Preparation method and device of 4-trifluoromethyl nicotinic acid

Abstract

The invention provides a preparation method and device of 4-trifluoromethyl nicotinic acid, and relates to the technical field of preparation of 4-trifluoromethyl nicotinic acid.The device comprises a mixing tank, a filter box is arranged on one side of the mixing tank, a conveying pipe is fixed in the filter box, and in the washing process, the conveying pipe is communicated with the mixing tank; a third motor at the top of a screw rod drives a driving bevel gear to rotate to be meshed with four driven bevel gears, through insertion connection of a shaft rod and a rotating rod, a third gear rotates to be meshed with a second gear ring, a whole shaft disc drives a cylindrical filter screen to rotate, and the cleaning effect can be improved under the condition that internal 4-trifluoromethyl nicotinic acid particles continuously shake; when the collecting assembly is close to the drying assembly, a third electric push rod pushes a circular ring and a vertical frame to move upwards, through rotation of a second gear, the extension end of a first telescopic plate slides along an arc groove, a combined magnet strip is unfolded along the arc groove, the whole filter screen is unfolded to be flat, 4-trifluoromethyl nicotinic acid particles in the filter screen are unfolded, and the drying efficiency is higher.

Description

Technical Field

[0001] This disclosure relates to the field of 4-trifluoromethylnicotinic acid preparation technology, and in particular to a method and apparatus for preparing 4-trifluoromethylnicotinic acid. Background Technology

[0002] 4-Trifluoromethylnicotinic acid is a key intermediate in the highly effective insecticide flonicamid. Its preparation involves various technical routes due to factors such as raw material costs, reaction conditions, and environmental requirements. Currently, industrially, the main methods employed are a multi-step synthesis using ethyl trifluoroacetoacetate and cyanoacetamide as starting materials, and a direct fluoroalkylation route using 3-cyanopyridine as a starting material. The latter route has greater industrial potential due to its high yield and inexpensive raw materials. The manufacture of 4-trifluoromethylnicotinic acid falls within the technical fields of biopharmaceutical manufacturing, gene-engineered drugs and vaccine manufacturing, and the preparation of chemical pharmaceutical raw materials.

[0003] In the preparation of 4-trifluoromethylnicotinic acid, when solid powder particles precipitate out, the existing technology requires cleaning and drying. However, the cleaning and drying efficiency is low due to the internal accumulation of the powdered 4-trifluoromethylnicotinic acid, requiring multiple and frequent cleaning processes, which affects the overall production efficiency. Summary of the Invention

[0004] This disclosure aims to at least partially address one of the technical problems in the related art.

[0005] Therefore, the purpose of this disclosure is to provide a method and apparatus for preparing 4-trifluoromethylnicotinic acid.

[0006] To achieve the above objectives, this disclosure provides an apparatus for preparing 4-trifluoromethylnicotinic acid, comprising: a mixing tank, a filter box disposed on one side of the mixing tank, a conveying pipe fixed inside the filter box, and a washing and drying box disposed on the side of the filter box located at the outlet end of the conveying pipe, a door disposed on the top side of the washing and drying box, a collection assembly disposed inside the washing and drying box, a washing assembly disposed at the bottom of the washing and drying box, and a drying assembly disposed at the top of the washing and drying box, the collection assembly being movable between the washing assembly and the drying assembly; the collection assembly includes a frame, mounting plates rotatably mounted on the four sides of the frame, a shaft disk rotatably mounted on the middle surface of the mounting plate, a fixing plate fixed on the bottom surface of the shaft disk facing outward, and a filter being fixed inside the fixing plate. The filter screen has magnetic strips fixed at both ends; the cleaning assembly includes a circular plate, which is fixed on the inner wall of the bottom of the cleaning and drying chamber. The circular plate has movable notches corresponding to the positions of the square frame and the cylindrical filter screen. A storage layer is fixed on the inner wall of the cleaning and drying chamber at the top of the circular plate. The storage layer is connected to an external water source through a pipe. Four sets of spray racks are equidistantly installed on the inner ring of the storage layer. The spray racks are fixedly connected to the storage layer through flexible hoses; the drying assembly includes a blower box, which is rotatably installed on the inner wall of the top of the cleaning and drying chamber. A rotating ring is rotatably installed on the outer end of the top of the cleaning and drying chamber. The rotating ring is fixedly connected to the blower box. An air outlet is opened at the lower end of the blower box. A fan and heating wire are installed inside the blower box. An air inlet is opened on the top surface of the rotating ring.

[0007] Optionally, the conveying pipe is inclined and fixed inside the filter box, the washing and drying box has a connecting port corresponding to the position of the conveying pipe, the bottom of the conveying pipe has a filter groove, and the outlet end of the conveying pipe is slidably fitted with a sleeve frame. The top of the conveying pipe is fixed with a first electric push rod, and the extended end of the first electric push rod is fixedly connected to the sleeve frame. The top side of the mixing tank is fixed with a suction pipe, and the other end of the suction pipe is fixedly connected to the top of the highest point of the conveying pipe.

[0008] Optionally, the cleaning assembly further includes: an internal gear ring, a slide rail, a fourth motor, and a fourth gear. The internal gear ring is fixed to the top of the circular plate and is rotatably mounted on the inner wall of the cleaning and drying chamber. A fourth gear is meshed with one side of the internal gear ring. A fourth motor is fixed to the top of the circular plate at the position corresponding to the fourth gear, and the output end of the fourth motor is fixedly connected to the fourth gear. A slide rail is fixed to the inner ring of the internal gear ring at the position corresponding to the spray frame, and the spray frame is slidably mounted inside the slide rail. A slot is provided on the circular plate at the position on the side of the filter screen, and a drive screw is installed inside the slide rail.

[0009] Optionally, the drying assembly further includes: a first motor, a first gear, and an external gear ring. The outer ring of the rotating ring is fixed with an external gear ring, and one side of the external gear ring is meshed with the first gear. The first gear is rotatably mounted on the top of the cleaning and drying chamber. The first motor is fixedly mounted on the top of the cleaning and drying chamber at a position corresponding to the first gear, and the output end of the first motor is fixedly connected to the first gear.

[0010] Optionally, the collecting component further includes: an arc groove, a second gear, a first telescopic plate, and a toothed plate. The mounting plate has arc grooves on both sides of the shaft disk. Two first telescopic plates are symmetrically and rotatably mounted on the bottom of the shaft disk. A second gear is fixedly sleeved on the first telescopic plate and the rotating shaft surface of the shaft disk. The two second gears are meshed and connected. The extended end of the first telescopic plate slides out of the arc groove and is fixedly connected to the magnet strip. A toothed plate is provided on the side plate of a set of second gears on the back of the shaft disk, and the toothed plate is meshed and connected to the second gear. A limit frame is fixed at the bottom of the toothed plate corresponding to the shaft disk, and the toothed plate slides along the inside of the limit frame.

[0011] Optionally, a second gear ring is fixed to the back of the shaft disk, and a third gear is meshed with the bottom of the second gear ring. A rotating rod is fixed at the shaft center of the third gear, and a sliding sleeve is slidably sleeved on the surface of the rotating rod; wherein, the third gear is rotatably mounted on the back of the mounting plate via a shaft bracket.

[0012] Optionally, a connecting ring is rotatably mounted on the top of the frame, and a second motor is fixed at the inner center of the frame located on the connecting ring. The output end of the second motor passes through the inside of the frame and is fixed with a screw. A movable ring is threaded onto the surface of the screw. The surface of the movable ring facing the rotating rod is rotatably connected to two connecting rods via a rotating shaft. The other ends of the two connecting rods are rotatably connected to both sides of the sliding sleeve on the rotating rod via a rotating shaft.

[0013] Optionally, a horizontal shaft is rotatably mounted at the bottom of the frame corresponding to the position of each rotating rod. A plate is fixed to one end of the rotating rod facing the shaft, and a slot is opened on the shaft corresponding to the position of the plate. A driven bevel gear is fixed to the other end of the shaft. A third motor is rotatably mounted at the bottom of the screw, and a driving bevel gear is fixed to the output end of the third motor. The driving bevel gear meshes with four driven bevel gears.

[0014] Optionally, the top of the connecting ring is provided with a circular ring, and the bottom of the circular ring is fixed with a vertical frame corresponding to the position of each mounting plate. The vertical frame slides through the square frame and is fixed with a second telescopic plate. The extended end of the second telescopic plate is rotatably connected to the top of the toothed plate through a rotating shaft. The bottom of the square frame is fixed with a third electric push rod corresponding to the circular ring, and the extended end of the third electric push rod is fixedly connected to the circular ring. In addition, four sets of second electric push rods are fixed at the top of the washing and drying box corresponding to the position of the connecting ring, and the extended ends of the second electric push rods are fixedly connected to the connecting ring.

[0015] A method for preparing 4-trifluoromethylnicotinic acid, the method comprising the following steps: (1) Take an appropriate amount of 4-trifluoromethylnicotinamide and 25% sodium hydroxide aqueous solution and add them to a mixing tank containing Pd / MCM-22 catalyst; (2) Heat the mixture to 100°C and keep it at that temperature for 4 hours. During this time, the solid gradually dissolves and the solution turns into a pale yellow and clear state. (3) After the reaction is complete, cool to room temperature, adjust the pH to about 2 with concentrated hydrochloric acid, and stir to allow the product to be fully separated; (4) The solid-liquid mixture is pumped into the filter box by a suction pump, and the solid particles are sent into the cylindrical filter screen of the collection component; (5) The solid particles inside the cylindrical filter screen are repeatedly rinsed by the cleaning component. After rinsing, the collection component is moved to the bottom of the drying component. (6) The cylindrical filter screen of the collection component is spread out in a planar shape, and the drying component dries the particles spread out in the planar shape.

[0016] The technical solution provided in this disclosure may include the following beneficial effects: 1. In this invention, after the cylindrical filter screen moves to the communication port position and rotates upward, the first electric push rod pushes the sleeve frame to move and insert into the cylindrical filter screen, preventing 4-trifluoromethylnicotinic acid particles from falling to the outside. When the suction tube sends the 4-trifluoromethylnicotinic acid particles and liquid into the conveying pipe, the liquid falls through the filter tank to the bottom of the filter box and is sent out through the drain pipe. The inclined conveying pipe also facilitates the sliding of the 4-trifluoromethylnicotinic acid particles. 2. The present invention uses a second electric push rod to drive the square frame to move vertically, which can correspond the collection component with the cleaning component and the drying component. When the square frame is inside the circular plate, the cylindrical filter screen is also located in the moving notch of the circular plate. The rotation of the circular plate can drive the square frame to rotate, so that the filter screens at different positions correspond to the communication port position, and the 4-trifluoromethylnicotinic acid particles sent out by the conveying pipe are received. 3. This invention uses a connecting ring to maintain the connection between the square frame and the extended end of the second electric push rod, and is unaffected by the rotation of the square frame. When receiving 4-trifluoromethylnicotinic acid particles, the second motor drives the screw to rotate, and the moving ring moves downward in a threaded engagement with the screw. The connecting rod pushes the insert plate of the rotating rod to separate from the shaft slot through the sliding sleeve. Subsequently, the rotating rod drives the mounting plate to rotate downward, while the open end of the cylindrical filter screen rotates upward to align with the outlet end of the conveying pipe, facilitating the feeding of 4-trifluoromethylnicotinic acid particles into the filter screen. After receiving, the cylindrical filter screen is rotated to a horizontal position, and the insert plate of the rotating rod re-aligns with the shaft. The rod is inserted into the slot. When the square frame is inside the circular plate, the rotation of the circular plate of the cleaning component will drive the square frame and the cylindrical filter screen to rotate together. When the square frame moves out of the circular plate, the rotation of the circular plate can independently control the rotation of the spray frame. This process can misalign the spray frame and slide rail with the cylindrical filter screen, thereby facilitating the upward movement of the collection component to approach the drying component. At the same time, during the cleaning stage, the spray frame and slide rail can also be moved to the top of the cylindrical filter screen. The drive screw inside the slide rail controls the movement of the spray frame, so that the spray frame can repeatedly rinse the 4-trifluoromethylnicotinic acid particles inside the cylindrical filter screen. 4. During the rinsing process, the third motor at the top of the screw drives the active bevel gear to rotate and mesh with four driven bevel gears. Through the insertion of the shaft and rotating rod, the third gear rotates and meshes with the second gear ring. The entire shaft disk drives the cylindrical filter screen to rotate. The continuous shaking of the 4-trifluoromethylnicotinic acid particles inside can improve the cleaning effect. When the collection component is close to the drying component, the third electric push rod pushes the ring and the vertical frame to move upward. Through the rotation of the second gear, the extended end of the first telescopic plate slides along the arc groove, unfolding the merged magnetic strips along the arc groove. The entire filter screen unfolds into a flat shape, and the 4-trifluoromethylnicotinic acid particles inside spread out, resulting in higher drying efficiency.

[0017] Additional aspects and advantages of this disclosure will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of this disclosure. Attached Figure Description

[0018] The above and / or additional aspects and advantages of this disclosure will become apparent and readily understood from the following description of the embodiments taken in conjunction with the accompanying drawings, in which: Figure 1 This is a schematic flowchart of a method for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 2 This is a schematic diagram of the overall structure of a 4-trifluoromethylnicotinic acid preparation apparatus according to an embodiment of this disclosure; Figure 3 This is a schematic diagram of the internal structure of the filter box and the cleaning and drying box in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 4This is a schematic diagram showing the corresponding delivery pipe and connecting port in a 4-trifluoromethylnicotinic acid preparation apparatus according to an embodiment of this disclosure; Figure 5 This is a schematic diagram of the drying component structure in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 6 This is a schematic diagram showing the connection between the collection component and the circular plate in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 7 This is a schematic diagram showing the connection between the cleaning component and the collection component in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 8 This is a schematic diagram of the cleaning component structure in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 9 This is a schematic diagram showing the positional relationship between the collecting component, drying component, and cleaning component in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure. Figure 10 This is a schematic diagram of the unfolded structure of a filter screen in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 11 This is a schematic diagram of the internal structure of a frame in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 12 This is a schematic diagram of the connection between the mounting plate and the moving ring in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; Figure 13 This is a schematic diagram of the connection between the shaft and the rotating rod in an apparatus for preparing 4-trifluoromethylnicotinic acid according to an embodiment of this disclosure; As shown in the figure: 1. Mixing tank; 11. Suction pipe; 2. Filter box; 21. Drain pipe; 22. Conveyor pipe; 23. Filter tank; 24. First electric push rod; 25. Sleeve frame; 3. Cleaning the drying oven; 31. Drain pipe; 32. Connecting port; 4. Drying assembly; 41. First motor; 42. First gear; 43. External gear ring; 44. Rotary ring; 45. Air box; 5. Collection component; 51. Second electric push rod; 52. Square frame; 53. Filter screen; 54. Connecting ring; 55. Second motor; 56. Circular ring; 57. Mounting plate; 58. Shaft disc; 59. Magnet strip; 510. Fixing plate; 511. Screw; 512. Moving ring; 513. Third electric push rod; 514. Vertical frame; 515. Connecting rod; 516. Rotating rod; 517. Insert plate; 518. Shaft; 519. Arc groove; 520. Second gear ring; 521. Second gear; 522. First telescopic plate; 523. Third gear; 524. Second telescopic plate; 525. Gear plate; 526. Driven bevel gear; 527. Driving bevel gear; 528. Third motor; 6. Cleaning assembly; 61. Circular plate; 62. Internal gear ring; 63. Storage layer; 64. Slide rail; 65. Spray rack; 66. Gutter; 67. Fourth motor; 68. Fourth gear. Detailed Implementation

[0019] Embodiments of this disclosure are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are used only to explain this disclosure, and should not be construed as limiting this disclosure. Rather, embodiments of this disclosure include all variations, modifications, and equivalents falling within the spirit and scope of the appended claims.

[0020] like Figure 1 As shown, a method for preparing 4-trifluoromethylnicotinic acid includes the following steps: (1) Take an appropriate amount of 4-trifluoromethylnicotinamide and 25% sodium hydroxide aqueous solution and add them to a mixing tank containing Pd / MCM-22 catalyst; (2) Heat the mixture to 100°C and keep it at that temperature for 4 hours. During this time, the solid gradually dissolves and the solution turns into a pale yellow and clear state. (3) After the reaction is complete, cool to room temperature, adjust the pH to about 2 with concentrated hydrochloric acid, and stir to allow the product to be fully separated; (4) The solid-liquid mixture is pumped into the filter box by a suction pump, and the solid particles are sent into the cylindrical filter screen of the collection component; (5) The solid particles inside the cylindrical filter screen are repeatedly rinsed by the cleaning component. After rinsing, the collection component is moved to the bottom of the drying component. (6) The cylindrical filter screen of the collection component is spread out in a planar shape, and the drying component dries the particles spread out in the planar shape.

[0021] like Figure 2 , Figure 3 , Figure 4 , Figure 6 , Figure 7and Figure 8 As shown in the present disclosure, an apparatus for preparing 4-trifluoromethylnicotinic acid is proposed, comprising: a mixing tank 1, a filter box 2 disposed on one side of the mixing tank 1, a conveying pipe 22 fixed inside the filter box 2, and a washing and drying box 3 disposed on the side of the filter box 2 located at the outlet end of the conveying pipe 22, a door disposed on the top side of the washing and drying box 3, a collection component 5 disposed inside the washing and drying box 3, a washing component 6 disposed at the bottom of the washing and drying box 3, and a drying component 4 disposed at the top of the washing and drying box 3; the collection component 5 is movable between the washing component 6 and the drying component 4; the collection component 5 includes a frame 52, and the four sides of the frame 52 are rotatably mounted. The system includes a mounting plate 57, on which a shaft disc 58 is rotatably mounted. A fixing plate 510 is fixed to the bottom surface of the shaft disc 58 facing outwards, and a filter screen 53 is fixed inside the fixing plate 510. Magnet strips 59 are fixed to both ends of the filter screen 53. The cleaning assembly 6 includes a circular plate 61, which is fixed to the inner wall of the bottom of the cleaning and drying chamber 3. The circular plate 61 has movable notches corresponding to the positions of the square frame 52 and the cylindrical filter screen 53. A storage layer 63 is fixed to the inner wall of the cleaning and drying chamber 3 at the top of the circular plate 61. The storage layer 63 is connected to an external water source through a pipe. Four sets of spray racks 65 are equidistantly installed on the inner ring of the storage layer 63. The spray frame 65 is fixedly connected to the storage layer 63 via a hose; the drying assembly 4 includes a blower box 45, which is rotatably mounted on the inner top wall of the cleaning and drying chamber 3, and a rotating ring 44 is rotatably mounted on the outer top of the cleaning and drying chamber 3. The rotating ring 44 is fixedly connected to the blower box 45. An air outlet is provided at the lower end of the blower box 45, and a fan and heating wire are installed inside the blower box 45. An air inlet is provided on the top surface of the rotating ring 44. When using the device, take an appropriate amount of 4-trifluoromethylnicotinamide and 25% sodium hydroxide aqueous solution and add them to the mixing tank 1 containing the Pd / MCM-22 catalyst. Heat the mixture to 100°C and keep it at that temperature for 4 hours. During the reaction, the solid gradually dissolves, and the solution becomes a pale yellow and clear state. After the reaction is completed, the solution is cooled to room temperature, and the pH is adjusted to about 2 with concentrated hydrochloric acid. The product is stirred to fully precipitate. The solid-liquid mixture is then pumped into the filter box 2 using a suction pump, and the solid particles are sent into the cylindrical filter screen 53 of the collection component 5. The solid particles in the cylindrical filter screen 53 are repeatedly rinsed by the cleaning component 6. After rinsing, the collection component 5 is moved to the bottom of the drying component 4, and the cylindrical filter screen 53 of the collection component 5 is spread out into a flat shape. The drying component 4 dries the spread-out particles. The door on the top side of the cleaning and drying box 3 is not shown in the diagram and can be removed after the 4-trifluoromethylnicotinamide is dried.

[0022] like Figure 3 and Figure 4As shown, in some embodiments, the conveying pipe 22 is inclined and fixed inside the filter box 2, the washing and drying box 3 has a connecting port 32 corresponding to the position of the conveying pipe 22, the bottom of the conveying pipe 22 has a filter groove 23, and the outlet end of the conveying pipe 22 is slidably sleeved with a sleeve frame 25. The top of the conveying pipe 22 is fixed with a first electric push rod 24, and the extended end of the first electric push rod 24 is fixedly connected to the sleeve frame 25. Among them, a suction pipe 11 is fixed on one side of the top of the mixing tank 1, and the other end of the suction pipe 11 is fixedly connected to the top of the highest point of the conveying pipe 22.

[0023] Understandably, after the cylindrical filter screen 53 moves to the position of the connecting port 32 and rotates upward, the first electric push rod 24 pushes the sleeve frame 25 to move and insert into the cylindrical filter screen 53, preventing 4-trifluoromethylnicotinic acid particles from falling to the outside. When the suction pipe 11 sends the 4-trifluoromethylnicotinic acid particles and liquid into the conveying pipe 22, the liquid falls through the filter tank 23 to the bottom of the filter box 2 and is sent out through the drain pipe 21. The inclined conveying pipe 22 also facilitates the sliding of the 4-trifluoromethylnicotinic acid particles.

[0024] like Figure 2 , Figure 6 , Figure 7 and Figure 8 As shown, in some embodiments, the cleaning assembly 6 further includes: an internal gear ring 62, a slide rail 64, a fourth motor 67, and a fourth gear 68. The internal gear ring 62 is fixed to the top of the circular plate 61 and is rotatably mounted on the inner wall of the cleaning and drying chamber 3. The fourth gear 68 is meshed with one side of the internal gear ring 62. The fourth motor 67 is fixed to the top of the circular plate 61 at the position corresponding to the fourth gear 68, and the output end of the fourth motor 67 is fixedly connected to the fourth gear 68. The slide rail 64 is fixed to the inner ring of the internal gear ring 62 at the position corresponding to the spray frame 65, and the spray frame 65 is slidably mounted inside the slide rail 64. The circular plate 61 has a slot 66 at the position on one side of the filter screen 53, and a drive screw is installed inside the slide rail 64.

[0025] Understandably, the fourth motor 67 drives the fourth gear 68 to rotate and mesh with the internal gear ring 62, so that the internal gear ring 62 and the circular plate 61 rotate synchronously. This allows the position of the spray frame 65 to be adjusted and different positions to be rinsed. The wastewater generated during rinsing flows into the bottom of the cleaning and drying box 3 through the filter screen 53 itself and the trough 66, and is then discharged through the drain pipe 31.

[0026] like Figure 3 , Figure 5 and Figure 9As shown, in some embodiments, the drying assembly 4 further includes: a first motor 41, a first gear 42, and an external gear ring 43. The outer ring of the rotating ring 44 is fixed with an external gear ring 43, and one side of the external gear ring 43 is meshed with the first gear 42. The first gear 42 is rotatably mounted on the top of the cleaning and drying chamber 3. The first motor 41 is fixedly mounted on the top of the cleaning and drying chamber 3 at the position corresponding to the first gear 42, and the output end of the first motor 41 is fixedly connected to the first gear 42.

[0027] It should be noted that the first motor 41 drives the first gear 42 to rotate and mesh with the external gear ring 43. The external gear ring 43 drives the rotating ring 44 and the air box 45 to rotate. With the help of the fan and heating wire inside the air box 45, air is drawn in from the air inlet of the rotating ring 44, heated and sent out from the air outlet at the bottom of the air box 45 to dry the 4-trifluoromethylnicotinic acid particles on the surface of the filter screen 53. The washing and drying technology used in this embodiment and the embodiment of the cleaning assembly are the washing and drying technology principles used in the prior art of biopharmaceutical manufacturing, gene-engineered drug and vaccine manufacturing, and chemical drug raw material preparation.

[0028] like Figure 6 , Figure 7 , Figure 10 , Figure 11 , Figure 12 and Figure 13As shown, in some embodiments, the collecting component 5 further includes: an arc groove 519, a second gear 521, a first telescopic plate 522, and a toothed plate 525. The mounting plate 57 has arc grooves 519 on both sides of the shaft disk 58. Two first telescopic plates 522 are symmetrically and rotatably mounted on the bottom of the shaft disk 58. A second gear 521 is fixedly sleeved on the surface of the first telescopic plate 522 and the rotating shaft of the shaft disk 58. The two second gears 521 mesh with each other. The extended ends of the first telescopic plates 522 slide out of the arc grooves 519 and are fixedly connected to the magnet strip 59. A toothed plate 525 is provided on the side plate of a set of second gears 521 on the back of the shaft disk 58, and the toothed plate 525 meshes with the second gears 521. A limiting frame is fixed to the bottom of the shaft disk 58 corresponding to the toothed plate 525, and the toothed plate 525 slides along the inside of the limiting frame. A second toothed ring 520 is fixed to the back of the shaft disk 58, and a third gear 523 is meshed with the bottom of the second toothed ring 520. A rotating rod 516 is fixed at the center of the shaft of the third gear 523, and a sliding sleeve is slidably sleeved on the surface of the rotating rod 516. The third gear 523 is rotatably mounted on the back of the mounting plate 57 via a shaft bracket. A connecting ring 54 is rotatably mounted on the top of the square frame 52, and a second motor 55 is fixed at the center of the inner circle of the connecting ring 54. The output end of the second motor 55 passes through the inside of the square frame 52 and a screw 511 is fixed thereon. A movable ring 512 is threaded onto the surface of the movable ring 512 facing the rotating rod 516, and two connecting rods 515 are rotatably connected to it via a rotating shaft. The other ends of the two connecting rods 515 are rotatably connected to both sides of the sliding sleeve on the rotating rod 516 via a rotating shaft. A transverse shaft 518 is rotatably mounted at the bottom of the frame 52 corresponding to the position of each rotating rod 516. A plate 517 is fixed to one end of the rotating rod 516 facing the shaft 518, and a slot is provided on the shaft 518 corresponding to the position of the plate 517. A driven bevel gear 526 is fixed to the other end of the shaft 518. A third motor 528 is rotatably mounted at the bottom of the screw 511, and a driving bevel gear 527 is fixed to the output end of the third motor 528. The bevel gear 527 meshes with four driven bevel gears 526. The top of the connecting ring 54 is provided with a ring 56, and the bottom of the ring 56 is fixed with a vertical frame 514 corresponding to the position of each mounting plate 57. The vertical frame 514 slides through the square frame 52 and is fixed with a second telescopic plate 524. The extended end of the second telescopic plate 524 is rotatably connected to the top of the toothed plate 525 through a rotating shaft. The bottom of the square frame 52 is fixed with a third electric push rod 513 corresponding to the ring 56, and the extended end of the third electric push rod 513 is fixedly connected to the ring 56. The top of the cleaning and drying box 3 is fixed with four sets of second electric push rods 51 corresponding to the position of the connecting ring 54, and the extended end of the second electric push rods 51 is fixedly connected to the connecting ring 54.

[0029] It should be noted that by moving the square frame 52 vertically via the second electric push rod 51, the collecting component 5 can be aligned with the washing component 6 and the drying component 4. When the square frame 52 is inside the circular plate 61, the cylindrical filter screen 53 is also located within the moving notch of the circular plate 61. The rotation of the circular plate 61 can drive the square frame 52 to rotate, aligning the filter screens 53 at different positions with the connecting port 32 to receive the 4-trifluoromethylnicotinic acid particles sent from the conveying pipe 22. During this process, the connection between the square frame 52 and the extended end of the second electric push rod 51 is maintained by the connecting ring 54, and is unaffected by the rotation of the square frame 52. When receiving 4-trifluoromethylnicotinic acid particles, the second motor 55 drives... When the screw 511 rotates, the moving ring 512 moves downward in a threaded engagement with the screw 511. The connecting rod 515 pushes the insert plate 517 of the rotating rod 516 to separate from the slot of the shaft 518 through the sliding sleeve. Then, the rotating rod 516 drives the mounting plate 57 to rotate downward, while the open end of the cylindrical filter screen 53 rotates upward to connect with the outlet end of the conveying pipe 22, facilitating the feeding of 4-trifluoromethylnicotinic acid particles into the filter screen 53. After receiving, the cylindrical filter screen 53 is rotated to a horizontal position, and the insert plate 517 of the rotating rod 516 re-engages with the slot of the shaft 518. When the square frame 52 is located inside the circular plate 61, the rotation of the circular plate 61 of the cleaning assembly 6 will drive the square frame 52 and the cylindrical filter screen 53 to rotate together. When the square frame 52 moves out of the circular plate 61, the circular plate 61 of the cleaning assembly 6 will rotate the square frame 52 and the cylindrical filter screen 53 together. After the circular plate 61, the rotation of the circular plate 61 can independently control the rotation of the spray frame 65. This process can misalign the spray frame 65 and the slide rail 64 with the cylindrical filter screen 53, thereby facilitating the upward movement of the collection component 5 towards the drying component 4. Simultaneously, during the cleaning stage, the spray frame 65 and the slide rail 64 can be moved to the top of the cylindrical filter screen 53. The drive screw inside the slide rail 64 controls the movement of the spray frame 65, allowing it to repeatedly rinse the 4-trifluoromethylnicotinic acid particles inside the cylindrical filter screen 53. During rinsing, the third motor 528 at the top of the screw 511 drives the active bevel gear 527 to rotate and mesh with four driven bevel gears 526. This is achieved through the shaft 518 and the rotating rod 516. The insertion allows the third gear 523 to rotate and mesh with the second gear ring 520. The entire shaft disk 58 drives the cylindrical filter screen 53 to rotate. The continuous shaking of the 4-trifluoromethylnicotinic acid particles inside improves the cleaning effect. When the collecting component 5 approaches the drying component 4, the third electric push rod 513 pushes the ring 56 and the vertical frame 514 upward. Through the rotation of the second gear 521, the extended end of the first telescopic plate 522 slides along the arc groove 519, unfolding the merged magnet strip 59 along the arc groove 519. The entire filter screen 53 unfolds into a flat shape, and the 4-trifluoromethylnicotinic acid particles inside spread out, resulting in higher drying efficiency. The filter screen in this solution is similar to that used in biopharmaceutical manufacturing; genetic engineering drugs and vaccine manufacturing.In technical solutions for the preparation of chemical pharmaceutical raw materials, the disc or plate receiving device for receiving or conveying the reagent differs from existing methods in that this solution uses a filter screen 53 for receiving. This filter screen can be cylindrical or unfolded into a flat shape, facilitating rinsing and drying, thus improving overall processing efficiency.

[0030] Working principle: When using the apparatus, add an appropriate amount of 4-trifluoromethylnicotinamide and 25% sodium hydroxide aqueous solution to the mixing tank 1 containing the Pd / MCM-22 catalyst. Heat the mixture to 100°C and maintain the temperature for 4 hours. During this time, the solid gradually dissolves, and the solution becomes a pale yellow and clear state. After the reaction is complete, cool to room temperature and adjust the pH to about 2 with concentrated hydrochloric acid. Stir to allow the product to fully precipitate. Use a suction pump to draw the solid-liquid mixture into the filter box 2. After the cylindrical filter screen 53 moves to the position of the connecting port 32 and rotates upward, the first electric push rod 24 pushes the sleeve 25 to move and insert it into the cylindrical filter screen 53 to prevent 4-trifluoromethylnicotinamide particles from falling to the outside. The 4-trifluoromethylnicotinamide particles and liquid are sent into the delivery pipe 22 through the suction pipe 11. Inside, the liquid falls from the filter tank 23 to the bottom of the filter box 2 and is discharged through the drain pipe 21. The inclined conveying pipe 22 also facilitates the sliding of 4-trifluoromethylnicotinic acid particles. The solid particles inside the cylindrical filter screen 53 are repeatedly washed by the cleaning component 6. The fourth motor 67 drives the fourth gear 68 to rotate and mesh with the internal gear ring 62, so that the internal gear ring 62 and the circular plate 61 rotate synchronously. The position of the spray frame 65 can be adjusted to wash different positions. The wastewater generated by washing flows into the bottom of the washing and drying box 3 through the filter screen 53 itself and the trough 66 and is discharged through the drain pipe 31. After washing, the collection component 5 is moved to the bottom of the drying component 4. The cylindrical filter screen 53 of the collection component 5 is spread out into a flat shape and driven by the first motor 41. The first gear 42 rotates and meshes with the external gear ring 43. The external gear ring 43 drives the rotating ring 44 and the air box 45 to rotate. In conjunction with the fan and heating wire inside the air box 45, air is drawn in through the air inlet of the rotating ring 44, heated, and then sent out through the air outlet at the bottom of the air box 45 to dry the 4-trifluoromethylnicotinic acid particles on the surface of the filter screen 53. The second electric push rod 51 drives the square frame 52 to move vertically, aligning the collecting component 5 with the cleaning component 6 and the drying component 4. When the square frame 52 is inside the circular plate 61, the cylindrical filter screen 53 is also located within the moving notch of the circular plate 61. The rotation of the circular plate 61 drives the square frame 52 to rotate, aligning the filter screens 53 at different positions with the connecting port 32, thus aligning the conveying pipe 22. The 4-trifluoromethylnicotinic acid particles are received. During this process, the connection between the frame 52 and the extended end of the second electric push rod 51 is maintained by the connecting ring 54, and is unaffected by the rotation of the frame 52. When receiving the 4-trifluoromethylnicotinic acid particles, the second motor 55 drives the screw 511 to rotate. The moving ring 512 moves downward in a threaded engagement with the screw 511. The connecting rod 515 pushes the insert plate 517 of the rotating rod 516 to separate from the slot of the shaft 518 through the sliding sleeve. Then, the rotating rod 516 drives the mounting plate 57 to rotate downward, while the open end of the cylindrical filter screen 53 rotates upward to align with the outlet end of the conveying pipe 22, facilitating the feeding of 4-trifluoromethylnicotinic acid particles into the filter screen 53. After receiving, the cylindrical filter screen 53 is rotated to a horizontal position.The insert plate 517 of the rotating rod 516 re-engages with the slot of the shaft 518. When the square frame 52 is inside the circular plate 61, the rotation of the circular plate 61 of the cleaning assembly 6 will cause the square frame 52 and the cylindrical filter screen 53 to rotate together. After the square frame 52 moves out of the circular plate 61, the rotation of the circular plate 61 can independently control the rotation of the spray frame 65. This process can misalign the spray frame 65 and the slide rail 64 with the cylindrical filter screen 53, thereby facilitating the upward movement of the collection assembly 5 towards the drying assembly 4. At the same time, during the cleaning stage, the spray frame 65 and the slide rail 64 can also be moved to the top of the cylindrical filter screen 53. The drive screw inside the slide rail 64 controls the movement of the spray frame 65, so that the spray frame 65 can repeatedly rinse the 4-trifluoromethylnicotinic acid particles inside the cylindrical filter screen 53. During the rinsing process... The third motor 528 at the top of the screw 511 drives the active bevel gear 527 to rotate and mesh with four driven bevel gears 526. Through the connection of the shaft 518 and the rotating rod 516, the third gear 523 rotates and meshes with the second gear ring 520. The entire shaft disc 58 drives the cylindrical filter screen 53 to rotate. The continuous shaking of the 4-trifluoromethylnicotinic acid particles inside improves the cleaning effect. When the collecting component 5 approaches the drying component 4, the third electric push rod 513 pushes the ring 56 and the vertical frame 514 upwards. Through the rotation of the second gear 521, the extended end of the first telescopic plate 522 slides along the arc groove 519, unfolding the merged magnet strip 59 along the arc groove 519. The entire filter screen 53 unfolds into a flat shape, and the internal 4-trifluoromethylnicotinic acid particles spread out, resulting in higher drying efficiency.

[0031] In the description of this disclosure, the terms "first," "second," etc., are used for descriptive purposes only and should not be construed as indicating or implying relative importance. Furthermore, in the description of this disclosure, unless otherwise stated, "a plurality of" means two or more.

[0032] Any process or method description in the flowchart or otherwise herein can be understood as representing a module, segment, or portion of code comprising one or more executable instructions for implementing a particular logical function or process, and the scope of preferred embodiments of this disclosure includes additional implementations in which functions may be performed not in the order shown or discussed, including substantially simultaneously or in reverse order depending on the function involved, as will be understood by those skilled in the art to which embodiments of this disclosure pertain.

[0033] In the description of this specification, references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of this disclosure. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.

[0034] Although embodiments of the present disclosure have been shown and described above, it is to be understood that the above embodiments are exemplary and should not be construed as limiting the present disclosure. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present disclosure.

Claims

1. An apparatus for preparing 4-trifluoromethylnicotinic acid, characterized in that, include: A mixing tank (1) is provided with a filter box (2) on one side of the mixing tank (1). A conveying pipe (22) is fixed inside the filter box (2). A cleaning and drying box (3) is provided on the side of the filter box (2) located at the outlet end of the conveying pipe (22). A box door is provided on the top side of the cleaning and drying box (3). A collection component (5) is provided inside the cleaning and drying box (3). A cleaning component (6) is provided at the bottom of the cleaning and drying box (3). A drying component (4) is provided at the top of the cleaning and drying box (3). The collection component (5) moves between the cleaning component (6) and the drying component (4). The collecting component (5) includes a frame (52), on which mounting plates (57) are rotatably mounted on the four sides. A shaft disk (58) is rotatably mounted on the middle surface of the mounting plate (57). A fixing plate (510) is fixed on the bottom surface of the shaft disk (58) facing outward. A filter screen (53) is fixed inside the fixing plate (510). Magnet strips (59) are fixed at both ends of the filter screen (53). The cleaning assembly (6) includes a circular plate (61). The circular plate (61) is fixed on the inner wall of the bottom of the cleaning and drying box (3). The circular plate (61) has a movable notch at the position corresponding to the square frame (52) and the cylindrical filter screen (53). A storage layer (63) is fixed on the inner wall of the cleaning and drying box (3) at the top of the circular plate (61). The storage layer (63) is connected to an external water source through a pipe. Four sets of spray racks (65) are installed equidistantly on the inner ring of the storage layer (63). The spray racks (65) are fixedly connected to the storage layer (63) through hoses. The drying assembly (4) includes a blower box (45). The blower box (45) is rotatably mounted on the top inner wall of the cleaning and drying box (3), and a rotating ring (44) is rotatably mounted on the top outer end of the cleaning and drying box (3). The rotating ring (44) is fixedly connected to the blower box (45). An air outlet is opened at the lower end of the blower box (45), and a fan and heating wire are installed inside the blower box (45). An air inlet is opened on the top surface of the rotating ring (44).

2. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 1, characterized in that, The conveying pipe (22) is fixed at an inclination inside the filter box (2). The cleaning and drying box (3) has a connecting port (32) at the position corresponding to the conveying pipe (22). The bottom of the conveying pipe (22) has a filter groove (23). The outlet end of the conveying pipe (22) is slidably sleeved with a sleeve frame (25). The top of the conveying pipe (22) is fixed with a first electric push rod (24), and the extended end of the first electric push rod (24) is fixedly connected to the sleeve frame (25). The mixing tank (1) is fixed with a suction pipe (11) on one side of the top, and the other end of the suction pipe (11) is fixedly connected to the top of the highest point of the conveying pipe (22).

3. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 1, characterized in that, The cleaning assembly (6) further includes: The internal gear ring (62), slide rail (64), fourth motor (67), and fourth gear (68) are provided. The top of the circular plate (61) is fixed with an internal gear ring (62), and the internal gear ring (62) is rotatably mounted on the inner wall of the cleaning and drying box (3). The fourth gear (68) is meshed with one side of the internal gear ring (62). The fourth motor (67) is fixed at the top of the circular plate (61) corresponding to the position of the fourth gear (68), and the output end of the fourth motor (67) is fixedly connected to the fourth gear (68). The slide rail (64) is fixed at the position of the inner ring of the internal gear ring (62) corresponding to the position of the spray frame (65). The spray frame (65) is slidably mounted inside the slide rail (64). The circular plate (61) has a slot (66) on one side of the filter screen (53), and a drive screw is installed inside the slide rail (64).

4. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 1, characterized in that, The drying component (4) also includes: The first motor (41), the first gear (42), and the external gear ring (43) are connected. The outer ring of the rotating ring (44) is fixed with the external gear ring (43). The first gear (42) is meshed with one side of the external gear ring (43). The first gear (42) is rotatably mounted on the top of the cleaning and drying box (3). The first motor (41) is fixedly installed on the top of the cleaning and drying box (3) at the position corresponding to the first gear (42), and the output end of the first motor (41) is fixedly connected to the first gear (42).

5. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 1, characterized in that, The collection component (5) also includes: Arc groove (519), second gear (521), first telescopic plate (522), toothed plate (525). The mounting plate (57) is provided with arc groove (519) on both sides of the shaft disk (58). Two first telescopic plates (522) are symmetrically rotated and installed at the bottom of the shaft disk (58). The first telescopic plate (522) and the rotating shaft surface of the shaft disk (58) are fixedly sleeved with the second gear (521). The two second gears (521) are meshed and connected. The extended end of the first telescopic plate (522) slides out of the arc groove (519) and is fixedly connected with the magnet strip (59). The back of the shaft disk (58) is provided with a toothed plate (525) on the side plate of a set of second gears (521). The toothed plate (525) is meshed and connected with the second gear (521). The shaft disk (58) is fixed with a limit frame at the bottom of the toothed plate (525), and the toothed plate (525) slides along the inside of the limit frame.

6. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 5, characterized in that, A second toothed ring (520) is fixed on the back of the shaft disk (58), and a third gear (523) is meshed with the bottom of the second toothed ring (520). A rotating rod (516) is fixed at the shaft center of the third gear (523), and a sliding sleeve is slidably sleeved on the surface of the rotating rod (516). The third gear (523) is rotatably mounted on the back of the mounting plate (57) via a shaft bracket.

7. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 6, characterized in that, A connecting ring (54) is rotatably mounted on the top of the frame (52), and a second motor (55) is fixed at the inner center of the connecting ring (54) of the frame (52). The output end of the second motor (55) is inserted into the inside of the frame (52) and a screw (511) is fixed thereon. A movable ring (512) is threaded onto the surface of the screw (511). The movable ring (512) facing the rotating rod (516) is rotatably connected to two connecting rods (515) through a rotating shaft. The other ends of the two connecting rods (515) are rotatably connected to the two sides of the upper sliding sleeve of the rotating rod (516) via a rotating shaft.

8. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 7, characterized in that, A transverse shaft (518) is rotatably mounted at the bottom of the frame (52) corresponding to the position of each rotating rod (516). A plate (517) is fixed at one end of the rotating rod (516) facing the shaft (518), and a slot is opened at the position of the shaft (518) corresponding to the plate (517). A driven bevel gear (526) is fixed at the other end of the shaft (518). A third motor (528) is rotatably mounted at the bottom of the screw (511), and a driving bevel gear (527) is fixed at the output end of the third motor (528). The driving bevel gear (527) meshes with four driven bevel gears (526).

9. The apparatus for preparing 4-trifluoromethylnicotinic acid according to claim 8, characterized in that, The top of the connecting ring (54) is provided with a ring (56), and the bottom of the ring (56) is fixed with a vertical frame (514) corresponding to the position of each mounting plate (57). The vertical frame (514) slides through the square frame (52) and is fixed with a second telescopic plate (524). The extended end of the second telescopic plate (524) is rotatably connected to the top of the toothed plate (525) through a rotating shaft. The bottom of the square frame (52) is fixed with a third electric push rod (513), and the extended end of the third electric push rod (513) is fixedly connected to the ring (56). Among them, four sets of second electric push rods (51) are fixed on the top of the cleaning and drying box (3) at the position corresponding to the connecting ring (54), and the extended end of the second electric push rod (51) is fixedly connected to the connecting ring (54).

10. A method for preparing 4-trifluoromethylnicotinic acid using the apparatus according to claim 1, characterized in that: The preparation method includes the following steps: (1) Take an appropriate amount of 4-trifluoromethylnicotinamide and 25% sodium hydroxide aqueous solution and add them to a mixing tank containing Pd / MCM-22 catalyst; (2) Heat the mixture to 100°C and keep it at that temperature for 4 hours. During this time, the solid gradually dissolves and the solution turns into a pale yellow and clear state. (3) After the reaction is complete, cool to room temperature, adjust the pH to about 2 with concentrated hydrochloric acid, and stir to allow the product to be fully separated; (4) The solid-liquid mixture is pumped into the filter box by a suction pump, and the solid particles are sent into the cylindrical filter screen of the collection component; (5) The solid particles inside the cylindrical filter screen are repeatedly rinsed by the cleaning component. After rinsing, the collection component is moved to the bottom of the drying component. (6) The cylindrical filter screen of the collection component is spread out in a planar shape, and the drying component dries the particles spread out in the planar shape.

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