for epoxy resins, accounting for less than half of the imidazole consumption in Japan. They can also be used as drugs for the treatment of trichomoniasis and turkey blackhead disease. In the production of imidazole antifungal drugs such as dichlorobenzazole, econazole and clotrimazole, imidazole is one of the main raw materials, so it is of great significance in various industries. With the rapid development of the field of biochemistry, imidazole and its derivatives are favored by the market, and the domestic market demand is increasing. Imidazole products have broad market prospects, the demand for project products has been showing a rapid growth, and new uses are constantly being developed. At present, the production capacity of the domestic industry is far from meeting the growing demand of the domestic market, and there is a large room for development. However, the drug synthesis in the existing technology has the following defects: In the prior art, when imidazole is crystallized, a solvent is usually added dropwise to a saturated imidazole solution. However, in the current crystallization treatment device for imidazole processing, the solvent is usually added dropwise above the saturated imidazole solution, resulting in a limited contact area between the saturated imidazole solution and the solvent, making it difficult to fully contact the saturated imidazole solution with the solvent. In the prior art, when a dissolving agent is dripped into a crystallization treatment device for imidazole processing, in order to increase the ratio of the imidazole saturated solution to the dissolving agent, a spreading component is usually installed in the imidazole saturated solution. However, the spreading component is located in the imidazole saturated solution, which easily causes the through hole of the spreading component to be blocked by crystals, thereby affecting the use of the spreading component. In the prior art, during the use of the crystallization treatment device for imidazole processing, poor crystal morphology is prone to occur. The reasons for the poor crystal morphology are due to factors such as improper stirring speed, inaccurate temperature control or too fast solvent drop acceleration; too fast stirring speed may destroy the crystal structure, and temperature fluctuations may affect the growth rate and morphology of the crystal; too fast solvent drop acceleration may lead to excessive local concentration, thereby quickly precipitating a large number of tiny crystals; therefore, the stirring speed and the solvent drop acceleration need to be coordinated with each other.

[0003] Therefore, in view of this, the existing structure and defects are studied and improved, and a crystallization treatment device and process for imidazole processing are provided, in order to achieve a more practical and valuable purpose. Summary of the invention

[0004] The present invention provides a crystallization treatment device for imidazole processing and a process thereof, which are used to overcome the above-mentioned defects in the prior art.

[0005] The purpose and effect of the crystallization treatment device for imidazole processing and the process thereof of the present invention are achieved by the following specific technical means: A crystallization treatment device for imidazole processing comprises a crystallizer body, a water bath is provided in the inner wall of the crystallizer body, a feed pipe is provided on the upper side of the crystallizer body, a discharge pipe is provided on the lower side of the crystallizer body, and two spreading assemblies are provided at both ends of the interior of the crystallizer body; the spreading assembly comprises a cylinder, the cylinder is fixed at one end of the interior of the crystallizer body, a piston plate is slidably provided inside the cylinder, a hydraulic chamber and a mixing chamber are separated from the interior of the cylinder by the piston plate, a plurality of first guide plates are fixedly provided on the side of the piston plate close to the mixing chamber, a circular tube is fixedly provided in the middle of each of the first guide plates, one end of the circular tube extends to the outside of the cylinder, a first spreading plate is fixedly provided at one end of the circular tube, a first slide plate is slidably provided inside the first spreading plate, a plurality of second spreading plates are fixedly provided on one side of the first slide plate, and a plurality of through holes are provided at intervals on both sides of each of the second spreading plates. One end of each of the second spreading plates extends to the outside of the first spreading plate, and two second slide plates are symmetrically arranged in the middle of the interior of each of the second spreading plates. A plurality of cleaning blocks are fixedly arranged at intervals on the sides of the two second slide plates away from each other, and two pairs of hollow elastic members are interconnected between the sides of each pair of the second slide plates away from each other and the two sides of the interior of each of the second spreading plates, and a connecting channel is arranged between the interior of each of the hollow elastic members and the through hole.

[0006] A further technical solution is that a plurality of second guide plates are fixedly provided on one side of the first spreading plate away from the second spreading plate, and both sides of one end of each of the second guide plates are respectively in sliding contact with the inclined surfaces of one end of each pair of the second slide plates, and two grooves are provided in the middle of the side close to each other of each pair of the second slide plates, and a plurality of first protrusions are fixedly provided at intervals in each of the grooves, and a plurality of second protrusions are fixedly provided at intervals on both sides of each of the second guide plates, and each of the first protrusions is in sliding contact with each of the second protrusions.

[0007] A further technical solution is that a rotating shaft is provided inside the crystallizer body, and a plurality of L-shaped parts are provided in a circular array on the outer walls at both ends of the rotating shaft, one end of each of the L-shaped parts is fixedly connected to the outer wall of the rotating shaft, the other end of each of the L-shaped parts is fixedly connected to the first slide plate, and the other end of each of the L-shaped parts is in sliding contact with the first spreading plate.

[0008] According to a further technical solution, two first sleeves are sleeved on the outer walls at both ends of the rotating shaft, and the inner wall of each of the first sleeves is in sliding contact with the outer wall of the rotating shaft. A first slider is fixedly provided on one side of the outer walls at both ends of the rotating shaft, and the outer portion of each of the first sliders is in axial sliding contact with the inner wall of the first sleeve.

[0009] A further technical solution is that a second sleeve is fixedly provided on one side of each of the cylinders, the inner wall of the second sleeve is in sliding contact with the outer wall of the first sleeve, a second slider is fixedly provided on one side of the outer wall of the first sleeve, the inner wall of the second sleeve is provided with a spiral groove which is interconnected at the head and tail, the second slider spirally slides in the spiral groove, and the outer wall of one end of the first sleeve is fixedly connected to the piston plate.

[0010] A further technical solution is that the hydraulic chamber is connected to the outside of the crystallizer body and is provided with a feed valve, the piston plate is provided with a first one-way valve, the hydraulic chamber is communicated with the mixing chamber through the first one-way valve, a second one-way valve is provided on the inner wall of one end of the circular tube, the interior of the circular tube is communicated with the hydraulic chamber through the second one-way valve, the interior of the circular tube is communicated with the interior of the first spreading plate, the interior of the first spreading plate is communicated with the interior of the first slide plate, the interior of the first slide plate is communicated with the interior of the second spreading plate, and a pressure relief valve is provided on one side of the hydraulic chamber.

[0011] According to a further technical solution, a first arc-shaped scraper is fixedly provided on one side of the outside of the first spreading plate, and a second arc-shaped scraper is fixedly provided on the other side of the outside of the first spreading plate, the inner wall of the first arc-shaped scraper is in sliding contact with the outer wall of the rotating shaft, and the outer wall of the second arc-shaped scraper is in sliding contact with the inner wall of the crystallizer body.

[0012] A further technical solution is that a circular plate is rotatably provided on one side of the mixing chamber, a plurality of openings are provided in a circular array on the circular plate, two baffles are slidably provided on both sides of each opening, one end of each pair of baffles close to each other is in sliding contact with the inclined surfaces on both sides of one end of the first guide plate, two springs are provided between one end of each pair of baffles far away from each other and the inside of the circular plate, an annular plate is fixedly provided on the outer wall of the circular plate, and the annular plate slides in an annular manner in the inner wall of the cylinder.

[0013] A further technical solution is that a circular ring is fixedly provided on one side of the circular plate close to the mixing chamber, the inner wall of the circular ring is a conical structure, a plurality of rubber parts are fixedly provided at intervals on both sides of the first guide plate, one end of each of the rubber parts is in contact with the inner wall of the mixing chamber, a stepper motor is installed at one end of the outside of the crystallizer body, the output end of the stepper motor is fixedly connected to one end of the rotating shaft, an inlet valve is provided at one end of the water bath, a water outlet valve is provided at the other end of the water bath, and two support frames are fixedly provided on the lower sides of both ends of the crystallizer body.

[0014] A crystallization process for imidazole processing comprises the following steps: S1: Prepare a saturated solution. According to the dissolved phase equilibrium experimental data, prepare a saturated imidazole solution in the crystallizer; S2: Temperature control, using a constant temperature water bath to control the temperature of the crystallizer; S3: dripping the solvent, making the temperature of the solvent consistent with the temperature of the saturated solution, and dripping the solvent into the crystallizer at a certain rate by using a stirring component; S4: stirring and growing crystals, stirring is started while dripping the solvent, and when crystals are precipitated, the dripping of the solvent is stopped, a certain amount of seed crystals is added, and the temperature and stirring rate are kept unchanged to grow crystals; S5: post-treatment, aging, filtering, drying and other treatments are performed on the crystals to obtain imidazole crystal products.

[0015] Compared with the prior art, the present invention has the following beneficial effects: The present invention provides a crystallization treatment device for imidazole processing. Through the arrangement of a piston plate, a first guide plate, and a through-port, the piston plate moves to suck the imidazole saturated solution in the crystallizer body into the mixing chamber through the through-port, so that the imidazole saturated solution and the dissolving agent are preliminarily mixed in the mixing chamber; and the rotation of the piston plate drives the rotation of a plurality of first guide plates, and the rotation of the plurality of first guide plates mixes the imidazole saturated solution and the dissolving agent in the mixing chamber, promoting the imidazole saturated solution and the dissolving agent to fully contact. Then, through the arrangement of a baffle plate and a spring, the movement of the piston plate drives the movement of the plurality of first guide plates, and the ends of the two baffle plates that are close to each other are respectively in sliding contact with the inclined surfaces on both sides of one end of the first guide plate, and the movement of the first guide plate guides and pushes the two baffle plates, so that the two baffle plates are moved away from each other, so as to increase the liquid flow through the through-port, so that the imidazole saturated solution and the dissolving agent preliminarily mixed in the mixing chamber are sprayed into the crystallizer body through the plurality of through-ports, further making the imidazole saturated solution and the dissolving agent fully contact, and avoiding crystallization from being blocked in the through-port.

[0016] The invention discloses a crystallization treatment device for imidazole processing, which controls the frequency of the piston plate moving back and forth in the cylinder by controlling the rotation speed of the rotating shaft, so as to control the solvent in the external solvent box to be drawn into the hydraulic cavity through the feed valve through the frequency of the piston plate moving back and forth in the cylinder, so that the spreading component can stir the solution in the crystallizer body at an appropriate speed and drip the solvent into the crystallizer body at a certain rate, thereby avoiding the phenomenon of poor crystal morphology.

[0017] The present invention discloses a crystallization treatment device for imidazole processing. The circular tube, the L-shaped member, the first slide plate, the second spreading plate and the through hole are arranged. The piston plate moves to drive the circular tube and the first spreading plate to move. The piston plate is fixed to the outer wall of the rotating shaft by the L-shaped member. The first slide plate is resisted by the L-shaped member. The first spreading plate moves to cooperate with the first slide plate and is fixed to a plurality of second spreading plates. The plurality of second spreading plates are extended from the first spreading plate so that the plurality of through holes on the second spreading plate are all located outside the first spreading plate. The solvent in the first spreading plate enters the plurality of second spreading plates through the interior of the first slide plate. The solvent in the second spreading plate is sprayed into the middle of the inner part of the crystallizer body through a plurality of through holes; and the rotation of the piston plate drives the plurality of round tubes to rotate, and the rotation of the round tubes drives the first spreading plate to rotate; the rotation of the rotating shaft drives the L-shaped part to rotate, so that the L-shaped part and the first spreading plate rotate synchronously, so that the first slide plate and the plurality of second spreading plates rotate, so that the solvent is diffusely sprayed through a plurality of through holes, increasing the contact area between the saturated imidazole solution and the solvent, which is beneficial to promoting the efficiency of imidazole crystallization, so that the solvent can be dripped into the crystallizer body at a certain rate using the spreading component.

[0018] The present invention provides a crystallization treatment device for imidazole processing. Through the arrangement of the second slide plate, the cleaning block, and the second guide plate, the first spreading plate moves to drive the movement of the plurality of second guide plates. The two sides of one end of the second guide plate respectively make sliding contact with the inclined surfaces of one end of the two second slide plates. One end of the second guide plate passes through the interior of the first slide plate and enters the second spreading plate. The movement of the second guide plate guides and pushes the two second slide plates, so that the two second slide plates move away from each other. The two second slide plates move away from each other to drive the plurality of cleaning blocks to move away from each other. The plurality of cleaning blocks move away from each other and enter the plurality of through holes respectively, so that the crystals blocked in the through holes are pushed out to avoid blockage of the through holes. Through the arrangement of the hollow elastic member and the connecting channel, the two second slide plates move away from each other to squeeze and compress the plurality of hollow elastic members respectively, so that the solution in the hollow elastic member is sprayed into the through hole through the connecting channel, which is conducive to the dredging effect of the through hole by the high-pressure solution. Finally, through the arrangement of the first protrusion and the second protrusion, under the guiding action of the first protrusion and the second protrusion and the elastic force of a plurality of pairs of hollow elastic members, the two second slides can be alternately moved closer to and farther from each other by a small amplitude, so that the cleaning block can move back and forth in the through hole by a small amplitude, further clearing the crystals blocked in the through hole, thereby utilizing the spreading assembly to drip the dissolving agent into the crystallizer body at a certain rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0020] The present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0021] Figure 1 It is an isometric structural schematic diagram of the present invention; Figure 2 It is a schematic diagram of the top view of the structure of the present invention; Figure 3 for Figure 2 Schematic diagram of the cross-sectional structure at AA in the middle; Figure 4 for Figure 3 A schematic diagram of the local enlarged structure at C in the middle; Figure 5 for Figure 3 A schematic diagram of the local enlarged structure at D in the middle; Figure 6 for Figure 3 A schematic diagram of the local enlarged structure at E in the middle; Figure 7 for Figure 6 A schematic diagram of the local enlarged structure at F in the middle; Figure 8 for Figure 6 Schematic diagram of the local enlarged structure at G in the middle; Fig. 9 It is a front view structural schematic diagram of the present invention; Fig.10 for Fig. 9 Schematic diagram of the cross-sectional structure at the middle BB; Fig.11 for Fig.10 Schematic diagram of the local enlarged structure at H in the middle; Fig.12 for Fig.10 Schematic diagram of the local enlarged structure at K in the middle; Fig.13 It is an isometric structural schematic diagram of the second sleeve in the present invention; Fig.14 It is a schematic cross-sectional structural diagram of the second sleeve in the present invention.

[0022] Description of reference numerals: Crystallizer body 10, stepper motor 11, support frame 12, feed pipe 13, discharge pipe 14, water inlet valve 15, water outlet valve 16, feed valve 17, water bath 18, rotating shaft 19, cylinder 20, piston plate 21, hydraulic chamber 22, mixing chamber 23, first guide plate 24, round tube 25, rubber member 26, ring 27, round plate 28, through port 29, baffle 30, spring 31, annular plate 32, first spreading plate 33, first slide plate 34 , L-shaped part 35, pressure relief valve 36, first arc scraper 37, second arc scraper 38, second spreading plate 39, through hole 40, second slide plate 41, hollow elastic part 42, cleaning block 43, connecting channel 45, groove 46, first protrusion 47, second guide plate 48, second protrusion 49, first one-way valve 51, second one-way valve 52, first sleeve 53, first slider 54, second sleeve 55, second slider 56, spiral slide groove 57. DETAILED DESCRIPTION

[0023] The following embodiments of the present invention are described in further detail in conjunction with the accompanying drawings and examples. The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0024] In the description of the present invention, unless otherwise specified, "plurality" means two or more than two; the orientations or positional relationships indicated by the terms "upper", "lower", "left", "right", "inner", "outer", "front end", "rear end", "head", "tail", etc. are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", "third", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0025] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connected" and "connection" 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 or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0026] As attached Figure 1 To Attachment Fig.14 As shown: The invention provides a crystallization treatment device for imidazole processing.

[0027] See attached Figure 1 To Attachment Fig.14, including a crystallizer body 10, a water bath 18 is provided in the inner wall of the crystallizer body 10, a feed pipe 13 is provided on the upper side of the crystallizer body 10, a discharge pipe 14 is provided on the lower side of the crystallizer body 10, and two spreading assemblies are provided at both ends of the interior of the crystallizer body 10; the spreading assembly includes a cylinder 20, the cylinder 20 is fixed at one end of the interior of the crystallizer body 10, a piston plate 21 is slidably provided inside the cylinder 20, a hydraulic chamber 22 and a mixing chamber 23 are separated inside the cylinder 20 by the piston plate 21, a plurality of first guide plates 24 are fixedly provided on one side of the piston plate 21 close to the mixing chamber 23, a circular tube 25 is fixedly provided in the middle of each first guide plate 24, one end of the circular tube 25 extends to the outside of the cylinder 20, a first spreading plate 33 is fixedly provided at one end of the circular tube 25, a first slide plate 34 is slidably provided inside the first spreading plate 33, a plurality of second spreading plates 39 are fixedly provided at intervals on one side of the first slide plate 34, and a plurality of through holes 40 are provided at intervals on both sides of each second spreading plate 39. One end of each second spreading plate 39 extends to the outside of the first spreading plate 33, and two second slide plates 41 are symmetrically provided in the middle of the interior of each second spreading plate 39, and a plurality of cleaning blocks 43 are fixedly provided at intervals on the sides of the two second slide plates 41 away from each other, and two pairs of hollow elastic members 42 are interconnected between the sides of each pair of second slide plates 41 away from each other and the inner sides of each second spreading plate 39, and a connecting channel 45 is provided between the interior of each hollow elastic member 42 and the through hole 40.

[0028] Preferably, see Attachment Figure 6 To Attachment Figure 8 , Attachment Fig.12 A plurality of second guide plates 48 are fixedly provided on one side of the first spreading plate 33 away from the second spreading plate 39, and both sides of one end of each second guide plate 48 are in sliding contact with the inclined surface of one end of each pair of second slide plates 41 respectively, and two grooves 46 are provided in the middle of the side close to each other of each pair of second slide plates 41, and a plurality of first protrusions 47 are fixedly provided in each groove 46 at intervals, and a plurality of second protrusions 49 are fixedly provided on both sides of each second guide plate 48 at intervals, and each first protrusion 47 is in sliding contact with each second protrusion 49.

[0029] Preferably, see Attachment Fig. 9 To Attachment Fig.10 , Attachment Fig.12 A rotating shaft 19 is provided inside the crystallizer body 10 for rotation, and a plurality of L-shaped parts 35 are provided in a circular array on the outer walls at both ends of the rotating shaft 19. One end of each L-shaped part 35 is fixedly connected to the outer wall of the rotating shaft 19, and the other end of each L-shaped part 35 is fixedly connected to the first slide plate 34, and the other end of each L-shaped part 35 is in sliding contact with the first spreading plate 33.

[0030] Preferably, see Attachment Figure 3 To Attachment Figure 4Two first sleeves 53 are sleeved on the outer walls at both ends of the rotating shaft 19, and the inner wall of each first sleeve 53 is in sliding contact with the outer wall of the rotating shaft 19. A first slider 54 is fixedly provided on one side of the outer wall at both ends of the rotating shaft 19, and the outer portion of each first slider 54 is in axial sliding contact with the inner wall of the first sleeve 53.

[0031] Preferably, see Attachment Figure 3 To Attachment Figure 4 , Attachment Fig.13 , Attachment Fig.14 A second sleeve 55 is fixedly provided on one side of each cylinder 20, and the inner wall of the second sleeve 55 is in sliding contact with the outer wall of the first sleeve 53. A second slider 56 is fixedly provided on one side of the outer wall of the first sleeve 53. The inner wall of the second sleeve 55 is provided with a spiral groove 57 which is interconnected at the head and tail. The second slider 56 spirally slides in the spiral groove 57, and the outer wall of one end of the first sleeve 53 is fixedly connected to the piston plate 21.

[0032] Preferably, see Attachment Figure 1 To Attachment Figure 3 , Attachment Figure 6 , Attachment Figure 7 , Attachment Fig. 9 To Attachment Fig.12 The hydraulic chamber 22 is connected to the outside of the crystallizer body 10 and is provided with a feed valve 17. A first one-way valve 51 is provided on the piston plate 21. The hydraulic chamber 22 is communicated with the mixing chamber 23 through the first one-way valve 51. A second one-way valve 52 is provided on the inner wall of one end of the circular tube 25. The interior of the circular tube 25 is communicated with the hydraulic chamber 22 through the second one-way valve 52. The interior of the circular tube 25 is communicated with the interior of the first spreading plate 33. The interior of the first spreading plate 33 is communicated with the interior of the first slide plate 34. The interior of the first slide plate 34 is communicated with the interior of the second spreading plate 39. A pressure relief valve 36 is provided on one side of the hydraulic chamber 22.

[0033] Preferably, see Attachment Figure 3 , Attachment Figure 6 , Attachment Fig.12 A first arc scraper 37 is fixedly provided on one side of the outside of the first spreading plate 33, and a second arc scraper 38 is fixedly provided on the other side of the outside of the first spreading plate 33. The inner wall of the first arc scraper 37 is in sliding contact with the outer wall of the rotating shaft 19, and the outer wall of the second arc scraper 38 is in sliding contact with the inner wall of the crystallizer body 10.

[0034] Preferably, see Attachment Fig. 9 To Attachment Fig.10A circular plate 28 is rotatably provided on one side of the mixing chamber 23, and a plurality of through holes 29 are arranged in a circular array on the circular plate 28. Two baffles 30 are slidably provided on both sides of each through hole 29. One end of each pair of baffles 30 close to each other is in sliding contact with the inclined surfaces on both sides of one end of the first guide plate 24. Two springs 31 are connected between one end of each pair of baffles 30 away from each other and the inside of the circular plate 28. An annular plate 32 is fixedly provided on the outer wall of the circular plate 28, and the annular plate 32 slides in an annular manner in the inner wall of the cylinder 20.

[0035] Preferably, see Attachment Figure 1 To Attachment Figure 3 , Attachment Figure 5 , Attachment Fig. 9 To Attachment Fig.11 A circular ring 27 is fixedly provided on one side of the circular plate 28 close to the mixing chamber 23, and the inner wall of the circular ring 27 is a conical structure. A plurality of rubber members 26 are fixedly provided at intervals on both sides of the first guide plate 24, and one end of each rubber member 26 contacts the inner wall of the mixing chamber 23. A stepper motor 11 is installed at one end of the outer side of the crystallizer body 10, and the output end of the stepper motor 11 is fixedly connected to one end of the rotating shaft 19. An inlet valve 15 is provided at one end of the water bath 18, and a water outlet valve 16 is provided at the other end of the water bath 18. Two support frames 12 are fixedly provided at the lower sides of both ends of the crystallizer body 10.

[0036] A crystallization process for imidazole processing comprises the following steps: S1: Prepare a saturated solution. According to the dissolved phase equilibrium experimental data, prepare a saturated imidazole solution in the crystallizer; S2: Temperature control, using a constant temperature water bath to control the temperature of the crystallizer; S3: dripping the solvent, making the temperature of the solvent consistent with the temperature of the saturated solution, and dripping the solvent into the crystallizer at a certain rate by using a stirring component; S4: stirring and growing crystals, stirring is started while dripping the solvent, and when crystals are precipitated, the dripping of the solvent is stopped, a certain amount of seed crystals is added, and the temperature and stirring rate are kept unchanged to grow crystals; S5: post-treatment, aging, filtering, drying and other treatments are performed on the crystals to obtain imidazole crystal products.

[0037] Specific use of the present invention: S1: Prepare a saturated solution. The staff prepares a saturated imidazole solution in the crystallizer body 10 according to the dissolved phase equilibrium experimental data.

[0038] S2: Temperature control, the staff connects the water inlet valve 15 with the external water tank, and the water outlet valve 16 with the external water tank, and the water in the water tank is heated and enters the water bath 18 through the water inlet valve 15, and the warm water in the water bath 18 returns to the external water tank through the water outlet valve 16. Thus, the warm water in the water bath 18 is kept at a constant temperature by controlling the temperature of the warm water in the external water tank, so that the constant temperature water in the water bath 18 can be used to control the temperature of the solution inside the crystallizer body 10.

[0039] S3: Solvent dripping and stirring, first, make the solvent temperature in the external solvent box consistent with the saturated solution temperature, and connect the external solvent box to the two feed valves 17 respectively. The control system controls the stepper motor 11 to start, and the stepper motor 11 starts to drive the rotating shaft 19 to rotate, and the rotation of the rotating shaft 19 drives the first slider 54 to rotate. The first slider 54 slides axially on the inner wall of the first sleeve 53, so that the first slider 54 has a spline effect, so that the rotation of the rotating shaft 19 drives the first sleeve 53 to rotate through the first slider 54. The rotation of the first sleeve 53 drives the second slider 56 to rotate, so that the second slider 56 spirally slides in the spiral chute 57. The spiral chute 57 is connected to each other at the head and tail, so that the second slider 56 moves back and forth in the spiral chute 57, and the second slider 56 moves back and forth to drive the first sleeve 53 to move back and forth, so that the first sleeve 53 rotates and moves back and forth.

[0040] Secondly, the first sleeve 53 rotates and moves back and forth to drive the piston plate 21 to rotate and move back and forth. When the piston plate 21 moves toward the mixing chamber 23, the piston plate 21 moves to draw the solvent in the external solvent box into the hydraulic chamber 22 through the feed valve 17.

[0041] When the piston plate 21 moves toward the hydraulic chamber 22, the piston plate 21 moves to allow a portion of the solvent in the hydraulic chamber 22 to enter the mixing chamber 23 through the first one-way valve 51, and another portion of the solvent in the hydraulic chamber 22 enters the first spreading plate 33 through the second one-way valve 52 and the circular tube 25. At the same time, the piston plate 21 moves to suck the imidazole saturated solution in the crystallizer body 10 into the mixing chamber 23 through the opening 29, so that the imidazole saturated solution and the solvent are preliminarily mixed in the mixing chamber 23. The rotation of the piston plate 21 drives the rotation of the first guide plates 24, and the rotation of the first guide plates 24 mixes the imidazole saturated solution and the solvent in the mixing chamber 23, promoting full contact between the imidazole saturated solution and the solvent. Among them, the rotation of the first guide plates 24 drives the circular plate 28 to rotate, and the rotation of the circular plate 28 drives the annular plate 32 to slide in an annular manner in the cylinder 20.

[0042] At the same time, the piston plate 21 moves toward the hydraulic chamber 22, and the movement of the piston plate 21 drives the circular tube 25 and the first spreading plate 33 to move, and the circular tube 25 and the first spreading plate 33 are fixed to the outer wall of the rotating shaft 19 through the L-shaped member 35. The first slide plate 34 is resisted by the L-shaped member 35, and the first spreading plate 33 moves to cooperate with the first slide plate 34 and fixes with the plurality of second spreading plates 39, so that the plurality of second spreading plates 39 extend from the first spreading plate 33, so that the plurality of through holes 40 on the second spreading plate 39 are all located outside the first spreading plate 33. The solvent in the first spreading plate 33 enters the plurality of second spreading plates 39 through the interior of the first slide plate 34, and the solvent in the second spreading plate 39 is sprayed into the middle of the interior of the crystallizer body 10 through the plurality of through holes 40. The rotation of the piston plate 21 drives the plurality of circular tubes 25 to rotate, and the rotation of the circular tubes 25 drives the first spreading plate 33 to rotate. The rotation of the rotating shaft 19 drives the L-shaped member 35 to rotate, so that the L-shaped member 35 and the first spreading plate 33 rotate synchronously, so that the first slide plate 34 and the plurality of second spreading plates 39 rotate, so that the solvent is diffusely sprayed through the plurality of through holes 40, and the contact area between the saturated imidazole solution and the solvent is increased, which is beneficial to promote the efficiency of imidazole crystallization, so that the solvent is dripped into the crystallizer body 10 at a certain rate by the spreading assembly. Among them, the frequency of the piston plate 21 moving back and forth in the cylinder 20 is controlled by controlling the speed of the rotating shaft 19, so that the solvent in the external solvent box is controlled by the frequency of the piston plate 21 moving back and forth in the cylinder 20 to be drawn into the hydraulic chamber 22 through the feed valve 17, so that the spreading assembly stirs the solution in the crystallizer body 10 at an appropriate speed and drips the solvent into the crystallizer body 10 at a certain rate, so as to avoid the phenomenon of poor crystal morphology.

[0043] When the piston plate 21 moves toward the mixing chamber 23 again, the piston plate 21 moves to draw the solvent in the external solvent box into the hydraulic chamber 22 through the feed valve 17. The movement of the piston plate 21 drives the first guide plates 24 to move, and the ends of the two baffles 30 that are close to each other are respectively in sliding contact with the inclined surfaces on both sides of one end of the first guide plate 24. The movement of the first guide plate 24 guides and pushes the two baffles 30, so that the two baffles 30 are separated from each other, so as to increase the liquid flow rate of the through port 29, so that the imidazole saturated solution and the solvent that are preliminarily mixed in the mixing chamber 23 are sprayed into the crystallizer body 10 through the plurality of through ports 29, so that the imidazole saturated solution and the solvent are further fully contacted, and the crystals are prevented from being blocked on the through ports 29. At the same time, the piston plate 21 rotates and moves, driving the first guide plates 24 to rotate and move. The first guide plates 24 rotate and move, driving the rubber parts 26 to rotate and move. The crystals adsorbed on the inner wall of the mixing chamber 23 are beaten and cleaned by the rotation and movement of the rubber parts 26. The inner wall of the ring 27 has a conical structure, so that the crystals in the mixing chamber 23 can be discharged into the crystallizer body 10 along the inner wall of the ring 27 through the opening 29.

[0044] At the same time, the piston plate 21 moves toward the mixing chamber 23, and the movement of the piston plate 21 drives the plurality of round tubes 25 and the first spreading plate 33 to move, and one end of the L-shaped member 35 is fixedly connected to the outer wall of the rotating shaft 19, so that the first slide plate 34 and the plurality of second spreading plates 39 are fixedly matched with the movement of the first spreading plate 33, so that the plurality of second spreading plates 39 move back into the first spreading plate 33. The movement of the first spreading plate 33 drives the plurality of second guide plates 48 to move, and the two sides of one end of the second guide plate 48 are respectively in sliding contact with the inclined surfaces of one end of the two second slide plates 41, and one end of the second guide plate 48 passes through the interior of the first slide plate 34 and enters the second spreading plate 39. The movement of the second guide plate 48 guides and pushes the two second slide plates 41, so that the two second slide plates 41 move away from each other. The two second slide plates 41 move away from each other and drive the plurality of pairs of cleaning blocks 43 to move away from each other, and the plurality of pairs of cleaning blocks 43 move away from each other and enter the plurality of pairs of through holes 40, so that the crystals blocked in the through holes 40 are pushed out to avoid the blockage of the through holes 40.

[0045] At the same time, the two second slide plates 41 move away from each other to squeeze and compress the pairs of hollow elastic members 42 respectively, so that the solution in the hollow elastic members 42 is sprayed into the through holes 40 through the connecting channels 45, which is conducive to clearing the through holes 40 with the high-pressure solution.

[0046] Next, the first spreading plate 33 moves to drive the second guide plates 48 to move, and the first protrusion 47 and the second protrusion 49 are in sliding contact, so that under the guidance of the first protrusion 47 and the second protrusion 49, the two second slide plates 41 are slightly away from each other. The two second slide plates 41 are slightly away from each other and squeezed by the several pairs of hollow elastic members 42 to generate elastic force. After the first protrusion 47 and the second protrusion 49 fall off and contact, under the elastic force of the several pairs of hollow elastic members 42, the two second slide plates 41 can be slightly close to each other. So that under the guidance of the first protrusion 47 and the second protrusion 49 and the elastic force of the several pairs of hollow elastic members 42, the two second slide plates 41 can be alternately close to each other and away from each other in a small range, so that the cleaning block 43 can move back and forth in a small range in the through hole 40, and further dredge the crystals blocked in the through hole 40, so that the dissolving agent is dripped into the crystallizer body 10 at a certain rate by using the spreading assembly.

[0047] S4: growing crystals. When crystals are precipitated, the dripping of the solvent is stopped, the control system controls the feed valve 17 to close, and the pressure relief valve 36 to open, so that the piston plate 21 can move back and forth normally in the cylinder 20. The staff adds a certain amount of seed crystals into the crystallizer body 10 through the feed pipe 13, and continues to grow crystals while keeping the temperature and stirring rate unchanged.

[0048] S5: post-treatment, aging, filtering, drying and other treatments are performed on the crystals to obtain imidazole crystal products.

[0049] The present invention provides a crystallization treatment device for imidazole processing. Through the arrangement of a piston plate 21, a first guide plate 24, and a through port 29, the piston plate 21 moves through the through port 29 to suck the imidazole saturated solution in the crystallizer body 10 into the mixing chamber 23, so that the imidazole saturated solution and the solvent are preliminarily mixed in the mixing chamber 23; and the rotation of the piston plate 21 drives the rotation of the first guide plates 24, and the rotation of the first guide plates 24 mixes the imidazole saturated solution and the solvent in the mixing chamber 23, thereby promoting full contact between the imidazole saturated solution and the solvent. Through the arrangement of the baffle 30 and the spring 31, the movement of the piston plate 21 drives the movement of the plurality of first guide plates 24, and the ends of the two baffles 30 that are close to each other are respectively in sliding contact with the inclined surfaces on both sides of one end of the first guide plate 24. The movement of the first guide plate 24 guides and pushes the two baffles 30, so that the two baffles 30 are moved away from each other, so as to increase the liquid flow rate of the port 29, so that the saturated imidazole solution and the solvent that are preliminarily mixed in the mixing chamber 23 are sprayed into the crystallizer body 10 through the plurality of ports 29, so that the saturated imidazole solution and the solvent are further fully contacted, and the crystals are prevented from being blocked on the port 29.

[0050] The crystallization treatment device for imidazole processing of the present invention controls the frequency of the piston plate 21 moving back and forth in the cylinder 20 by controlling the rotation speed of the rotating shaft 19, so that the solvent in the external solvent box is controlled by the frequency of the piston plate 21 moving back and forth in the cylinder 20 to be drawn into the hydraulic chamber 22 through the feed valve 17, so that the spreading component can stir the solution in the crystallizer body 10 at an appropriate speed and drip the solvent into the crystallizer body 10 at a certain rate, thereby avoiding the phenomenon of poor crystal morphology.

[0051] The present invention relates to a crystallization treatment device for imidazole processing. Through the arrangement of the circular tube 25, the L-shaped member 35, the first slide plate 34, the second spreading plate 39, and the through hole 40, the piston plate 21 moves to drive the circular tube 25 and the first spreading plate 33 to move. The circular tube 25 and the first spreading plate 33 are fixed to the outer wall of the rotating shaft 19 through the L-shaped member 35. The first slide plate 34 is resisted by the L-shaped member 35. The first spreading plate 33 moves to cooperate with the first slide plate 34 and the second spreading plates 39 to be fixed, so that the second spreading plates 39 extend from the first spreading plate 33, so that the through holes 40 on the second spreading plates 39 are all located outside the first spreading plate 33; the solvent in the first spreading plate 33 enters the plurality of second spreading plates 39 through the interior of the first slide plate 34. The second spreading plate 39 is dry, and the solvent in the second spreading plate 39 is sprayed into the middle of the interior of the crystallizer body 10 through the plurality of through holes 40; and the rotation of the piston plate 21 drives the plurality of round tubes 25 to rotate, and the rotation of the round tubes 25 drives the first spreading plate 33 to rotate; the rotation of the rotating shaft 19 drives the L-shaped part 35 to rotate, so that the L-shaped part 35 and the first spreading plate 33 rotate synchronously, so that the first slide plate 34 and the plurality of second spreading plates 39 rotate, so that the solvent is diffusely sprayed through the plurality of through holes 40, increasing the contact area between the saturated imidazole solution and the solvent, which is beneficial to promoting the efficiency of imidazole crystallization, so that the solvent can be dripped into the crystallizer body 10 at a certain rate using the spreading component.

[0052] The present invention provides a crystallization treatment device for imidazole processing. Through the arrangement of the second slide plate 41, the cleaning block 43, and the second guide plate 48, the first spreading plate 33 moves to drive the plurality of second guide plates 48 to move. The two sides of one end of the second guide plate 48 respectively make sliding contact with the inclined surfaces of one end of the two second slide plates 41. One end of the second guide plate 48 passes through the interior of the first slide plate 34 and enters the second spreading plate 39. The movement of the second guide plate 48 guides and pushes the two second slide plates 41, so that the two second slide plates 41 move away from each other. The two second slide plates 41 move away from each other, driving the plurality of pairs of cleaning blocks 43 to move away from each other. The plurality of pairs of cleaning blocks 43 move away from each other and respectively enter the plurality of pairs of through holes 40, so that the crystals blocked in the through holes 40 are pushed out to avoid blockage of the through holes 40. Then, by setting the hollow elastic member 42 and the connecting channel 45, the two second slide plates 41 move away from each other to squeeze and compress the several pairs of hollow elastic members 42, so that the solution in the hollow elastic member 42 is ejected into the through hole 40 through the connecting channel 45, which is conducive to the high-pressure solution to dredge the through hole 40. Finally, by setting the first protrusion 47 and the second protrusion 49, under the guidance of the first protrusion 47 and the second protrusion 49 and the elastic force of the several pairs of hollow elastic members 42, the two second slide plates 41 can be alternately moved closer to each other and farther away from each other in a small range, so that the cleaning block 43 can move back and forth in a small range in the through hole 40, and further dredge the crystals blocked in the through hole 40, so that the dissolving agent is dripped into the crystallizer body 10 at a certain rate by using the spreading assembly.

[0053] The embodiments of the present invention are given for the purpose of illustration and description, and are not intended to be exhaustive or to limit the invention to the disclosed forms. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments are selected and described in order to better illustrate the principles and practical applications of the present invention and to enable those of ordinary skill in the art to understand the present invention and thereby design various embodiments with various modifications suitable for specific uses.

Claims

1. A crystallization treatment device for imidazole processing, characterized in that: The invention comprises a crystallizer body (10), wherein a water bath (18) is arranged in the inner wall of the crystallizer body (10), a feed pipe (13) is arranged on the upper side of the crystallizer body (10), a discharge pipe (14) is arranged on the lower side of the crystallizer body (10), and two spreading assemblies are arranged at both ends of the interior of the crystallizer body (10); The spreading assembly comprises a cylinder (20), wherein the cylinder (20) is fixed to one end of the interior of the crystallizer body (10), a piston plate (21) is slidably provided inside the cylinder (20), a hydraulic chamber (22) and a mixing chamber (23) are separated inside the cylinder (20) by the piston plate (21), a plurality of first guide plates (24) are fixedly provided on one side of the piston plate (21) close to the mixing chamber (23), a circular tube (25) is fixedly provided in the middle of each first guide plate (24), one end of the circular tube (25) extends to the outside of the cylinder (20), a first spreading plate (33) is fixedly provided at one end of the circular tube (25), a first sliding plate (34) is slidably provided inside the first spreading plate (33), and the first sliding plate (34) is fixedly provided inside the first spreading plate (33). A plurality of second spreading plates (39) are fixedly provided at intervals on one side of a slide plate (34), and a plurality of through holes (40) are provided at intervals on both sides of each second spreading plate (39). One end of each second spreading plate (39) extends to the outside of the first spreading plate (33), and two second slide plates (41) are symmetrically provided in the middle of the interior of each second spreading plate (39). A plurality of cleaning blocks (43) are fixedly provided at intervals on the sides of the two second slide plates (41) that are away from each other, and two pairs of hollow elastic members (42) are connected to each other between the sides of each pair of second slide plates (41) that are away from each other and the two sides of the interior of each second spreading plate (39), and a connecting channel (45) is provided between the interior of each hollow elastic member (42) and the through hole (40).

2. A crystallization treatment device for imidazole processing according to claim 1, characterized in that: A plurality of second guide plates (48) are fixedly provided on one side of the first spreading plate (33) away from the second spreading plate (39); both sides of one end of each second guide plate (48) are in sliding contact with the inclined surface of one end of each pair of second slide plates (41); two grooves (46) are provided in the middle of one side of each pair of second slide plates (41) close to each other; a plurality of first protrusions (47) are fixedly provided at intervals in each of the grooves (46); a plurality of second protrusions (49) are fixedly provided at intervals on both sides of each second guide plate (48); and each of the first protrusions (47) is in sliding contact with each of the second protrusions (49).

3. A crystallization treatment device for imidazole processing according to claim 1, characterized in that: A rotating shaft (19) is rotatably provided inside the crystallizer body (10), and a plurality of L-shaped parts (35) are provided in a circumferential array on the outer walls at both ends of the rotating shaft (19), one end of each of the L-shaped parts (35) is fixedly connected to the outer wall of the rotating shaft (19), the other end of each of the L-shaped parts (35) is fixedly connected to the first slide plate (34), and the other end of each of the L-shaped parts (35) is in sliding contact with the first spreading plate (33).

4. A crystallization treatment device for imidazole processing according to claim 3, characterized in that: Two first sleeves (53) are sleeved on the outer walls at both ends of the rotating shaft (19), and the inner wall of each of the first sleeves (53) is in sliding contact with the outer wall of the rotating shaft (19). A first slider (54) is fixedly provided on one side of the outer wall at both ends of the rotating shaft (19), and the outer portion of each of the first sliders (54) is in axial sliding contact with the inner wall of the first sleeve (53).

5. A crystallization treatment device for imidazole processing according to claim 4, characterized in that: A second sleeve (55) is fixedly provided on one side of each of the cylinders (20), the inner wall of the second sleeve (55) is in sliding contact with the outer wall of the first sleeve (53), a second slider (56) is fixedly provided on one side of the outer wall of the first sleeve (53), the inner wall of the second sleeve (55) is provided with a spiral groove (57) which is interconnected at the head and tail, the second slider (56) spirally slides in the spiral groove (57), and the outer wall of one end of the first sleeve (53) is fixedly connected to the piston plate (21).

6. The crystallization treatment device for imidazole processing according to claim 1, characterized in that: The hydraulic chamber (22) is connected to the outside of the crystallizer body (10) and is provided with a feed valve (17). The piston plate (21) is provided with a first one-way valve (51). The hydraulic chamber (22) is communicated with the mixing chamber (23) through the first one-way valve (51). A second one-way valve (52) is provided on the inner wall of one end of the circular tube (25). The interior of the circular tube (25) is communicated with the hydraulic chamber (22) through the second one-way valve (52). The interior of the circular tube (25) is communicated with the interior of the first spreading plate (33). The interior of the first spreading plate (33) is communicated with the interior of the first slide plate (34). The interior of the first slide plate (34) is communicated with the interior of the second spreading plate (39). A pressure relief valve (36) is provided on one side of the hydraulic chamber (22).

7. The crystallization treatment device for imidazole processing according to claim 3, characterized in that: A first arc-shaped scraper (37) is fixedly provided on one side of the outside of the first spreading plate (33), and a second arc-shaped scraper (38) is fixedly provided on the other side of the outside of the first spreading plate (33). The inner wall of the first arc-shaped scraper (37) is in sliding contact with the outer wall of the rotating shaft (19), and the outer wall of the second arc-shaped scraper (38) is in sliding contact with the inner wall of the crystallizer body (10).

8. The crystallization treatment device for imidazole processing according to claim 3, characterized in that: A circular plate (28) is rotatably provided on one side of the mixing chamber (23), a plurality of openings (29) are arranged in a circular array on the circular plate (28), two baffles (30) are slidably provided on both sides of each opening (29), one end of each pair of baffles (30) close to each other is in sliding contact with the inclined surfaces on both sides of one end of the first guide plate (24), and two springs (31) are mutually connected between one end of each pair of baffles (30) away from each other and the inside of the circular plate (28), and an annular plate (32) is fixedly provided on the outer wall of the circular plate (28), and the annular plate (32) slides in an annular manner in the inner wall of the cylinder (20).

9. A crystallization treatment device for imidazole processing according to claim 8, characterized in that: A circular ring (27) is fixedly provided on one side of the circular plate (28) close to the mixing chamber (23), and the inner wall of the circular ring (27) is of a conical structure. A plurality of rubber pieces (26) are fixedly provided at intervals on both sides of the first guide plate (24), and one end of each of the rubber pieces (26) contacts the inner wall of the mixing chamber (23). A stepper motor (11) is installed at one end of the exterior of the crystallizer body (10), and the output end of the stepper motor (11) is fixedly connected to one end of the rotating shaft (19). A water inlet valve (15) is provided at one end of the water bath (18), and a water outlet valve (16) is provided at the other end of the water bath (18). Two support frames (12) are fixedly provided at the lower sides of both ends of the crystallizer body (10).

10. A crystallization process for imidazole processing, comprising a crystallization device for imidazole processing according to any one of claims 1 to 9, characterized in that: The following steps are involved: S1: Prepare a saturated solution. According to the dissolved phase equilibrium experimental data, prepare a saturated imidazole solution in the crystallizer; S2: Temperature control, using a constant temperature water bath to control the temperature of the crystallizer; S3: dripping the solvent, making the temperature of the solvent consistent with the temperature of the saturated solution, and dripping the solvent into the crystallizer at a certain rate by using a stirring component; S4: stirring and growing crystals, stirring is started while dripping the solvent, and when crystals are precipitated, the dripping of the solvent is stopped, a certain amount of seed crystals is added, and the temperature and stirring rate are kept unchanged to grow crystals; S5: post-treatment, aging, filtering, drying and other treatments are performed on the crystals to obtain imidazole crystal products.

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