Composite stirring device for levofloxacin lactate synthesis

Abstract

The utility model stirring device technical field especially relates to composite stirring device for levofloxacin ester synthesis, including be used for the stirring tank of levofloxacin ester synthesis stirring processing, the sealing cover plate for protecting inside is provided with in the top of stirring tank buckling, the filling pipe for filling levofloxacin ester synthesis material is connected with the top symmetry of sealing cover plate, the vibration subassembly for preventing side wall adhesion to carry out acceleration composite stirring is equipped with in stirring tank, the bottom of stirring tank is connected with several groups of drain pipe in ring, through ultrasonic vibration and multistage stirring combination, make high viscosity material form global circulation flow in tank, eliminate corner dead zone in traditional device, carry out pre -crushing raw material agglomeration with filter plate, whip conductive strip to scatter bubble, spiral shear leaf intensifies mass transfer, scraper removes wall surface residue, improves overall reaction efficiency, the ultrasonic module of vibration subassembly makes kettle wall shear stress to be promoted, eliminates high viscosity material dead zone scraper and can with material viscosity adaptive deflection, increase overall stirring effect.

Description

Technical Field

[0001] This utility model relates to the field of stirring device technology, and in particular to a composite stirring device for the synthesis of levofluorocycloesters. Background Technology

[0002] Levofloxacin cyclase is a key intermediate in the synthesis of levofloxacin (a third-generation fluoroquinolone antibacterial drug). It is a direct precursor for the synthesis of levofloxacin. Through precise synthesis and purification processes, levofloxacin cyclase provides a core guarantee for the efficient and low-toxicity production of levofloxacin. In the synthesis process of levofloxacin cyclase, composite stirring refers to the multi-dimensional mixing operation of the reaction system by combining different types of stirrers (such as paddle, turbine, anchor, etc.) or combining them with airflow stirring. This optimizes material contact efficiency and ensures the uniformity and stability of the synthesis reaction.

[0003] Traditional oxyfluorine cyclization ester synthesis uses a multi-layer paddle stirrer. During the stirring process, high-viscosity materials form dead zones in the corners of the reactor, resulting in incomplete local reactions. Oxygen can easily seep into the mechanical seal, causing ester oxidation and deterioration, and reducing the overall stirring effect. Utility Model Content

[0004] To overcome the problems of traditional stirring devices where high-viscosity materials form dead zones in the corners of the reactor, leading to incomplete local reactions and easy oxygen infiltration into the mechanical seal, resulting in ester oxidation and deterioration, this invention provides a composite stirring device for the synthesis of levofluorocyclic esters.

[0005] The technical solution is as follows: A composite stirring device for the synthesis of levofluorocycloesters includes a stirring tank for the synthesis and stirring of levofluorocycloesters. A sealing cover plate for protecting the interior is fastened to the top of the stirring tank. A filling pipe for adding levofluorocycloester synthesis materials is symmetrically connected to the top of the sealing cover plate. A vibration component for accelerating composite stirring and preventing side wall adhesion is provided on the stirring tank. Several sets of drain pipes are circumferentially connected to the bottom of the stirring tank.

[0006] Furthermore, the mixing tank is covered with a heat insulation sleeve, and several sets of brackets are fixedly connected to the bottom of the mixing tank in a circumferential manner. Several sets of drainage holes corresponding to the drainage pipes are opened on the bottom of the inner side of the mixing tank. A mounting base is fixedly connected to the center of the bottom of the mixing tank, and a rotary joint is connected to the center of the top of the mounting base. The side wall of the mixing tank is coated with an anti-corrosion coating.

[0007] Furthermore, a fixed sleeve is fixedly connected to the center of the sealing cover, a rotating rod is inserted through the center of the fixed sleeve, a drive motor is fixedly connected to the top of the rotating rod, and a snap hole is opened at the bottom of the rotating rod to mate with the rotating joint.

[0008] Furthermore, several sets of guide rods are circumferentially fixed to the rotating rod near the sealing cover plate. A filter plate is fixed to the guide rod away from the rotating rod. Several filter holes are distributed on the filter plate. A crushing block is fixed to the outer edge of the filter plate.

[0009] Furthermore, several sets of whip-like conductive strips are circumferentially fixed to the middle of the rotating rod, and a spiral shearing blade is fixed to the rotating rod below the whip-like conductive strips. Several sets of scrapers are circumferentially fixed to the rotating rod near the bottom, and a shovel plate is integrally formed at the bottom of the scraper. Two sets of extension rods are connected to the side end of the spiral shearing blade on the rotating rod. Scraper bars are fixed to the extension rods away from the rotating rod. The drive motor drives the rotating rod to sequentially rotate the filter plate, whip-like conductive strips, spiral shearing blades, scraper bars, and scraper plates.

[0010] Furthermore, a conduit is provided below the filling pipe, and a pressure-bearing collision sleeve is provided between the conduit and the filling pipe. A spring rubber damping layer is provided on the inner side of the pressure-bearing collision sleeve. A reinforcement hole is provided through the conduit, and a solenoid valve module is provided inside the conduit. A sealing sleeve is provided on the outside of the filling pipe.

[0011] Furthermore, the vibration assembly includes two sets of linearly arranged rings, with a control board connected to the outer ends of the two sets of rings. The control board has a control display screen at its center. An ultrasonic module is embedded in the mixing tank and electrically connected to the control display screen on the inner side of the two sets of rings. The ultrasonic module includes a conductive ball, an ultrasonic transmitter, an ultrasonic receiver, and a lithium battery pack that are electrically connected to each other.

[0012] Furthermore, a conveying pipe is fixedly connected to the end of the drain pipe away from the mixing tank, and a control valve is provided between the conveying pipe and the drain pipe.

[0013] The beneficial effects are: This utility model combines ultrasonic vibration with multi-stage stirring to form a full-area circulation flow of high-viscosity materials in the tank, eliminating dead zones in corners in traditional devices, pre-crushing raw material agglomeration by filter plates, breaking up bubbles by whipping conduction strips, enhancing mass transfer by spiral shear blades, and removing residues from the wall by scrapers, thereby improving the overall reaction efficiency.

[0014] The ultrasonic module of the vibration assembly enhances the shear stress of the vessel wall, eliminates dead zones in high-viscosity materials, and allows the scraper to deflect adaptively according to the material viscosity, reducing mechanical wear and increasing the overall stirring effect. Attached Figure Description

[0015] Figure 1 This is a three-dimensional schematic diagram of the composite stirring device for the synthesis of levofluorocycloesters according to the present invention.

[0016] Figure 2 This is a schematic diagram of the mixing tank of this utility model;

[0017] Figure 3 This is a schematic diagram of the sealing cover and filling pipe of this utility model;

[0018] Figure 4 This is a schematic diagram of the filling tube of this utility model from another angle;

[0019] Figure 5 This is a schematic diagram of the vibration component of this utility model.

[0020] In the attached diagram, the following are the reference numerals: 1. Mixing tank; 2. Sealing cover; 3. Filling pipe; 4. Vibration assembly; 5. Drain pipe; 101. Insulation sleeve; 102. Mounting chassis; 103. Bracket; 104. Drain hole; 105. Anti-corrosion coating; 106. Rotary joint; 201. Rotating rod; 202. Fixing sleeve; 203. Drive motor; 204. Whip conduction strip; 205. Spiral shear blade; 206. Scraper; 207. Extension rod; 208. Scraper; 209. Shovel plate; 210. Filter plate; 211. Crushing block; 212. Filter hole; 213. Guide rod; 301. Pressure-bearing impact sleeve; 302. Conduit; 303. Sealing sleeve; 304. Reinforcement hole; 305. Solenoid valve module; 401. Control board; 402. Control display screen; 403. Ultrasonic module; 501. Delivery pipe; 502. Control valve. Detailed Implementation

[0021] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0022] like Figure 1 - Figure 5 As shown, the composite stirring device for the synthesis of levofluorocyclohexane includes a stirring tank 1 for stirring treatment in the synthesis of levofluorocyclohexane. A sealing cover 2 for protecting the interior is fastened to the top of the stirring tank 1. A filling pipe 3 for adding levofluorocyclohexane synthesis material is symmetrically connected to the top of the sealing cover 2. A vibration component 4 is provided on the stirring tank 1 to accelerate composite stirring and prevent side wall adhesion. Several sets of drain pipes 5 are circumferentially connected to the bottom of the stirring tank 1.

[0023] Please see Figure 2 - Figure 4 In this embodiment, the mixing tank 1 is covered with a heat insulation sleeve 101. Several sets of brackets 103 are fixedly connected to the bottom of the mixing tank 1 in a circumferential direction. Several sets of drainage holes 104 corresponding to the drainage pipes 5 are opened on the bottom inner side of the mixing tank 1. A mounting base 102 is fixedly connected to the center of the bottom of the mixing tank 1. A rotary joint 106 is connected to the center of the top of the mounting base 102. The side wall of the mixing tank 1 is coated with an anti-corrosion coating 105. A fixing sleeve 202 is fixedly connected to the center of the sealing cover plate 2. A rotating rod 201 passes through the center of the fixing sleeve 202. A drive motor 203 is fixedly connected to the top of the rotating rod 201. A locking hole for docking with the rotary joint 106 is opened at the bottom of the rotating rod 201.

[0024] Please see Figure 3 - Figure 4In this embodiment, several sets of guide rods 213 are circumferentially fixed to the rotating rod 201 near the sealing cover plate 2. A filter plate 210 is fixed to the guide rods 213 away from the rotating rod 201. The filter plate 210 has several sets of filter holes 212 distributed on it (which also function as an oxygen barrier; the filter holes 212 (conical design) reduce gas backmixing). Crushing blocks 211 are fixed along the outer edge of the filter plate 210. Several sets of whipping conduction strips 204 are circumferentially fixed to the middle of the rotating rod 201. The rotating rod 201 is located on the whipping conduction strips 204... 04. A spiral shearing blade 205 is fixedly connected below. Several sets of scrapers 208 are fixedly connected around the bottom of the rotating rod 201. A shovel 209 is integrally formed at the bottom of the scraper 208. Two sets of extension rods 207 are connected to the side of the spiral shearing blade 205 on the rotating rod 201. A scraper 206 is fixedly connected to the extension rod 207 away from the rotating rod 201. The drive motor 203 drives the rotating rod 201 to drive the filter plate 210, the whipping guide strip 204, the spiral shearing blade 205, the scraper 206 and the scraper 208 to rotate in sequence.

[0025] Please see Figure 4 - Figure 5 In this embodiment, a conduit 302 is provided below the filling pipe 3, and a pressure-bearing collision sleeve 301 is provided between the conduit 302 and the filling pipe 3. A spring rubber damping layer is provided on the inner side of the pressure-bearing collision sleeve 301. A reinforcement hole 304 is provided through the conduit 302. An oxygen sensor and a nitrogen purging device are integrated at the mechanical seal to form a dynamic protection barrier. A solenoid valve module 305 is provided inside the conduit 302. A sealing sleeve 303 is provided on the outside of the filling pipe 3. The vibration component 4 includes two sets of linearly arranged rings (the rings are embedded with piezoelectric ceramic vibrators (diameter 20mm), and the conductive balls (zirconia material) are in close contact with the vessel wall to transmit ultrasonic waves). The outer ends of the two sets of rings are connected to a control board 401. The center of the control board 401 is provided with The control display screen 402 has an ultrasonic module 403 embedded in the inner side of the two ring sleeves and electrically connected to the control display screen 402. The ultrasonic module 403 includes a conductive ball, an ultrasonic transmitter, an ultrasonic receiver, and a lithium battery pack that are electrically connected to each other. The lithium battery pack (24V / 10Ah) supports continuous operation for 48 hours. The control display screen 402 sets the pulse period. The drain pipe 5 is fixed to a delivery pipe 501 at the end away from the mixing tank 1. A control valve 502 is provided between the delivery pipe 501 and the drain pipe 5. Levofloxacin cyclized ester is synthesized in a 500L reactor with a product yield of 92.5% (82.1% with conventional equipment), an acid value of <0.1mgKOH / g, and a batch-to-batch deviation of <0.3%.

[0026] The synthetic raw materials are injected into the mixing tank 1 through the injection pipe 3. The solenoid valve module 305 (model: 2W-160-15) in the conduit 302 precisely controls the flow rate. The pressure-bearing collision sleeve 301 (with built-in fluororubber damping layer) buffers pressure fluctuations to ensure a smooth injection process.

[0027] After the material enters, the filter plate 210 (made of 316L stainless steel with a pore size of 2mm) disperses the raw material into fine streams through the filter holes 212. The guide rod 213 driven by the rotating rod 201 drives the filter plate 210 to rotate (the speed is adjustable from 0 to 500 rpm), thus achieving preliminary radial mixing.

[0028] Upper layer shearing: Whip conduction strip 204 (304 stainless steel, surface coated with polytetrafluoroethylene) uses high-frequency vibration (frequency 20-50Hz) to turbulently disturb the material and destroy the surface tension of the liquid;

[0029] Intermediate mixing: The spiral shear blade 205 (pitch ratio 1:1.5) generates axial flow, which, together with the scraper 206 (silicone material, Shore A60 hardness) on the extension rod 207, scrapes the residual material on the tank wall to prevent adhesion;

[0030] Bottom layer anti-settling: The scraper 208 and the bottom shovel 209 (with a gap of ≤1mm from the bottom of the tank) fit against the bottom curved surface of the mixing tank 1, and the rotating rod 201 driven by the rotary joint 106 (model: KF-16) rotates at a low speed (10-30rpm) to thoroughly remove the sediment;

[0031] The vibration component 4 emits ultrasonic waves through the ultrasonic module 403 (model: HY-25D, frequency 25kHz), and the conduction ball (made of tungsten steel) transmits the vibration to the tank. Combined with the linear layout of the ring sleeve (linear spacing 50mm), the material inside the tank generates micron-level amplitude vibration, eliminating the accumulation of high-viscosity materials in the corners.

[0032] The mechanical seal is equipped with a nitrogen protection system (nitrogen flow rate adjustable from 0-5L / min). The oxygen content is monitored in real time by an oxygen sensor (model: Alphasense OX-B431) embedded in the sealing cover plate 2 to ensure that the oxygen concentration in the reaction environment is ≤1ppm.

[0033] The insulation jacket 101 (made of rock wool) maintains a stable temperature inside the tank, and the temperature sensor (PT100, accuracy ±0.1℃) feeds back to the control display screen 402 to achieve PID closed-loop control.

[0034] After the reaction is complete, the drain hole 104 is opened by the control valve 502 (ball valve, DN25 specification), and the material is transported to the next process through the drain pipe 5. Residue is completely discharged through the combined action of the scraper 208 and the shovel 209.

[0035] The above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. 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. A complex stirring device for the synthesis of levofloxacin lactate, characterized by: The mixture includes a mixing tank (1) for the synthesis and stirring of levofluorocycloesters. The top of the mixing tank (1) is fitted with a sealing cover (2) for protecting the interior. The top of the sealing cover (2) is symmetrically connected with a filling pipe (3) for adding levofluorocycloester synthesis materials. The mixing tank (1) is equipped with a vibration assembly (4) to prevent sidewall adhesion and accelerate the composite stirring. The bottom of the mixing tank (1) is circumferentially connected with several sets of drain pipes (5).

2. The complex agitating device for the synthesis of levofloxacin ester according to claim 1, characterized in that, The mixing tank (1) is covered with a heat insulation sleeve (101). Several sets of brackets (103) are fixedly connected to the bottom of the mixing tank (1) in a circumferential direction. Several sets of drainage holes (104) corresponding to the drainage pipes (5) are opened on the bottom of the inner side of the mixing tank (1). A mounting base (102) is fixedly connected to the center of the bottom of the mixing tank (1). A rotary joint (106) is connected to the center of the top of the mounting base (102). The side wall of the mixing tank (1) is coated with an anti-corrosion coating (105).

3. The complex agitator for the synthesis of levofloxacin ester according to claim 2, characterized in that, A fixed sleeve (202) is fixedly connected to the center of the sealing cover plate (2). A rotating rod (201) is inserted through the center of the fixed sleeve (202). A drive motor (203) is fixedly connected to the top of the rotating rod (201). A snap hole is opened at the bottom of the rotating rod (201) to mate with the rotating joint (106).

4. The complex stirring device for the synthesis of levofloxacin ester according to claim 3, characterized in that, Several sets of guide rods (213) are fixedly connected around the rotating rod (201) near the sealing cover plate (2). A filter plate (210) is fixedly connected to the guide rods (213) away from the rotating rod (201). Several filter holes (212) are distributed on the filter plate (210). A crushing block (211) is fixedly connected along the outer edge of the filter plate (210).

5. The complex agitating device for the synthesis of levofloxacin ester according to claim 3, characterized in that, Several sets of whipping conduction strips (204) are fixedly connected to the middle of the rotating rod (201). A spiral shearing blade (205) is fixedly connected to the rotating rod (201) below the whipping conduction strips (204). Several sets of scrapers (208) are fixedly connected to the rotating rod (201) near the bottom. A shovel plate (209) is integrally formed at the bottom of the scraper (208). Two sets of extension rods (207) are connected to the side of the spiral shearing blade (205) on the rotating rod (201). A scraper (206) is fixedly connected to the extension rod (207) away from the rotating rod (201). The drive motor (203) drives the rotating rod (201) to drive the filter plate (210), whipping conduction strips (204), spiral shearing blades (205), scraper (206) and scraper (208) to rotate in sequence.

6. The complex agitating device for the synthesis of levofloxacin ester according to claim 1, characterized in that, Below the filling tube (3) is a conduit (302), and between the conduit (302) and the filling tube (3) is a pressure-bearing collision sleeve (301). The inner side of the pressure-bearing collision sleeve (301) is provided with a spring rubber damping layer. A reinforcing hole (304) is opened through the conduit (302). A solenoid valve module (305) is provided inside the conduit (302). A sealing sleeve (303) is fitted on the outside of the filling tube (3).

7. The complex agitating device for the synthesis of levofloxacin ester according to claim 1, characterized in that, The vibration assembly (4) includes two sets of linearly arranged rings. The outer ends of the two sets of rings are connected to a control board (401). The center of the control board (401) is provided with a control display screen (402). The inner sides of the two sets of rings are provided with an ultrasonic module (403) that is embedded in the mixing tank (1) and electrically connected to the control display screen (402). The ultrasonic module (403) includes a conductive ball, an ultrasonic transmitter, an ultrasonic receiver and a lithium battery pack that are electrically connected to each other.

8. The composite stirring apparatus for synthesizing levofluorocycloesters according to claim 1, characterized in that, A conveying pipe (501) is fixedly connected to one end of the drain pipe (5) away from the mixing tank (1), and a control valve (502) is provided between the conveying pipe (501) and the drain pipe (5).

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