An apparatus for the synthesis of 5-fluorouracil derivatives

Abstract

The utility model relates to chemical substance mixing production technical field discloses a kind of synthesis device of 5-fluorouracil derivative, including reaction bin, the temperature control bin is fixedly connected with reaction bin outer wall, the thermostat is installed in the temperature control bin inner wall, the water pump is installed in the bottom end of reaction bin, the processing bin is fixedly connected with the water pump bottom end, the motor one is fixedly connected with the top end of reaction bin, the drive end of the motor one is fixedly connected with reciprocating screw rod, the outer wall of reciprocating screw rod is connected with gear plate by reciprocating group, the outer wall of gear plate is engaged and is connected with driven gear. In the utility model, through the synergy of different direction mechanical shearing, forced convection, dynamic temperature control, the local concentration gradient and temperature lag phenomenon existing in traditional stirring device is completely eliminated, the reaction bin is uniformly mixed, and the periodic rotation of screen mesh is driven by adapter block and traction plate, and the precipitate is discharged, and centrifugal processing is facilitated.

Description

Technical Field

[0001] This utility model relates to the field of chemical substance mixing and production technology, and in particular to a synthesis apparatus for 5-fluorouracil derivatives. Background Technology

[0002] 5-Fluorouracil (5-FU) is a broad-spectrum antitumor drug widely used in the treatment of solid tumors such as colorectal cancer and breast cancer. It is produced by mixing uracil, fluorinating agents and alkylating agents. Through structural modification, the drug's targeting and stability have been improved, making it a hot topic in anticancer drug research and development.

[0003] In the existing technology for the synthesis of 5-fluorouracil (5-FU) derivatives, the mixing efficiency of uracil, fluorinating reagent and alkylating reagent directly affects the reaction rate and product quality. Traditional stirring devices such as paddle stirrers have poor mixing effect on solid and liquid reagents in the reaction vessel, which can easily lead to excessively high or low local concentrations, affecting the uniformity of the reaction. Furthermore, due to the low mixing efficiency, the reaction time is prolonged, which increases the risk of side reactions and reduces the product yield and purity.

[0004] In response to this technical problem, this application proposes an apparatus for synthesizing 5-fluorouracil derivatives. Utility Model Content

[0005] The purpose of this invention is to address the shortcomings of existing technologies by proposing a synthesis device for 5-fluorouracil derivatives. Through the synergistic effects of anisotropic mechanical shearing, forced convection, and dynamic temperature control, the device completely eliminates the local concentration gradient and temperature lag phenomena present in traditional stirring devices, ensuring uniform mixing in the reaction chamber. The device also uses a transfer block and traction plate to drive the screen to rotate periodically, discharging precipitates and facilitating centrifugal processing.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] An apparatus for synthesizing a 5-fluorouracil derivative includes a reaction chamber, a temperature control chamber fixedly connected to the outer wall of the reaction chamber, a thermostat installed on the inner wall of the temperature control chamber, a water pump installed at the bottom of the reaction chamber, a processing chamber fixedly connected to the bottom of the water pump, a motor fixedly connected to the top of the reaction chamber, a reciprocating lead screw fixedly connected to the drive end of the motor, a gear plate connected to the outer wall of the reciprocating lead screw via a reciprocating assembly, a driven gear meshing with the outer wall of the gear plate, a connecting column and a connecting pipe connected to the front end of the driven gear via a stirring assembly, a second motor fixedly connected to the bottom of the reaction chamber, a separation chamber connected to the drive end of the second motor via a separation assembly, a feed pipe fixedly connected to the bottom of the processing chamber, and a screen rotatably connected to the inner wall of the feed pipe via a filter assembly.

[0008] Furthermore, the reciprocating assembly includes a slider sleeved on the outer wall of the reciprocating lead screw. The outer wall of the slider is fixedly connected to the inner wall of the gear plate. The bottom end of the gear plate is slidably connected to the top of the reaction chamber. The top end of the gear plate and the outer diameter of the driven gear are meshed.

[0009] Furthermore, the stirring assembly includes a first bevel gear fixedly connected to the front end of the driven gear, and a second bevel gear fixedly connected to the top of both the connecting column and the connecting pipe. The outer diameters of the second bevel gear and the first bevel gear are meshed together.

[0010] Furthermore, a second stirring rack is fixedly connected to the outer wall of the connecting pipe, and a first stirring rack is fixedly connected to the bottom end of the connecting column.

[0011] Furthermore, an input chamber is fixedly connected to the top left side of the reaction chamber, and an output chamber is fixedly connected to the left end of the processing chamber and extends through it.

[0012] Furthermore, the separation assembly includes a drive gear fixedly connected to the second drive end of the motor, an internal gear ring fixedly connected to the top of the separation chamber, the inner diameter of the internal gear ring and the outer diameter of the drive gear being meshed, and the outer wall of the separation chamber being rotatably connected to the inner wall of the delivery chamber.

[0013] Furthermore, the filter assembly includes an electro-hydraulic cylinder fixedly connected to the inner wall of the feed pipe, and an adapter block is fixedly connected to the drive end of the electro-hydraulic cylinder.

[0014] Furthermore, the adapter block is rotatably connected to traction plates at both ends, and the opposite ends of the traction plates are rotatably connected to the opposite ends of the screen.

[0015] This utility model has the following beneficial effects:

[0016] 1. In this utility model, after the material is put into the reaction chamber by the input chamber, the motor is started to drive the reciprocating screw, which drives the gear plate to move back and forth through the slider, drives the driven gear to rotate forward and backward, and through the transmission of bevel gears one and two, the connecting pipe and the connecting column rotate synchronously in opposite directions, driving the stirring rack one and the stirring rack two to rotate in opposite directions, and combined with the temperature controller of the temperature control chamber, the reaction liquid is efficiently and uniformly mixed.

[0017] 2. In this utility model, after the water pump delivers the mixed solution to the separation chamber of the processing chamber, the motor drives the active gear to mesh with the internal gear ring, driving the separation chamber to rotate at high speed, centrifugally separating the effective components and impurities. When the separated liquid is discharged through the discharge pipe, the screen traps the sediment. The electric hydraulic cylinder drives the screen to rotate periodically through the transfer block and traction plate to discharge the sediment, facilitating the centrifugal processing of the device. Attached Figure Description

[0018] Figure 1This is a perspective view of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model;

[0019] Figure 2 This is a half-sectional view of the temperature control chamber of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model.

[0020] Figure 3 This is a half-sectional view of the reaction chamber of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model.

[0021] Figure 4 This is a half-sectional view of the connecting tube of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model;

[0022] Figure 5 This is a half-sectional view of the gear plate of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model;

[0023] Figure 6 This is a half-sectional view of the separation chamber of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model;

[0024] Figure 7 This is a half-sectional view of the feed tube of a synthesis apparatus for a 5-fluorouracil derivative proposed in this utility model.

[0025] Legend:

[0026] 1. Reaction chamber; 2. Temperature control chamber; 3. Motor 1; 4. Feeding chamber; 5. Processing chamber; 6. Dispensing chamber; 7. Gear plate; 8. Bevel gear 1; 9. Bevel gear 2; 10. Thermostat; 11. Connecting column; 12. Connecting pipe; 13. Separation chamber; 14. Internal gear ring; 15. Water pump; 16. Motor 2; 17. Drive gear; 18. Stirring rack 1; 19. Stirring rack 2; 20. Driven gear; 21. Reciprocating screw; 22. Sliding block; 23. Feeding pipe; 24. Electric hydraulic cylinder; 25. Adapter block; 26. Traction plate; 27. Screen. Detailed Implementation

[0027] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0028] Reference Figures 1-3This utility model provides an embodiment of a 5-fluorouracil derivative synthesis apparatus, comprising a reaction chamber 1, a temperature control chamber 2 fixedly connected to the outer wall of the reaction chamber 1, a thermostat 10 installed on the inner wall of the temperature control chamber 2, a water pump 15 installed at the bottom of the reaction chamber 1, a processing chamber 5 fixedly connected to the bottom of the water pump 15, a motor 3 fixedly connected to the top of the reaction chamber 1, a reciprocating screw 21 fixedly connected to the drive end of the motor 3, a gear plate 7 connected to the outer wall of the reciprocating screw 21 via a reciprocating assembly, a driven gear 20 meshing with the outer wall of the gear plate 7, a connecting column 11 and a connecting pipe 12 connected to the front end of the driven gear 20 via a stirring assembly, and a slider 22 sleeved on the outer wall of the reciprocating screw 21. (Refer to...) Figure 4 and Figure 5 The outer wall of the slider 22 is fixedly connected to the inner wall of the gear plate 7. The bottom end of the gear plate 7 is slidably connected to the top end of the reaction chamber 1. The top end of the gear plate 7 and the outer diameter of the driven gear 20 are meshed. The stirring assembly includes a bevel gear 8 fixedly connected to the front end of the driven gear 20. The top ends of the connecting column 11 and the connecting pipe 12 are both fixedly connected to bevel gears 9. The outer diameters of bevel gears 9 and 8 are meshed. The outer wall of the connecting pipe 12 is fixedly connected to a stirring rack 19. The bottom end of the connecting column 11 is fixedly connected to a stirring rack 18. The left side of the top end of the reaction chamber 1 is fixedly connected to an input chamber 4. The left end of the processing chamber 5 is fixedly connected to an input chamber 6 and passes through it.

[0029] Specifically: After the feed chamber 4 at reaction chamber 1 accurately feeds uracil, fluorinating reagent, and alkylating reagent into reaction chamber 1 according to a preset ratio, motor 3 is started. Motor 3 drives the reciprocating screw 21 to rotate at an adjustable speed of 0-200 rpm. The reciprocating screw 21, through its threaded groove and engagement with the slider 22, drives the slider 22 to reciprocate linearly along the screw axis, with a stroke range of ±50 mm and an adjustable frequency of 5-20 Hz. The slider 22 is fixed to the gear plate 7 through a rigid connecting piece, driving the gear plate 7 to reciprocate horizontally within reaction chamber 1. The reciprocating motion of the gear plate 7, through its rack structure meshing with the driven gear 20, causes the driven gear 20 to rotate periodically in both directions at a speed of ±15 rpm. The rotational power of the driven gear 20 is transmitted to the bevel gear 8 through the drive shaft. The bevel gear 8 and the bevel gear 9 mesh at a 90° orthogonal angle, converting the horizontal axial rotation into vertical axial power, driving the connecting pipe 12 (outer shaft) and the connecting column 11 (inner shaft) to rotate synchronously in opposite directions. The outer shaft rotates at 0-100 rpm, and the inner shaft rotates at 0-85 rpm, with opposite directions. The connecting column 11 and the connecting pipe 12 are connected by flanges, driving the stirring frame 18 (outer shaft stirrer) and the stirring frame 19 (inner shaft stirrer) to perform opposite circular motion. The stirring frame 18 adopts a three-bladed propeller design with a blade diameter of 200 mm and an inclination angle of 45°. The stirring frame 19 adopts an anchor frame structure with a gap of ≤5 mm between its outer edge and the inner wall of the reaction chamber 1. The opposite rotation of the two creates high-intensity shear force and convection circulation, enabling the high-viscosity mixture in the reaction chamber 1 to achieve uniform dispersion within 30 seconds. Meanwhile, the temperature controller 10 in the temperature control chamber 2 controls the jacket circulation system through a PID algorithm, using silicone oil as the heat transfer medium to achieve precise temperature control within the reaction chamber 1. The temperature control accuracy is ±0.5℃, and the heating and cooling rate is ≥5℃ / min, meeting the multi-mode requirements of the low-temperature stage of fluorination reaction (-10℃ to 0℃) and the high-temperature stage of alkylation reaction (60-80℃). This integrated stirring and temperature control system, through the synergistic effect of anti-directional mechanical shearing, forced convection, and dynamic temperature control, completely eliminates the local concentration gradient and temperature lag phenomena present in traditional stirring devices, enabling the mixture in the reaction chamber 1 to achieve molecular-level uniform mixing within 5 minutes. The lining of the reaction chamber 1 is made of Hastelloy C-276 nickel-based alloy and PTFE composite coating, which improves corrosion resistance by 3 times. The surfaces of stirring racks 18 and 19 are coated with tungsten carbide, with a hardness ≥1500HV and a wear resistance life ≥5000 hours. The reciprocating screw 21 is made of 40Cr alloy steel with a quenching process, and the transmission efficiency is ≥92%.

[0030] Reference Figure 6 and Figure 7A motor 16 is fixedly connected to the bottom of reaction chamber 1. The drive end of motor 16 is connected to separation chamber 13 via separation assembly. A feed pipe 23 is fixedly connected to the bottom of processing chamber 5. A screen 27 is rotatably connected to the inner wall of feed pipe 23 via filter assembly. Separation assembly includes drive gear 17 fixedly connected to the drive end of motor 16. An internal gear ring 14 is fixedly connected to the top of separation chamber 13. The inner diameter of internal gear ring 14 and the outer diameter of drive gear 17 are meshed. The outer wall of separation chamber 13 is rotatably connected to the inner wall of feeding chamber 6. Filter assembly includes electric hydraulic cylinder 24 fixedly connected to the inner wall of feed pipe 23. A transition block 25 is fixedly connected to the drive end of electric hydraulic cylinder 24. Traction plates 26 are rotatably connected to both ends of transition block 25. The opposite ends of traction plates 26 are rotatably connected to the opposite ends of screen 27.

[0031] Specifically: After the water pump 15 quantitatively delivers the mixed solution in reaction chamber 1 to separation chamber 13 in processing chamber 5 through a corrosion-resistant pipe, motor 16 (7.5kW, adjustable speed 0-3000rpm) is started. Motor 16 drives the drive gear 17 to mesh with the internal gear ring 14 via a coupling, causing separation chamber 13 to rotate at high speed of 8000rpm within processing chamber 5. The centrifugal force of separation chamber 13 causes beneficial components such as 5-fluorouracil derivatives in the mixture to separate from impurities. High-density active ingredients are deposited on the inner wall of separation chamber 13 under centrifugal force, while light phase impurities concentrate in the central area. After separation, the pneumatic valve at the bottom of processing chamber 5 is opened, and the separated liquid is discharged through discharge pipe 23. Discharge pipe 23 is embedded with a PTFE screen 27 with an adjustable pore size of 10-50μm and a filtration area of ​​0.5m². 2 The separated liquid undergoes precision filtration to retain solid precipitates with a particle size ≥10μm. An electric hydraulic cylinder 24, with a stroke of 200mm and a thrust of 5kN, is hinged to a traction plate 26 via an adapter block 25. The electric hydraulic cylinder 24, with a stroke of 200mm and a thrust of 5kN, drives the traction plate 26 to reciprocate along the axis of the feed pipe 23, causing the screen 27 to rotate periodically within the feed pipe 23. This mechanically scrapes off the precipitates adhering to the surface of the screen 27 and discharges them along the guide channel. The discharged wet material is then conveyed to the downstream section via a screw conveyor. The drying unit dries the product at 60-80℃ and a vacuum of -0.08MPa for 2-4 hours, ultimately obtaining 5-fluorouracil powder with a moisture content of ≤0.5%, which can be directly used for tableting or capsule filling. When the separation chamber 13 rotates at 8000rpm, the effective ingredient recovery rate is ≥95% and the impurity removal rate is ≥90%. The rotating cleaning mechanism of the screen 27 improves the filtration efficiency by 40%, avoiding the risk of metal contamination from traditional vibrating screens. The drying unit has a thermal efficiency of ≥85%, and its energy consumption is 35% lower than that of traditional drying ovens.

[0032] Working principle: After uracil, fluorinating reagent, and alkylating reagent are placed in reaction chamber 1 via loading chamber 4, motor 3 is started to drive reciprocating screw 21 to rotate. This reciprocating screw 21, through slider 22, drives gear plate 7 to reciprocate within reaction chamber 1. This causes driven gear 20 to rotate in both directions under the transmission of gear plate 7. Gear plate 7 then drives bevel gear 8 to drive bevel gear 9, causing connecting pipe 12 and connecting column 11 to rotate synchronously in opposite directions. This, in turn, drives stirring rack 18 and stirring rack 19 to perform circular motion, ensuring thorough mixing of the mixture within reaction chamber 1. The temperature is then regulated by thermostat 10 within temperature control chamber 2. The mixture in reaction chamber 1 is mixed evenly. Water pump 15 delivers the mixed solution to separation chamber 13 in processing chamber 5. Motor 16 drives drive gear 17 to rotate internal gear ring 14, causing separation chamber 13 to rotate at high speed in processing chamber 5. This separates the beneficial components in the mixture in separation chamber 13. After separation in separation chamber 13, the mixture is discharged through feed pipe 23. The screen 27 in feed pipe 23 filters out the separated precipitate. Electric hydraulic cylinder 24 drives transfer block 25 to pull traction plate 26 to stretch screen 27 to rotate in feed pipe 23, causing the precipitate filtered by screen 27 to be discharged and dried by subsequent drying device, making it convenient to make 5-fluorouracil into powder for use.

[0033] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. An apparatus for synthesizing a 5-fluorouracil derivative, comprising a reaction chamber (1), characterized in that: A temperature control chamber (2) is fixedly connected to the outer wall of the reaction chamber (1). A thermostat (10) is installed on the inner wall of the temperature control chamber (2). A water pump (15) is installed at the bottom of the reaction chamber (1). A processing chamber (5) is fixedly connected to the bottom of the water pump (15). A motor (3) is fixedly connected to the top of the reaction chamber (1). A reciprocating lead screw (21) is fixedly connected to the drive end of the motor (3). A gear plate (7) is connected to the outer wall of the reciprocating lead screw (21) through a reciprocating assembly. A driven gear (20) is meshed with the outer wall of the gear plate (7). The front end of the driven gear (20) is connected to a connecting column (11) and a connecting pipe (12) through a stirring assembly. A second motor (16) is fixedly connected to the bottom end of the reaction chamber (1). The driving end of the second motor (16) is connected to a separation chamber (13) through a separation assembly. A discharge pipe (23) is fixedly connected to the bottom end of the processing chamber (5). A screen (27) is rotatably connected to the inner wall of the discharge pipe (23) through a filter assembly.

2. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 1, characterized in that: The reciprocating assembly includes a slider (22) sleeved on the outer wall of the reciprocating lead screw (21). The outer wall of the slider (22) is fixedly connected to the inner wall of the gear plate (7). The bottom end of the gear plate (7) is slidably connected to the top end of the reaction chamber (1). The top end of the gear plate (7) and the outer diameter of the driven gear (20) are meshed.

3. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 1, characterized in that: The stirring assembly includes a bevel gear one (8) fixedly connected to the front end of the driven gear (20), and a bevel gear two (9) fixedly connected to the top ends of the connecting column (11) and the connecting pipe (12). The outer diameters of the bevel gear two (9) and the bevel gear one (8) are meshed.

4. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 1, characterized in that: The outer wall of the connecting pipe (12) is fixedly connected to a second stirring rack (19), and the bottom end of the connecting column (11) is fixedly connected to a first stirring rack (18).

5. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 1, characterized in that: The reaction chamber (1) is fixedly connected to the left side of the top end of the feed chamber (4), and the processing chamber (5) is fixedly connected to the left end of the feed chamber (6) and passes through it.

6. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 1, characterized in that: The separation assembly includes a drive gear (17) fixedly connected to the drive end of motor 2 (16), an internal gear ring (14) fixedly connected to the top of the separation chamber (13), the inner diameter of the internal gear ring (14) and the outer diameter of the drive gear (17) are meshed, and the outer wall of the separation chamber (13) is rotatably connected to the inner wall of the delivery chamber (6).

7. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 1, characterized in that: The filter assembly includes an electric hydraulic cylinder (24) fixedly connected to the inner wall of the feed pipe (23), and an adapter block (25) is fixedly connected to the drive end of the electric hydraulic cylinder (24).

8. The apparatus for synthesizing a 5-fluorouracil derivative according to claim 7, characterized in that: The adapter block (25) is rotatably connected to traction plates (26) at both ends, and the opposite ends of the traction plates (26) are rotatably connected to the opposite ends of the screen (27).

Images