Ethyl acetoacetate purification device for preparing pyrazole raw material and use method of ethyl acetoacetate purification device

Abstract

The invention discloses an ethyl acetoacetate purification device for pyrazole raw material preparation and a use method thereof, and relates to the field of ethyl acetoacetate purification, the ethyl acetoacetate purification device comprises a loading cylinder, a filter cylinder and a dehydration cylinder, the filter cylinder and the dehydration cylinder are inserted above the loading cylinder, one side of the loading cylinder is provided with a positioning frame and a drying assembly in the positioning frame, the filter cylinder is communicated with the dehydration cylinder, and the dehydration cylinder is communicated with the loading cylinder. One side of the filter cartridge is fixedly connected with a pushing assembly, the pushing assembly is fixedly mounted on the upper surface of the loading cylinder in a horizontal state, and a limiting convex strip is fixedly mounted at the joint of the loading cylinder and the filter cartridge. The dehydration efficiency can be guaranteed, batch production can be carried out, the stirring assembly is arranged in the dehydration barrel, in the dehydration process, drying agents can be continuously stirred, the size of caking of the drying agents can be reduced so as to achieve the effect of improving the water absorption efficiency, and it is guaranteed that ethyl acetoacetate makes full contact with the drying agents.

Description

Technical Field

[0001] The invention relates to the technical field of ethyl acetoacetate purification, in particular to an ethyl acetoacetate purification device for preparing pyrazole raw materials and a use method thereof. Background Art

[0002] In organic synthesis, ethyl acetoacetate has an active methylene structure, which can react with hydrazine compounds to construct a pyrazole ring through a series of condensation, cyclization and other steps. The purification of ethyl acetoacetate is the process of removing impurities from ethyl acetoacetate containing impurities through a series of methods and operations to obtain high-purity ethyl acetoacetate.

[0003] For example, the "A high-purity difluoroacetoacetic acid ethyl purifying device and method" with publication number CN102989189A, the purification device mainly includes an intelligent temperature-controlled electric heating jacket, a three-necked flask, a distillation column, a distillation head, a circulating water multi-purpose vacuum pump, a low-temperature cooling circulation pump, a storage tank, a thermometer and other auxiliary equipment. Among them, the three-necked flask, the distillation column and the distillation tower are used as intermittent distillation towers, and the filling method is adopted, and glass spring random packing is selected. After purification, the crude product containing 75-85% of difluoroacetoacetic acid ethyl ester concentration by mass is obtained to obtain 90-99.1% of difluoroacetoacetic acid ethyl ester.

[0004] However, in the prior art, when sodium sulfate hydrate is used as a desiccant to dehydrate ethyl acetoacetate, the desiccant needs to be placed in the ethyl acetoacetate. However, after the moisture absorbed by the desiccant reaches saturation, effective dehydration cannot continue, and during this process, the desiccant gradually agglomerates. Conventional devices lack subsequent treatment methods for the agglomerated desiccant, resulting in low desiccant utilization efficiency, causing the desiccant to remain in the ethyl acetoacetate for a long time. The contact area between the agglomerated sodium sulfate hydrate and the ethyl acetoacetate is reduced, reducing its absorption efficiency of the remaining moisture. If the agglomeration is severe, part of the ethyl acetoacetate will be wrapped inside the agglomerate and unable to fully contact the desiccant, resulting in incomplete drying. Summary of the Invention

[0005] The object of the present invention is to provide an apparatus for purifying ethyl acetoacetate for preparing a pyrazole raw material and a method for using the same, so as to solve the problem that the conventional apparatus proposed in the above-mentioned background art lacks subsequent processing means for agglomerated desiccant, resulting in low utilization efficiency of the desiccant, causing the desiccant to be retained in ethyl acetoacetate for a long time, reducing the contact area between agglomerated sodium sulfate hydrate and ethyl acetoacetate, and reducing the efficiency of the desiccant in absorbing residual moisture.

[0006] To achieve the above-mentioned object, the present invention provides the following technical solution: a device for purifying ethyl acetoacetate for preparing pyrazole raw materials, which is arranged in an ethyl acetoacetate purification production line for supporting use. The ethyl acetoacetate purification production line consists of processes such as pretreatment, water washing, drying and distillation, and includes a charging cylinder and a filter cylinder and a dehydration cylinder inserted above the charging cylinder. A positioning frame and a drying component inside the filter cylinder are provided on one side of the charging cylinder. The filter cylinder is connected to the dehydration cylinder. A pushing component is fixedly connected to one side of the filter cylinder. The pushing component is fixedly mounted on the upper surface of the charging cylinder in a horizontal state. A limiting convex strip is fixedly mounted at the intersection of the charging cylinder and the filter cylinder. The filter cylinder is used to filter agglomerated desiccant. A stirring component is vertically arranged inside the dehydration cylinder. The dehydration cylinder is used to initially store ethyl acetoacetate. The stirring component is used to stir the desiccant in the ethyl acetoacetate in the dehydration cylinder. The pushing component is used to push the filter cylinder and pour the residue therein into the drying component. The drying component dries the agglomerated desiccant and puts it back into the dehydration cylinder for secondary use. A discharge pipe is fixedly connected to one side of the dehydration cylinder.

[0007] Preferably, the stirring assembly includes a rotating rod, a connecting plate and a cylindrical block, the cylindrical block is rotatably installed at both ends of the connecting plate, a limiting ring is fixedly installed at the intersection of the cylindrical block and the connecting plate, the connecting plate is fixedly installed at both ends of the rotating rod in a horizontal state, the axis of the rotating rod coincides with the axis of the dehydration cylinder, and a stirring support rod is fixedly installed at the bottom of the cylindrical block.

[0008] Preferably, a turntable is rotatably mounted on the upper surface of the connecting plate, connecting rods are fixedly mounted in a circular arrangement on the edge of the turntable, a main gear is rotatably mounted on the outer wall of the rotating rod, and a driven gear is fixedly mounted on the top of the cylindrical block, and both the main gear and the driven gear are engaged with the turntable through the provided connecting rods.

[0009] Preferably, a positioning plate is fixedly installed on the top of the dehydration cylinder, the main gear is fixedly installed on the lower surface of the positioning plate, a reduction motor is fixedly installed on one side of the positioning plate, the output end of the reduction motor is fixedly connected to a belt transmission assembly, another pulley in the belt transmission assembly is fixedly connected to one end of the rotating rod, and a protective ring is fixedly installed at the junction of the dehydration cylinder and the filter cylinder.

[0010] Preferably, a widening plate is fixedly installed on the outer wall of the dehydration cylinder, the lower surface of the widening plate is rotatably connected to an electric cylinder, the upper surface of the loading cylinder is fixedly installed with a limit seat, the bottom of the electric cylinder is rotatably installed inside the limit seat, the bottom of the filter cylinder is fixedly installed with a filter screen, a blocking plate is clamped at the junction of the loading cylinder and the filter screen, the bottom of the blocking plate is fixedly connected to an electric telescopic rod, and a vertical rod is fixedly installed on the inner wall of the loading cylinder.

[0011] Preferably, the pushing assembly includes a positioning tube and a movable block, the positioning tube is fixedly mounted on the upper surface of the loading barrel, one end of the movable block is rotatably connected to a push rod, a micro motor is fixedly mounted on the top of the movable block, a connecting gear is fixedly mounted on the output end of the micro motor, a tooth plate is fixedly mounted on the top of the positioning tube, and the tooth plate is meshingly connected to the connecting gear.

[0012] Preferably, a cavity is provided inside the positioning tube, the push rod is located inside the cavity, an extension rod is fixedly installed on the outer wall of the push rod, one side of the cavity is connected to a strip-shaped notch, the movable block is slidably connected to the inside of the strip-shaped notch, a straight groove is provided on the inner wall of the cavity, one end of the straight groove is fixedly connected to a curved groove, and the curved groove rotates ninety degrees along the inner wall of the cavity.

[0013] Preferably, the drying component includes a movable frame, which is sleeved on the outer wall of the positioning frame. A servo motor is movably installed on one side of the movable frame. The output end of the servo motor is fixedly connected to a large gear. Bumps are fixedly installed in a linear array on the outer wall of the positioning frame. The large gear and the bumps are meshed together. An annular groove is provided at the junction of the positioning frame and the output end of the servo motor.

[0014] Preferably, one side of the movable frame is rotatably connected to a stirring base through a torsion spring, an electric heating box is fixedly installed on the top of the stirring base, a rolling rod is rotatably installed inside the electric heating box, the rolling rod is fixedly connected to the output end of the stirring base, a limit block is fixedly installed on the outer casing of the servo motor, the limit block is slidably connected to the inside of the movable frame, and a blocking rod is fixedly installed at a corner of the top of the positioning frame.

[0015] A method for using an ethyl acetoacetate purification device for preparing a pyrazole raw material comprises the following steps:

[0016] S1. The filter cylinder is docked on the top of the charging cylinder, and the filter screen is blocked with a baffle. Then, the ethyl acetoacetate to be purified is poured into the dehydration cylinder. The ethyl acetoacetate will be concentrated in the filter cylinder and the dehydration cylinder. Then, the desiccant is added and the stirring component is started;

[0017] S2. The reduction motor drives the rotating rod through the belt drive assembly. During the rotation of the rotating rod, the two cylindrical blocks are simultaneously driven through the connecting plate, so that the stirring rod at the bottom of the cylindrical block stirs the desiccant in the ethyl acetoacetate. As the cylindrical block rotates around the rotating rod, the driven gear at its top is pushed by the connecting rod at the edge of the turntable, causing the cylindrical block itself to rotate synchronously;

[0018] S3. After the desiccant absorbs moisture, the stirring assembly stops, and the electric telescopic rod moves the blocking plate downward, allowing the ethyl acetoacetate to pass through the filter and enter the charging barrel. The agglomerated desiccant will be blocked by the filter. After the ethyl acetoacetate has completely flowed into the charging barrel, the electric cylinder lifts the dehydration barrel through the widening plate, separating the dehydration barrel from the filter barrel. At this time, the pushing assembly is started again;

[0019] S4. The micro motor drives the connecting gear and uses the reaction force of the tooth plate to drive the movable block to move along the direction of the strip notch. During this process, the movable block pushes the filter cartridge through the push rod. The extension rod on the push rod moves along the direction of the straight groove until it enters the curved groove. Under the obstruction of the curved groove, the push rod is forced to rotate, pouring the agglomerated desiccant in the filter cartridge into the electric heating box.

[0020] S5. The electric heating box heats the desiccant to evaporate the moisture in it, and the stirring base drives the crushing rod to crush the agglomerated desiccant into powder. Then the servo motor drives the large gear and uses the reaction force of the protrusion to lift the movable frame, so that the entire stirring base and the electric heating box rise together. Under the obstruction of the blocking rod, the electric heating box will tilt, thereby pouring the desiccant back into the dehydration cylinder.

[0021] Compared with the prior art, the present invention has the following beneficial effects:

[0022] 1. In the present invention, a complete dehydration and purification device is formed by assembling a dehydration cylinder, a filter cylinder and a charging cylinder, which can ensure the efficiency of dehydration and can be mass-produced. A stirring component is provided in the dehydration cylinder. During the dehydration process, the desiccant can be continuously stirred to reduce the volume of its agglomerates to achieve the effect of improving the water absorption efficiency, ensuring that the ethyl acetoacetate is in full contact with the desiccant. After completing a single dehydration process, the used desiccant can be quickly cleaned out for the next dehydration process, thereby avoiding the situation where the desiccant affects the dehydration progress. The cleaned desiccant is poured into the drying component, dried, and finally put back into the dehydration process for secondary use. This method can greatly improve the utilization efficiency of the desiccant.

[0023] 2. In the present invention, the stirring assembly adopts a rotating rod to drive the cylindrical block, so that the stirring support rod can completely cover the dehydration cylinder to ensure that there is no stirring dead angle. In the process of the cylindrical block rotating around the rotating rod, the driven gear on its top is always engaged with the connecting rod on the edge of the turntable. Under the push of the connecting rod, the cylindrical block will also rotate itself in the process of rotating with the rotating rod as the center, thereby avoiding the problem of eddy currents in the dehydration cylinder causing the desiccant to concentrate in one piece.

[0024] 3. In the present invention, the push rod in the pushing assembly is used to push the filter cartridge, so that the filter cartridge moves to the edge of the loading cylinder. Then, under the action of the curved groove, the filter cartridge is driven to rotate, and the block desiccant therein is poured into the drying assembly. This process saves the step of manually salvaging the desiccant and can quickly restore the state of connection with the loading cylinder and the dehydration cylinder, greatly reducing the time for separating the desiccant. The separated desiccant will be heated by the electric heating box to evaporate the moisture therein, so that it can be reused, thereby improving the utilization rate of the desiccant and reducing the loss rate. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 This is a schematic diagram of the three-dimensional structure of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0026] Figure 2 This is a front view of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0027] Figure 3 This is a schematic diagram of the internal structure of a charging cylinder, a filtering cylinder and a dehydrating cylinder of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0028] Figure 4 This is a schematic diagram of the connection and structure of a dehydration cylinder and a stirring component of an ethyl acetoacetate purification device for preparing pyrazole raw materials of the present invention;

[0029] Figure 5 For the present invention Figure 4 A schematic diagram of the structure of part A;

[0030] Figure 6 This is a schematic diagram of the three-dimensional structure of a stirring assembly of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0031] Figure 7 This is a schematic diagram of the positions and structure of the charging barrel and positioning frame of an ethyl acetoacetate purification device for preparing pyrazole raw materials of the present invention;

[0032] Figure 8 This is a schematic diagram of the exploded structure of a pushing component of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0033] Figure 9 This is a schematic diagram of the internal structure of a positioning tube of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0034] Figure 10 This is a schematic diagram of the three-dimensional structure of a push rod in a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0035] Figure 11This is a top view of an apparatus for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0036] Figure 12 This is a schematic structural diagram of a positioning frame and drying assembly of an ethyl acetoacetate purification device for preparing pyrazole raw materials according to the present invention;

[0037] Figure 13 This is a schematic diagram of the pushing process of a pushing component of a device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to the present invention;

[0038] Figure 14 The present invention provides a schematic diagram of the movement process of a drying component of an ethyl acetoacetate purification device for preparing pyrazole raw materials.

[0039] Figure: 1, charging cylinder; 2, filter cylinder; 3, dehydration cylinder; 4, positioning frame; 5, pushing assembly; 6, stirring assembly; 7, drying assembly; 8, widening plate; 9, feeding pipe; 10, protection ring; 11, vertical rod; 12, electric telescopic rod; 13, electric cylinder; 14, filter screen; 15, limit seat; 16, limit rib; 17, blocking plate; 18, blocking rod; 51, positioning tube; 52, movable block; 53, tooth plate; 54, push rod; 55, strip notch; 56, cavity; 57, micro motor; 5 8. Straight groove; 59. Curved groove; 510. Extension rod; 61. Positioning plate; 62. Reducer motor; 63. Belt drive assembly; 64. Rotating rod; 65. Connecting plate; 66. Cylindrical block; 67. Stirring support rod; 68. Main gear; 69. Turntable; 610. Connecting rod; 611. Driven gear; 612. Limiting ring; 71. Movable frame; 72. Servo motor; 73. Limiting block; 74. Electric heating box; 75. Rolling rod; 76. Stirring base; 77. Annular groove; 78. Bump; 79. Large gear. DETAILED DESCRIPTION

[0040] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the implementation regulations described are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention.

[0041] Example 1: Reference Figure 1 、 Figure 2 、 Figure 3 、 Figure 13 and Figure 14As shown: A device for purifying ethyl acetoacetate for preparing pyrazole raw materials, which is arranged on an ethyl acetoacetate purification production line for supporting use. The ethyl acetoacetate purification production line consists of processes such as pretreatment, water washing, drying and distillation, including a charging cylinder 1 and a filter cylinder 2 and a dehydration cylinder 3 inserted thereon. A positioning frame 4 and a drying component 7 inside the charging cylinder 1 are provided on one side of the charging cylinder 1. The filter cylinder 2 is connected to the dehydration cylinder 3. A pushing component 5 is fixedly connected to one side of the filter cylinder 2. The pushing component 5 is fixedly mounted on the upper surface of the charging cylinder 1 in a horizontal state. A limiting convex strip 16 is fixedly mounted at the intersection of the charging cylinder 1 and the filter cylinder 2. The filter cylinder 2 is used to filter the agglomerated desiccant. The interior of the dehydration cylinder 3 is provided with a stirring component 6 in a vertical state. The dehydration cylinder 3 is used to initially store ethyl acetoacetate. The stirring component 6 is used to stir the ethyl acetoacetate in the dehydration cylinder 3. The desiccant in ethyl acetate, the pushing component 5 is used to push the filter cylinder 2 and pour the residue therein into the drying component 7. The drying component 7 uses the dried agglomerated desiccant and puts it back into the dehydration cylinder 3 for secondary utilization. One side of the dehydration cylinder 3 is fixedly connected with a discharge pipe 9, and a widening plate 8 is fixedly installed on the outer wall of the dehydration cylinder 3. The lower surface of the widening plate 8 is rotatably connected to the electric cylinder 13. The upper surface of the loading cylinder 1 is fixedly installed with a limit seat 15, and the bottom of the electric cylinder 13 is rotatably installed inside the limit seat 15. The bottom of the filter cylinder 2 is fixedly installed with a filter screen 14, and a blocking plate 17 is clamped at the junction of the loading cylinder 1 and the filter screen 14. The bottom of the blocking plate 17 is fixedly connected to an electric telescopic rod 12, and a vertical rod 11 is fixedly installed on the inner wall of the loading cylinder 1. A protective ring 10 is fixedly installed at the junction of the dehydration cylinder 3 and the filter cylinder 2.

[0042] In this embodiment, the dehydration cylinder 3 is inserted above the filter cylinder 2, and a protective ring 10 is provided at the intersection to ensure sealing and prevent leakage of ethyl acetoacetate. When in use, the filter screen 14 of the filter cylinder 2 is aligned with the blocking plate 17, and the position of the filter cylinder 2 is determined by the limiting ridge 16. At this time, the blocking plate 17 will prevent the ethyl acetoacetate in the filter cylinder 2 from flowing into the charging cylinder 1. Pour ethyl acetoacetate into the dehydration cylinder 3 and add a corresponding amount of anhydrous sodium sulfate desiccant. After anhydrous sodium sulfate contacts ethyl acetoacetate, it will quickly absorb the moisture in the ethyl acetoacetate and agglomerate. 10-20g of anhydrous sodium sulfate is used for every 100ml of ethyl acetoacetate.

[0043] After the desiccant comes into contact with the ethyl acetoacetate, the stirring assembly 6 stirs the ethyl acetoacetate to ensure full contact between the ethyl acetoacetate and the desiccant. After a period of stirring, the electric telescopic rod 12 moves the blocking plate 17 away from the filter screen 14, allowing the ethyl acetoacetate to flow into the charging barrel 1. At this time, the agglomerated desiccant is blocked by the filter screen 14 in the filter barrel 2. The position of the electric telescopic rod 12 is determined by the vertical rod 11.

[0044] Then the electric cylinder 13 pushes the widening plate 8 to take the dehydration cylinder 3 away from the filter cylinder 2. During this process, the electric cylinder 13 itself can rotate around the limit seat 15. After the dehydration cylinder 3 is separated from the filter cylinder 2, the pushing component 5 pushes the filter cylinder 2 to the edge of the loading cylinder 1. When the filter cylinder 2 is about to leave the loading cylinder 1, it will rotate and pour the block desiccant therein into the drying component 7. After evaporating the moisture in the desiccant, the drying component 7 will be ground into powder and will move upward along the positioning frame 4 to pour the desiccant back into the dehydration cylinder 3.

[0045] Example 2: According to Figure 3 、 Figure 4 、 Figure 5 and Figure 6 As shown, the stirring assembly 6 includes a rotating rod 64, a connecting plate 65 and a cylindrical block 66. The cylindrical block 66 is rotatably mounted on both ends of the connecting plate 65. A limit ring 612 is fixedly installed at the intersection of the cylindrical block 66 and the connecting plate 65. The connecting plate 65 is fixedly mounted on both ends of the rotating rod 64 in a horizontal state. The axis of the rotating rod 64 coincides with the axis of the dehydration cylinder 3. A stirring support rod 67 is fixedly mounted on the bottom of the cylindrical block 66. A turntable 69 is rotatably mounted on the upper surface of the connecting plate 65. The edge of the turntable 69 is fixedly mounted with connecting rods 610 in a circular arrangement. The rotating rod 6 4 is rotatably mounted on the outer wall thereof, a driven gear 611 is fixedly mounted on the top of the cylindrical block 66, and both the main gear 68 and the driven gear 611 are meshed and connected with the turntable 69 through a connecting rod 610. A positioning plate 61 is fixedly mounted on the top of the dehydration cylinder 3, and the main gear 68 is fixedly mounted on the lower surface of the positioning plate 61. A reduction motor 62 is fixedly mounted on one side of the positioning plate 61, and the output end of the reduction motor 62 is fixedly connected to a belt drive assembly 63, and another pulley in the belt drive assembly 63 is fixedly connected to one end of a rotating rod 64.

[0046] In this embodiment, the reduction motor 62 drives the rotating rod 64 through the belt transmission assembly 63. During the rotation of the rotating rod 64, the two cylindrical blocks 66 are simultaneously driven through the connecting plate 65. The stirring support rod 67 at the bottom of the cylindrical block 66 continuously stirs the ethyl acetoacetate in the dehydration cylinder 3 to ensure that the ethyl acetoacetate and the desiccant are in full contact. The reduction motor 62 is installed on the side of the positioning plate 61 and will not affect the feeding of the ethyl acetoacetate and the desiccant.

[0047] During the rotation of the cylindrical block 66 with the rotating rod 64 as the center, the turntable 69 will be pushed by the main gear 68, and the driven gear 611 at the top of the cylindrical block 66 will be pushed by the connecting rod 610 at the edge of the turntable 69, thereby driving the entire cylindrical block 66 to rotate. In this way, eddy currents are avoided in the dehydration cylinder 3, thereby preventing the desiccant from gathering together. The position of the cylindrical block 66 is determined by the limiting ring 612 to ensure the structural stability of the cylindrical block 66.

[0048] Example 3: According to Figure 7 、 Figure 8 、 Figure 9 and Figure 10 As shown, the pushing assembly 5 includes a positioning tube 51 and a movable block 52. The positioning tube 51 is fixedly mounted on the upper surface of the charging barrel 1. One end of the movable block 52 is rotatably connected to a push rod 54. A micro motor 57 is fixedly mounted on the top of the movable block 52. The output end of the micro motor 57 is fixedly mounted with a connecting gear. A tooth plate 53 is fixedly mounted on the top of the positioning tube 51. The tooth plate 53 is meshed with the connecting gear. A cavity 56 is provided inside the positioning tube 51. The push rod 54 is located inside the cavity 56. An extension rod 510 is fixedly mounted on the outer wall of the push rod 54. A strip notch 55 is connected to one side of the cavity 56. The movable block 52 is slidably connected to the inside of the strip notch 55. A straight groove 58 is provided on the inner wall of the cavity 56. One end of the straight groove 58 is fixedly connected to a curved groove 59. The curved groove 59 rotates ninety degrees along the inner wall of the cavity 56.

[0049] In this embodiment, the gear at the output end of the micro motor 57 is meshed with the toothed plate 53. When in use, the micro motor 57 drives the connecting gear. Under the reaction force of the toothed plate 53, the movable block 52 is driven to move along the direction of the positioning tube 51. The movable block 52 is located in the strip-shaped notch 55 to prevent the movable block 52 from shaking during movement. The push rod 54 is located in the cavity 56. When the movable block 52 moves, the push rod 54 pushes the filter cartridge 2 and pushes the filter cartridge 2 away from the loading barrel 1. During this process, the extension rod 510 on the push rod 54 moves in the linear groove 58.

[0050] When the filter cartridge 2 moves to the edge of the loading cylinder 1 , the extension rod 510 on the push rod 54 enters the curved groove 59 and, under the obstruction of the curved groove 59 , forces the push rod 54 to rotate, thereby driving the filter cartridge 2 . After the filter cartridge 2 rotates, the desiccant inside it will be poured into the drying assembly 7 .

[0051] Example 4: According to Figure 7 、 Figure 11 and Figure 12As shown, the drying component 7 includes a movable frame 71, which is sleeved on the outer wall of the positioning frame 4. A servo motor 72 is movably installed on one side of the movable frame 71, and the output end of the servo motor 72 is fixedly connected to a large gear 79. A protrusion 78 is fixedly installed in a linear array on the outer wall of the positioning frame 4, and the large gear 79 is meshed with the protrusion 78. An annular groove 77 is provided at the intersection of the positioning frame 4 and the output end of the servo motor 72. One side of the movable frame 71 is rotatably connected to a stirring base 76 through a torsion spring. An electric heating box 74 is fixedly installed on the top of the stirring base 76, and a rolling rod 75 is rotatably installed inside the electric heating box 74. The rolling rod 75 is fixedly connected to the output end of the stirring base 76. A limit block 73 is fixedly installed on the outer casing of the servo motor 72, and the limit block 73 is slidably connected to the inside of the movable frame 71. A blocking rod 18 is fixedly installed at a corner of the top of the positioning frame 4.

[0052] In this embodiment, the desiccant poured out by the filter cartridge 2 will fall into the electric heating box 74, which will continue to heat the desiccant to evaporate the water therein. The sodium sulfate hydrate will lose its crystal water during heating and turn back into anhydrous sodium sulfate, which can be used for drying again. During the heating process, the crushing rod 75 will be driven by the motor in the stirring base 76 to crush the block desiccant into powder.

[0053] After the desiccant is processed, the servo motor 72 drives the large gear 79. Under the action of the protrusion 78, the movable frame 71 moves up and down along the direction of the positioning frame 4. During the movement, the output end of the servo motor 72 moves in the annular groove 77 to ensure that the large gear 79 can always maintain an engagement state with the protrusion 78. In addition, during the movement of the servo motor 72, the limit block 73 moves in the movable frame 71 to ensure that the movable frame 71 does not affect the normal movement of the servo motor 72.

[0054] After the movable frame 71 moves to the top of the positioning frame 4, one side of the electric heating box 74 will contact the blocking rod 18. Under the obstruction of the blocking rod 18, the electric heating box 74 will rotate to an inclined state and pour the powdered desiccant inside it into the discharge pipe 9.

[0055] The method of use and working principle of this device are as follows: the filter cylinder 2 is docked on the top of the charging cylinder 1, the filter screen 14 is blocked with the blocking plate 17, and then the ethyl acetoacetate to be purified is poured into the dehydration cylinder 3. The ethyl acetoacetate will be concentrated in the filter cylinder 2 and the dehydration cylinder 3. Then, the desiccant is added and the stirring component 6 is started;

[0056] The reduction motor 62 drives the rotating rod 64 through the belt drive assembly 63. During the rotation of the rotating rod 64, the two cylindrical blocks 66 are simultaneously driven through the connecting plate 65, so that the stirring support rod 67 at the bottom of the cylindrical block 66 stirs the desiccant in the ethyl acetoacetate. As the cylindrical block 66 rotates around the rotating rod 64, the driven gear 611 at the top of the cylindrical block 66 is pushed by the connecting rod 610 at the edge of the turntable 69, causing the cylindrical block 66 to rotate synchronously.

[0057] After the desiccant absorbs moisture, the stirring assembly 6 is stopped, and the electric telescopic rod 12 moves the blocking plate 17 downward, allowing the ethyl acetoacetate to pass through the filter screen 14 and enter the charging barrel 1. The agglomerated desiccant will be blocked by the filter screen 14. After the ethyl acetoacetate has completely flowed into the charging barrel 1, the electric cylinder 13 lifts the dehydration barrel 3 via the widening plate 8, separating the dehydration barrel 3 from the filter barrel 2. At this time, the pushing assembly 5 is started again;

[0058] The micro motor 57 drives the connecting gear, and uses the reaction force of the tooth plate 53 to drive the movable block 52 to move along the direction of the strip-shaped notch 55. During this process, the movable block 52 pushes the filter cartridge 2 through the push rod 54. The extension rod 510 on the push rod 54 moves along the direction of the linear groove 58 until it enters the curved groove 59. Under the obstruction of the curved groove 59, the push rod 54 is forced to rotate, pouring the agglomerated desiccant in the filter cartridge 2 into the electric heating box 74.

[0059] The electric heating box 74 heats the desiccant to evaporate the moisture therein, and the stirring base 76 drives the crushing rod 75 to crush the agglomerated desiccant into powder. Then the servo motor 72 drives the large gear 79, and uses the reaction force of the protrusion 78 to lift the movable frame 71, so that the entire stirring base 76 and the electric heating box 74 rise together. Under the obstruction of the blocking rod 18, the electric heating box 74 will tilt, thereby pouring the desiccant back into the dehydration cylinder 3.

[0060] Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments, or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A ethyl acetoacetate purification device for preparing pyrazole raw materials, which is arranged on an ethyl acetoacetate purification production line for use in conjunction with the ethyl acetoacetate purification production line, which consists of processes such as pretreatment, washing, drying and distillation, and is characterized in that: The invention comprises a loading cylinder (1) and a filter cylinder (2) and a dehydration cylinder (3) inserted thereon. A positioning frame (4) and a drying assembly (7) therein are provided on one side of the loading cylinder (1). The filter cylinder (2) is connected to the dehydration cylinder (3). A pushing assembly (5) is fixedly connected to one side of the filter cylinder (2). The pushing assembly (5) is fixedly installed on the upper surface of the loading cylinder (1) in a horizontal state. A limiting convex strip (16) is fixedly installed at the intersection of the loading cylinder (1) and the filter cylinder (2). The filter cylinder (2) is used to filter agglomerated particles. Desiccant, wherein a stirring assembly (6) is provided in a vertical state inside the dehydration cylinder (3), the dehydration cylinder (3) is used for initially storing ethyl acetoacetate, the stirring assembly (6) is used for stirring the desiccant in the ethyl acetoacetate in the dehydration cylinder (3), the pushing assembly (5) is used for pushing out the filter cylinder (2) and pouring the residue therein into the drying assembly (7), the drying assembly (7) uses the dried agglomerated desiccant and puts it back into the dehydration cylinder (3) for secondary use, and a discharge pipe (9) is fixedly connected to one side of the dehydration cylinder (3).

2. The ethyl acetoacetate purification device for preparing pyrazole raw materials according to claim 1, wherein: The stirring assembly (6) comprises a rotating rod (64), a connecting plate (65) and a cylindrical block (66); the cylindrical block (66) is rotatably mounted on both ends of the connecting plate (65); a limiting ring (612) is fixedly mounted at the intersection of the cylindrical block (66) and the connecting plate (65); the connecting plate (65) is fixedly mounted on both ends of the rotating rod (64) in a horizontal state; the axis of the rotating rod (64) coincides with the axis of the dehydration cylinder (3); and a stirring support rod (67) is fixedly mounted at the bottom of the cylindrical block (66).

3. The ethyl acetoacetate purification device for preparing pyrazole raw materials according to claim 2, wherein: A turntable (69) is rotatably mounted on the upper surface of the connecting plate (65), and connecting rods (610) are fixedly mounted in a circumferential arrangement on the edge of the turntable (69). A main gear (68) is rotatably mounted on the outer wall of the rotating rod (64), and a driven gear (611) is fixedly mounted on the top of the cylindrical block (66). Both the main gear (68) and the driven gear (611) are meshed and connected with the turntable (69) through the provided connecting rods (610).

4. The ethyl acetoacetate purification device for preparing pyrazole raw materials according to claim 3, wherein: A positioning plate (61) is fixedly installed on the top of the dehydration cylinder (3), the main gear (68) is fixedly installed on the lower surface of the positioning plate (61), a reduction motor (62) is fixedly installed on one side of the positioning plate (61), the output end of the reduction motor (62) is fixedly connected to a belt transmission assembly (63), another pulley in the belt transmission assembly (63) is fixedly connected to one end of a rotating rod (64), and a protective ring (10) is fixedly installed at the intersection of the dehydration cylinder (3) and the filter cylinder (2).

5. The ethyl acetoacetate purification device for preparing pyrazole raw materials according to claim 4, characterized in that: A widening plate (8) is fixedly mounted on the outer wall of the dehydration cylinder (3), and the lower surface of the widening plate (8) is rotatably connected to an electric cylinder (13). A limiting seat (15) is fixedly mounted on the upper surface of the charging cylinder (1), and the bottom of the electric cylinder (13) is rotatably mounted inside the limiting seat (15). A filter screen (14) is fixedly mounted on the bottom of the filter cylinder (2). A blocking plate (17) is clamped at the junction of the charging cylinder (1) and the filter screen (14), and the bottom of the blocking plate (17) is fixedly connected to an electric telescopic rod (12). A vertical rod (11) is fixedly mounted on the inner wall of the charging cylinder (1).

6. The ethyl acetoacetate purification device for preparing pyrazole raw materials according to claim 5, characterized in that: The pushing assembly (5) comprises a positioning tube (51) and a movable block (52), wherein the positioning tube (51) is fixedly mounted on the upper surface of the charging barrel (1), one end of the movable block (52) is rotatably connected to a push rod (54), a micro motor (57) is fixedly mounted on the top of the movable block (52), an engaging gear is fixedly mounted on the output end of the micro motor (57), a tooth plate (53) is fixedly mounted on the top of the positioning tube (51), and the tooth plate (53) is meshedly connected to the engaging gear.

7. The device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to claim 6, wherein: A cavity (56) is provided inside the positioning tube (51), the push rod (54) is located inside the cavity (56), an extension rod (510) is fixedly installed on the outer wall of the push rod (54), one side of the cavity (56) is connected to a strip-shaped notch (55), the movable block (52) is slidably connected to the inside of the strip-shaped notch (55), a straight groove (58) is provided on the inner wall of the cavity (56), one end of the straight groove (58) is fixedly connected to a curved groove (59), and the curved groove (59) rotates ninety degrees along the inner wall of the cavity (56).

8. The device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to claim 7, wherein: The drying assembly (7) includes a movable frame (71), which is sleeved on the outer wall of the positioning frame (4). A servo motor (72) is movably installed on one side of the movable frame (71), and the output end of the servo motor (72) is fixedly connected to a large gear (79). The outer wall of the positioning frame (4) is fixedly installed with protrusions (78) in a linear array, and the large gear (79) and the protrusions (78) are meshed and connected. An annular groove (77) is provided at the intersection of the positioning frame (4) and the output end of the servo motor (72).

9. The device for purifying ethyl acetoacetate for preparing pyrazole raw materials according to claim 8, wherein: One side of the movable frame (71) is rotatably connected to a stirring base (76) via a torsion spring, an electric heating box (74) is fixedly installed on the top of the stirring base (76), a rolling rod (75) is rotatably installed inside the electric heating box (74), and the rolling rod (75) is fixedly connected to the output end of the stirring base (76), a limit block (73) is fixedly installed on the housing of the servo motor (72), and the limit block (73) is slidably connected to the inside of the movable frame (71), and a blocking rod (18) is fixedly installed at a corner of the top of the positioning frame (4).

10. A method for using a device for purifying ethyl acetoacetate for preparing a pyrazole raw material, comprising using the device for purifying ethyl acetoacetate for preparing a pyrazole raw material according to any one of claims 1 to 9, wherein: The following steps are involved: S1, the filter cylinder (2) is docked on the top of the charging cylinder (1), the filter screen (14) is blocked with a blocking plate (17), and then the ethyl acetoacetate to be purified is poured into the dehydration cylinder (3). The ethyl acetoacetate will be concentrated in the filter cylinder (2) and the dehydration cylinder (3), and then the desiccant is added and the stirring assembly (6) is started; S2, the reduction motor (62) drives the rotating rod (64) through the belt transmission assembly (63), and during the rotation of the rotating rod (64), the two cylindrical blocks (66) are simultaneously driven through the connecting plate (65), so that the stirring support rod (67) at the bottom of the cylindrical block (66) stirs the desiccant in the ethyl acetoacetate. During the rotation of the cylindrical block (66) around the rotating rod (64), the driven gear (611) located at the top of the cylindrical block (66) is pushed by the connecting rod (610) at the edge of the turntable (69), prompting the cylindrical block (66) itself to rotate synchronously; S3. After the desiccant absorbs moisture, the stirring assembly (6) is stopped, and the electric telescopic rod (12) moves the blocking plate (17) downward, so that the ethyl acetoacetate passes through the filter (14) and enters the charging barrel (1). The agglomerated desiccant will be blocked by the filter (14). After the ethyl acetoacetate completely flows into the charging barrel (1), the electric cylinder (13) lifts the dehydration barrel (3) through the widening plate (8), and separates the dehydration barrel (3) from the filter barrel (2). At this time, the pushing assembly (5) is started again; S4, the micro motor (57) drives the connecting gear, and uses the reaction force of the tooth plate (53) to drive the movable block (52) to move along the direction of the strip notch (55). During this process, the movable block (52) pushes the filter cartridge (2) through the push rod (54), and the extension rod (510) on the push rod (54) moves along the direction of the linear groove (58) until it enters the curved groove (59). Under the obstruction of the curved groove (59), the push rod (54) is forced to rotate, and the desiccant agglomerated in the filter cartridge (2) is poured into the electric heating box (74); S5, the electric heating box (74) heats the desiccant to evaporate the moisture therein, and the stirring base (76) drives the crushing rod (75) to crush the agglomerated desiccant into powder. Then the servo motor (72) drives the large gear (79), and uses the reaction force of the protrusion (78) to lift the movable frame (71), so that the entire stirring base (76) and the electric heating box (74) rise together. Under the obstruction of the blocking rod (18), the electric heating box (74) will tilt, thereby pouring the desiccant back into the dehydration cylinder (3).

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