CN113877242B - A purification system for producing chiral medicine - Google Patents
A purification system for producing chiral medicine Download PDFInfo
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- CN113877242B CN113877242B CN202111163739.0A CN202111163739A CN113877242B CN 113877242 B CN113877242 B CN 113877242B CN 202111163739 A CN202111163739 A CN 202111163739A CN 113877242 B CN113877242 B CN 113877242B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0492—Applications, solvents used
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0426—Counter-current multistage extraction towers in a vertical or sloping position
- B01D11/0434—Counter-current multistage extraction towers in a vertical or sloping position comprising rotating mechanisms, e.g. mixers, rotational oscillating motion, mixing pumps
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0063—Control or regulation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C2/00—Crushing or disintegrating by gyratory or cone crushers
- B02C2/10—Crushing or disintegrating by gyratory or cone crushers concentrically moved; Bell crushers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B11/00—Machines or apparatus for drying solid materials or objects with movement which is non-progressive
- F26B11/12—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices
- F26B11/14—Machines or apparatus for drying solid materials or objects with movement which is non-progressive in stationary drums or other mainly-closed receptacles with moving stirring devices the stirring device moving in a horizontal or slightly-inclined plane
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/04—Agitating, stirring, or scraping devices
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Abstract
The invention discloses a purification system for producing chiral drugs, which comprises an extraction crystallization device and a drying cold grinding device connected with a discharge port of the extraction crystallization device, wherein a separation liquid outlet of the extraction crystallization device is connected with a self-cleaning centrifugal impurity removal device. The invention realizes the purposes of quickly and fully contacting the reaction solution with the extraction liquid and displacing the chiral drug, and simultaneously reducing the investment of equipment and personnel in the processes of impurity removal, drying and grinding. The invention is suitable for the technical field of chiral drug production equipment.
Description
Technical Field
The invention belongs to the technical field of chiral drug production equipment, and particularly relates to a purification system for producing chiral drugs.
Background
In the process for producing chiral drugs, most of the chiral drugs need to be extracted from the reaction solution, so that the subsequent separation conditions of the chiral drugs and the extraction solution are easier. In the existing extraction process, because the reaction liquid and the extraction liquid are required to be in full contact so as to be convenient for fully replacing the chiral medicine, the density is time-consuming to realize, the mixing sufficiency cannot be ensured, the extraction liquid and the reaction liquid are difficult to separate after layering, and the general difficulty lies in that the layering position often fluctuates, so that a part of the reaction liquid is doped and is extracted from a reaction kettle in the extraction process of the extraction liquid. In addition, impurities in the reaction liquid or the extraction liquid which is finally obtained at present need to be removed, the long-used equipment at present is an impurity removing machine, the input cost of the impurity removing machine is high, and the impurity removing efficiency is high. After the chiral drug is crystallized, a drying cylinder is generally adopted for drying, and then a grinding machine is used for grinding after drying, so that the investment of equipment and personnel is increased.
Disclosure of Invention
The invention provides a purification system for producing chiral drugs, which is used for quickly and fully contacting a reaction liquid with an extraction liquid and displacing the chiral drugs, and simultaneously, the purpose of reducing the investment of equipment and personnel in the processes of impurity removal, drying and grinding is achieved.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
the utility model provides a purification system for producing chiral medicine, includes extraction crystallization device and the dry cold grinding device of being connected with this extraction crystallization device's bin outlet, extraction crystallization device's separation liquid outlet is connected with self-cleaning formula centrifugation edulcoration device.
Further, the extraction crystallization device is including placing the mixed extraction mechanism in the extraction cauldron in, the mixed extraction mechanism rotates with the extraction cauldron to be connected, and in the extraction liquid got into the extraction cauldron through mixed extraction mechanism, be equipped with heating mechanism in the extraction cauldron overcoat, and the extraction cauldron communicates outward and has the liquid level pipe.
Further, the mixed extraction mechanism comprises a hole cylinder, wherein the upper end and the lower end of the hole cylinder respectively extend out of the extraction kettle and are rotatably connected with the extraction kettle, a first liquid injection and drainage unit and a second liquid injection and drainage unit are arranged in the hole cylinder, the first liquid injection and drainage unit and the second liquid injection and drainage unit are driven by a power motor connected with the second liquid injection and drainage unit to rotate, the hole cylinder synchronously rotates along with the first liquid injection and drainage unit and the second liquid injection and drainage unit, a scraping and guiding claw is arranged at the lower part of the hole cylinder and is contacted with the lower wall of the inner wall of the corresponding position of the extraction kettle, the lower wall of the extraction kettle is provided with an annular blanking groove which is sunken downwards, and a crystallization discharge joint is constructed at the lower end of the extraction kettle and the position of the annular blanking groove.
Further, first notes flowing back unit includes that one end is along the vertical first pipe that stretches into a hole section of thick bamboo by the upper end of extraction cauldron, in the lower extreme intercommunication of first pipe has first piston, and first pipe is through first piston and the inside intercommunication of a hole section of thick bamboo, and rotate on the position that first pipe is located the extraction cauldron outside and install first conducting terminal, the sliding seat is installed to first pipe upper end, the sliding seat is installed on the slide rail and through first cylinder drive and along vertical motion.
Furthermore, the second liquid injection and drainage unit comprises a second guide pipe, one end of the second guide pipe vertically extends into the hole cylinder from the lower end of the extraction kettle, a second piston is communicated with the upper end of the second guide pipe, the second guide pipe is communicated with the inside of the hole cylinder through the second piston, a second conduction joint is rotatably arranged on the part, located outside the extraction kettle, of the second guide pipe, and the lower end of the second guide pipe is connected with a power motor.
Furthermore, the aperture of the through hole fully distributed on the hole cylinder is gradually decreased from top to bottom, a drainage impeller is detachably mounted on the outer wall of the hole cylinder, the drainage impeller comprises a fixed disk with an internal connection edge, the internal connection edge is detachably connected with the outer wall of the hole cylinder, a plurality of drainage blades are uniformly constructed on the fixed disk along the circumferential direction of the fixed disk, drainage flanges are formed on two sides of each drainage blade respectively, a flow stabilizing disk is arranged below the drainage impeller and close to the drainage impeller, the flow stabilizing disk is provided with an external connection edge detachably connected with the inner wall of the extraction kettle, a plurality of overflowing channels are formed in the flow stabilizing disk, and when liquid in the extraction kettle is layered, the drainage blades correspond to the overflowing channels.
Further, dry cryomilling device is including the dry cryomilling cauldron that has the feeding joint, in dry cryomilling cauldron internal rotation is connected with the rabbling mechanism that adjusts the temperature, in the lower extreme of rabbling mechanism that adjusts the temperature is constructed and is ground the piece, in the lower extreme of dry cryomilling cauldron just is located to grind the piece department and sets up a plurality of unloading holes that evenly set up along dry cryomilling cauldron's circumference, in outside the dry cryomilling cauldron just be located unloading hole department swing joint and be used for opening and close the cover of opening and close of unloading hole.
Further, the rabbling mechanism adjusts the temperature is constructed the rotatory assembly body of medium outlet pipe and medium inlet pipe respectively including upper and lower both ends, the grinding piece has the first medium chamber with medium inlet pipe intercommunication, the upper portion of rotatory assembly body is constructed the second medium chamber with medium outlet pipe intercommunication, installs the stirring pipe that adjusts the temperature uniformly along its circumference outside the rotatory assembly body, the stirring pipe that adjusts the temperature is along vertical circuitous extension of buckling, and the both ends of stirring pipe that adjusts the temperature communicate with first medium chamber and second medium chamber respectively, it is connected with medium import adapter and medium outlet adapter to rotate respectively on the position that dry cold grinding cauldron is stretched out to medium inlet pipe and medium outlet pipe, installs the drive wheel on medium inlet pipe.
Furthermore, the lower end of the drying and cold-milling kettle is constructed into a horn-shaped milling shell which is reduced downwards, the milling part is a conical milling body matched with the milling shell, the lower end of the drying and cold-milling kettle is constructed into a connecting cylinder, the lower part of the opening and closing cover is constructed into an adjusting sleeve which is sleeved on the outer wall of the connecting cylinder and is in threaded connection with the connecting cylinder, and the outer wall of the adjusting sleeve is uniformly provided with a plurality of operating handles along the circumferential direction.
Furthermore, the self-cleaning centrifugal impurity removing device comprises a centrifugal mechanism which is arranged in the centrifugal kettle in a rotating way and is connected with the centrifugal kettle in a rotating way, the centrifugal mechanism comprises a centrifugal net cylinder, the lower end of the centrifugal net cylinder is connected with the centrifugal kettle in a rotating way, a discharge joint is constructed at the lower end of the centrifugal kettle, the upper end of the centrifugal net cylinder extends out of the centrifugal kettle and is communicated with a separation liquid outlet through a quick joint, a plurality of annular elastic baffles are arranged in the centrifugal net cylinder along the vertical direction of the centrifugal net cylinder, the outer edge of each annular elastic baffle is fixedly connected with the inner wall of the centrifugal net cylinder, the inner edge of each annular elastic baffle is connected with an adjusting rod through a plurality of connecting rods, the adjusting rod is superposed with the axis of the centrifugal net cylinder, a pipe body extending out of the centrifugal kettle is connected with the lower end of the adjusting rod, the position of the pipe body in the centrifugal kettle is communicated with the centrifugal net cylinder, and the position of the pipe body extending out of the centrifugal kettle is rotatably connected with a slag discharge adapter, and the lower extreme of body is connected with driving motor, and driving motor drives and can follow vertical action through the second cylinder.
Due to the adoption of the structure, compared with the prior art, the invention has the technical progress that: an operator injects reaction liquid into the extraction crystallization device, after the preset liquid level is reached, the extraction liquid is injected into the extraction crystallization device, the extraction liquid and the reaction liquid are fully contacted and mixed in the injection process of the extraction liquid, so that chiral drugs in the reaction liquid are replaced into the extraction liquid, then the reaction liquid is discharged out of the extraction crystallization device, the extraction liquid is evaporated in the extraction crystallization device in a heating mode, the chiral drugs are gradually separated out, the extraction liquid is evaporated and additionally collected, and then the crystallized chiral drugs are dried and cold-milled; the drying and cold-milling device heats and dries the chiral drug crystal, and after drying is finished, the temperature is reduced for grinding, so that the particle size of the crystal particles reaches a preset size, and then the crystal particles are discharged out of the drying and cold-milling device; the reaction liquid or the extraction liquid for separating the chiral medicine enters a self-cleaning type centrifugal impurity removal device, the self-cleaning type centrifugal impurity removal device separates impurities in the reaction liquid or the extraction liquid, when dirty and blocked, self-cleaning can be carried out to remove the impurities, and then separation operation is carried out; in conclusion, the invention realizes the purposes of quickly and fully contacting the reaction liquid with the extraction liquid and displacing the chiral drug, and simultaneously reduces the investment of equipment and personnel in the processes of impurity removal, drying and grinding.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a schematic structural diagram of an extraction crystallization apparatus according to an embodiment of the present invention;
FIG. 2 is a sectional view showing an axial structure of an extraction crystallization apparatus according to an embodiment of the present invention;
FIG. 3 is a schematic view of a mixing and extracting mechanism according to an embodiment of the present invention;
FIG. 4 is a schematic structural diagram of a first liquid injection and discharge unit according to an embodiment of the present invention;
FIG. 5 is a schematic structural diagram of a second liquid injection and discharge unit according to an embodiment of the present invention;
FIG. 6 is a schematic structural diagram of a flow stabilizing disc according to an embodiment of the present invention;
FIG. 7 is a schematic structural view of a flow-inducing impeller according to an embodiment of the present invention;
FIG. 8 is a schematic structural diagram of a drying and cold-milling apparatus according to an embodiment of the present invention;
FIG. 9 is a partial sectional structural view of a drying and cold-milling apparatus according to an embodiment of the present invention;
FIG. 10 is a partial cross-sectional structural view of a dry cryomilling kettle according to an embodiment of the present invention;
FIG. 11 is a schematic structural diagram of a temperature-regulating stirring mechanism according to an embodiment of the present invention;
FIG. 12 is an axial structural sectional view of a self-cleaning centrifugal impurity removing apparatus according to an embodiment of the present invention;
FIG. 13 is a partial structural cross-sectional view of a centrifugal mechanism in accordance with an embodiment of the present invention;
FIG. 14 is an axial structural section view of a centrifugal mechanism according to an embodiment of the invention.
Labeling components: 100-extraction kettle, 101-annular charging chute, 102-crystallization discharge joint, 103-liquid level pipe, 104-heating mechanism, 105-first heat medium joint, 106-steady flow disc, 107-overflowing channel, 108-external connecting edge, 109-scraping guide claw, 110-second heat medium joint, 200-hole cylinder, 201-first piston, 202-first guide pipe, 203-first conducting joint, 204-sliding seat, 205-second piston, 206-second guide pipe, 207-second conducting joint, 208-output shaft, 209-first limiting groove, 210-second limiting groove, 211-guide impeller, 212-fixed disc, 213-guide flanging, 214-internal connecting edge, 300-drying cold grinding kettle, 301-grinding shell, 302-blanking hole, 303-connecting cylinder, 304-opening and closing cover, 305-adjusting sleeve, 306-operating handle, 307-feeding joint, 400-rotating assembly body, 401-medium inlet pipe, 402-medium inlet adapter, 403-grinding piece, 404-first medium cavity, 405-temperature adjusting stirring pipe, 406-driving wheel, 407-second medium cavity, 408-medium outlet pipe, 409-medium outlet adapter, 500-centrifugal kettle, 501-discharging adapter, 600-centrifugal net cylinder, 601-adjusting rod, 602-pipe body, 603-deslagging hole, 604-annular elastic baffle, 605-connecting rod, 606-deslagging adapter.
Detailed Description
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. It should be understood that the preferred embodiments described herein are for purposes of illustration and explanation only and are not intended to limit the present invention.
The invention discloses a purification system for producing chiral drugs, which comprises an extraction crystallization device, a drying cold grinding device and a self-cleaning centrifugal impurity removal device, wherein the drying cold grinding device is connected with a discharge port of the extraction crystallization device, and a separation liquid outlet of the extraction crystallization device is connected with an inlet of the self-cleaning centrifugal impurity removal device, as shown in figures 1-14. The working principle and the advantages of the invention are as follows: an operator injects reaction liquid into the extraction crystallization device, after the preset liquid level is reached, the extraction liquid is injected into the extraction crystallization device, the extraction liquid and the reaction liquid are fully contacted and mixed in the injection process of the extraction liquid, so that chiral drugs in the reaction liquid are replaced into the extraction liquid, then the reaction liquid is discharged out of the extraction crystallization device, the extraction liquid is evaporated in the extraction crystallization device in a heating mode, the chiral drugs are gradually separated out, the extraction liquid is evaporated and additionally collected, and then the crystallized chiral drugs are dried and cold-milled; the drying and cold-milling device heats and dries the chiral drug crystal, and after drying is finished, the temperature is reduced for grinding, so that the particle size of the crystal particles reaches a preset size, and then the crystal particles are discharged out of the drying and cold-milling device; the reaction liquid or the extraction liquid for separating the chiral medicine enters a self-cleaning type centrifugal impurity removal device, the self-cleaning type centrifugal impurity removal device separates impurities in the reaction liquid or the extraction liquid, when dirty and blocked, self-cleaning can be carried out to remove the impurities, and then separation operation is carried out; in conclusion, the invention realizes the purposes of quickly and fully contacting the reaction liquid with the extraction liquid and displacing the chiral drug, and simultaneously reduces the investment of equipment and personnel in the processes of impurity removal, drying and grinding.
As a preferred embodiment of the present invention, as shown in fig. 1-7, the extraction crystallization apparatus includes an extraction kettle 100 and a mixing extraction mechanism, the mixing extraction mechanism is disposed in the extraction kettle 100, and the mixing extraction mechanism is rotatably connected to the extraction kettle 100, an extraction liquid enters the extraction kettle 100 through the mixing extraction mechanism, a heating mechanism 104 is disposed outside the extraction kettle 100, and a liquid level pipe 103 is connected to the outside of the extraction kettle 100. In order to enable heating to be faster, more sufficient and more uniform, the heating mechanism 104 adopts a plurality of annular heating pipes which are respectively sleeved outside the extraction kettle 100 and are arranged at intervals along the vertical direction, the annular heating pipes are mutually communicated through a plurality of vertical pipes which are arranged vertically, a second heat medium connector 110 and a first heat medium connector 105 are respectively communicated on the annular heating pipe which is positioned at the uppermost position and the annular heating pipe which is positioned at the lowermost position, a heat medium enters from the first heat medium connector 105 and is discharged from the second heat medium connector 110, so that the heat medium is uniformly distributed in each annular heating pipe and each vertical pipe, extraction liquid after reaction liquid separation in the extraction kettle 100 is heated, the heated extraction liquid is gradually evaporated, and chiral drugs are gradually separated out.
As a preferred embodiment of the present invention, as shown in fig. 2-3, the hybrid extraction mechanism includes a hole cylinder 200, a first liquid injection and drainage unit and a second liquid injection and drainage unit, wherein the upper and lower ends of the hole cylinder 200 respectively extend out of the extraction kettle 100 and are rotatably connected to the extraction kettle 100, the first liquid injection and drainage unit and the second liquid injection and drainage unit are both disposed in the hole cylinder 200, the second liquid injection and drainage unit is connected to an output shaft 208 of a power motor, the first liquid injection and drainage unit and the second liquid injection and drainage unit are driven by the power motor to rotate, and the hole cylinder 200 rotates synchronously with the first liquid injection and drainage unit and the second liquid injection and drainage unit. Thus, the extract is injected into the bore tube 200 through the first liquid injection and drainage unit and the second liquid injection and drainage unit, and along with the rotation of the bore tube 200, the extract is uniformly injected into the reaction liquid and is allowed to contact and react with the reaction liquid in all directions, so that the chiral drug in the reaction liquid is sufficiently displaced, then the bore tube 200 is reversed to offset the energy of the liquid flowing in the extraction kettle 100, and after a short period of time, the solution is kept stand and layered. The invention is provided with a scraping and guiding claw 109 at the lower part of a hole barrel 200, the scraping and guiding claw 109 is contacted with the lower wall of the inner wall at the corresponding position of an extraction kettle 100, the lower wall of the extraction kettle 100 is provided with a downward concave annular blanking groove 101, and a crystallization discharge joint 102 is constructed at the lower end of the extraction kettle 100 and the annular blanking groove 101; during the crystallization process, the scraping and guiding claw 109 stirs the crystals and scrapes off a part of the crystals from the inner wall of the extraction kettle 100, and then the crystals gradually gather in the annular charging chute 101 at the lowest part of the extraction kettle 100 and are gradually discharged out of the extraction kettle 100 through the crystal discharge joint 102.
As a preferred embodiment of the present invention, as shown in fig. 2 and fig. 4 to 5, the first liquid injection and discharge unit includes a first conduit 202, one end of the first conduit 202 vertically extends into the hole cylinder 200 from the upper end of the extraction kettle 100, a first piston 201 is communicated with the lower end of the first conduit 202, the first conduit 202 is communicated with the inside of the hole cylinder 200 through the first piston 201, a first conducting joint 203 is rotatably mounted on a portion of the first conduit 202 located outside the extraction kettle 100, the first conducting joint 203 is connected to a hose, a sliding seat 204 is mounted on the upper end of the first conduit 202, the sliding seat 204 is mounted on a sliding rail, and the sliding seat 204 is driven by a first cylinder to drive the first conduit 202 to move vertically. The second liquid injection and drainage unit comprises a second conduit 206, one end of the second conduit 206 vertically extends into the hole cylinder 200 from the lower end of the extraction kettle 100, the upper end of the second conduit 206 is communicated with a second piston 205, the second conduit 206 is communicated with the inside of the hole cylinder 200 through the second piston 205, a second conducting joint 207 is rotatably installed on the part of the second conduit 206, which is positioned outside the extraction kettle 100, the second conducting joint 207 is connected with another hose, and the lower end of the second conduit 206 is connected with a power motor. According to the invention, the circumferential surfaces of the first piston 201 and the second piston 205 are respectively provided with a first limiting groove 209 and a second limiting groove 210, the inner wall of the hole cylinder 200 is provided with a guide strip, the guide strip vertically extends from one end of the hole cylinder 200 to the other end, and the first limiting groove 209 and the second limiting groove 210 are assembled with the guide strip. According to the invention, the first guide pipe 202 is driven by the first cylinder to move vertically, so that in the rotating process of the bore cylinder 200, the extract liquid enters the bore cylinder 200 through the first piston 201 and the second piston 205 and is discharged into the extraction kettle 100 side by side, and due to the movement of the first piston 201, the area of the extract liquid entering the extraction kettle 100 is changed, and the pressure injected into the extraction kettle 100 is changed, so that the extract liquid and the reaction liquid are mixed in a pulse mode, and further, the extract liquid and the reaction liquid are fully mixed. After the reaction liquid and the extraction liquid are layered, the position of the first piston 201 is adjusted according to the liquid level layering of the liquid level pipe 103, so that the position of the first piston 201 is slightly higher than the layered surface, then the suction is carried out, the liquid is sucked from the extraction kettle 100 through the first piston 201, when the liquid is the extraction liquid, the residual reaction liquid in the extraction kettle 100 needs to be discharged to a self-cleaning type centrifugal impurity removal device for impurity removal, then the extraction kettle 100 is cleaned, the extraction liquid containing chiral drugs is injected into the extraction kettle 100 for heating, the chiral drugs are gradually separated out, after the evaporation of the extraction liquid is finished, the crystal discharge joint 102 is opened, and the crystals are discharged to a drying and cold grinding device for drying and grinding; when the liquid is reaction liquid, the reaction liquid is directly discharged to a self-cleaning centrifugal impurity removal device for impurity removal through the change of a pipe system and a valve system, extraction liquid containing chiral medicine is remained in the extraction kettle 100, the extraction kettle 100 is heated, the chiral medicine is gradually separated out, after the evaporation of the extraction liquid is finished, the crystal discharge joint 102 is opened, and the crystal is discharged to a drying cold grinding device for drying and grinding.
As a preferred embodiment of the present invention, the aperture of the through holes distributed on the bore 200 decreases gradually from top to bottom, and the drainage impeller 211 is detachably mounted on the outer wall of the bore 200, as shown in fig. 3 and 6-7, the drainage impeller 211 comprises a fixed disk 212 having an inner connecting edge 214, the inner connecting edge 214 is detachably connected to the outer wall of the bore 200, a plurality of drainage blades are uniformly configured on the fixed disk 212 along the circumferential direction thereof, drainage flanges 213 are respectively formed on both sides of each drainage blade, and when the drainage impeller 211 rotates with the bore 200, the drainage impeller 211 conducts upward drainage on the liquid in the extraction kettle 100, so that the liquid in the extraction kettle 100 turns upward, so as to overlap, mix and replace the hand medicine. The invention is provided with a flow stabilizing disc 106 below the drainage impeller 211 and close to the drainage impeller 211, the flow stabilizing disc 106 is provided with an outer connecting edge 108 detachably connected with the inner wall of the extraction kettle 100, the flow stabilizing disc 106 is provided with a plurality of flow passage 107, and the drained liquid realizes the purpose of rolling through the flow passage 107. In order to avoid that the layering surface fluctuates greatly in the separation process of the extraction liquid and the reaction liquid to cause the reaction liquid to be mixed in the extraction liquid, when the liquid in the extraction kettle 100 is layered, the drainage blade corresponds to the overflowing channel 107, so that the drainage blade is matched with the flow stabilizing disc 106 to stabilize the fluctuation generated in the extraction liquid extraction process. In order to ensure the effect of rolling or stabilizing the liquid in the extraction kettle 100, a plurality of the drainage impellers 211 and the flow stabilizing disc 106 are matched.
As a preferred embodiment of the present invention, as shown in fig. 8 to 11, the dry-cold grinding apparatus includes a dry-cold grinding kettle 300 and a temperature-adjusting stirring mechanism, the upper end of the dry-cold grinding kettle 300 has a feeding joint 307, the temperature-adjusting stirring mechanism is disposed in the dry-cold grinding kettle 300, the temperature-adjusting stirring mechanism is rotatably connected to the dry-cold grinding kettle 300, the lower end of the temperature-adjusting stirring mechanism is configured with a grinding member 403, a plurality of discharging holes 302 are disposed at the lower end of the dry-cold grinding kettle 300 and at the position of the grinding member 403, the discharging holes 302 are uniformly disposed along the circumferential direction of the dry-cold grinding kettle 300, an opening and closing cover 304 is movably connected to the position of the discharging holes 302 outside the dry-cold grinding kettle 300, and the opening and closing cover 304 is used for opening and closing the discharging holes 302. Chiral medicine crystallization gets into in dry cold grinding cauldron 300, it carries out the temperature to adjust the temperature rabbling mechanism, the rabbling mechanism that adjusts the temperature stirs and heats the crystallization, and then make the crystallization by the abundant heating, make the moisture that contains in it by abundant stoving, after the crystallization is by abundant stoving, it cools down to adjust the temperature rabbling mechanism, later open and close cover 304, along with the rotation of the rabbling mechanism that adjusts the temperature, make grinding piece 403 to grind the crystallization, and the crystallization in dry cold grinding cauldron 300 is at the rotatory in-process of the rabbling mechanism that adjusts the temperature, fully cool down, make and grind and keep going on under the lower temperature all the time, and then avoided the problem that the property of a medicine changes to appear in the chiral medicine.
As a preferred embodiment of the present invention, as shown in fig. 9 to 11, the temperature-adjusting stirring mechanism comprises a rotary assembly 400, the upper and lower ends of the rotary assembly body 400 are respectively provided with a medium outlet pipe 408 and a medium inlet pipe 401, the grinding member 403 is provided with a first medium cavity 404 communicated with the medium inlet pipe 401, the upper part of the rotary assembly body 400 is provided with a second medium cavity 407 communicated with the medium outlet pipe 408, a temperature adjusting stirring pipe 405 is uniformly arranged outside the rotary assembly body 400 along the circumferential direction thereof, the temperature-adjusting stirring pipe 405 is bent vertically and extends in a circuitous manner, two ends of the temperature-adjusting stirring pipe 405 are respectively communicated with the first medium cavity 404 and the second medium cavity 407, the parts of the medium inlet pipe 401 and the medium outlet pipe 408 extending out of the drying and cold-milling kettle 300 are respectively and rotatably connected with a medium inlet adapter 402 and a medium outlet adapter 409, and the medium inlet pipe 401 is provided with a driving wheel 406. The drive wheel 406 is driven and drives medium import pipe 401 and rotates, and then realize that rotatory assembly body 400 rotates, the effect of the stirred tube 405 that adjusts the temperature is the function of stirring and heating or cooling, as long as realize the change of the stirred tube 405 temperature that adjusts the temperature through changing the medium (like using hot water, hot oil and cold water or cryogen), and then realize that the stirred tube 405 that adjusts the temperature is at the dry crystallization of in-process of stirring or reduce crystallization temperature, at the in-process of grinding, cool down first medium chamber 404, it goes on to have realized keeping the low temperature all the time among the grinding process.
As a preferred embodiment of the present invention, as shown in fig. 9 to 10, the lower end of the dry-type cold grinding kettle 300 is configured as a horn-shaped grinding shell 301 which is tapered downward, the grinding member 403 is a conical grinding body which is engaged with the grinding shell 301, the lower end of the dry-type cold grinding kettle 300 is configured with a connecting cylinder 303, the lower part of the open-close cover 304 is configured with an adjusting sleeve 305 which is sleeved on the outer wall of the connecting cylinder 303, the adjusting sleeve 305 of the open-close cover 304 is in threaded connection with the connecting cylinder 303, and the outer wall of the adjusting sleeve is uniformly provided with a plurality of operating handles 306 along the circumferential direction thereof. When discharging is needed, an operator holds the operating handle 306 to rotate, so that the opening and closing cover 304 moves downwards, the discharging hole 302 is exposed, and the ground crystal particles are discharged from the discharging hole 302 and collected.
As a preferred embodiment of the present invention, as shown in FIGS. 12 to 14, the self-cleaning type centrifugal trash removal device includes a centrifugal vessel 500 and a centrifugal mechanism disposed in the centrifugal vessel 500 and rotatably connected to the centrifugal vessel 500. Wherein, the centrifugation mechanism includes a centrifugal net barrel 600, the lower extreme of this centrifugal net barrel 600 rotates with the centrifugation cauldron 500 to be connected, the lower extreme of centrifugation cauldron 500 is constructed and is had discharge joint 501, the upper end of centrifugation net barrel 600 stretches out the centrifugation cauldron 500 and passes through quick-operation joint intercommunication with the separation liquid export, be provided with a plurality of annular elastic baffle 604 along its vertical interval in the centrifugation net barrel 600, the outer edge of every annular elastic baffle 604 and the inner wall fixed connection of centrifugation net barrel 600, and the interior edge of annular elastic baffle 604 is connected with adjusting lever 601 through many connecting rods 605, adjusting lever 601 and the coincidence of the axis of centrifugation net barrel 600. The lower end of the adjusting rod 601 is connected with a pipe body 602 extending out of the centrifugal kettle 500, a slag discharge hole 603 is formed in the pipe body 602, the position of the pipe body 602 in the centrifugal kettle 500 is communicated with the centrifugal net barrel 600 through the slag discharge hole 603, the position of the pipe body 602 extending out of the centrifugal kettle 500 is rotatably connected with a slag discharge adapter 606, the lower end of the pipe body 602 is connected with a driving motor, and the driving motor is driven by the second cylinder and can move vertically. The rotation of the centrifugal net cylinder 600 is realized by the driving motor, so that the liquid entering the centrifugal net cylinder 600 is discharged into the centrifugal kettle 500 through the cylinder wall of the centrifugal net cylinder 600 in a centrifugal state and is discharged through the discharge connector 501, and most of impurities are accumulated at the connection position of the annular elastic baffle 604 and the cylinder wall of the centrifugal net cylinder 600 under the action of centrifugal force. When self-cleaning is needed, the second cylinder is controlled to drive the adjusting rod 601 to move downwards, the adjusting rod 601 drives the inner edge of the annular elastic baffle 604 to move downwards, so that an included angle between the annular elastic baffle 604 and the wall of the centrifugal screen cylinder 600 is an obtuse angle, cleaning liquid enters the rotating centrifugal screen cylinder 600 and carries impurities to be pumped out through the slag discharge adapter 606, and self-cleaning of the centrifugal screen cylinder 600 is achieved.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the claims of the present invention.
Claims (6)
1. A purification system for producing a chiral drug, characterized by: the device comprises an extraction crystallization device and a drying cold grinding device connected with a discharge port of the extraction crystallization device, wherein a separation liquid outlet of the extraction crystallization device is connected with a self-cleaning centrifugal impurity removal device; the extraction crystallization device comprises a mixing extraction mechanism arranged in an extraction kettle, the mixing extraction mechanism is rotationally connected with the extraction kettle, an extraction liquid enters the extraction kettle through the mixing extraction mechanism, a heating mechanism is sleeved outside the extraction kettle, and a liquid level pipe is communicated with the outside of the extraction kettle; the mixed extraction mechanism comprises a hole cylinder, wherein the upper end and the lower end of the hole cylinder respectively extend out of the extraction kettle and are rotationally connected with the extraction kettle, a first liquid injection and drainage unit and a second liquid injection and drainage unit are arranged in the hole cylinder, the first liquid injection and drainage unit and the second liquid injection and drainage unit are driven by a power motor connected with the second liquid injection and drainage unit to rotate, the hole cylinder synchronously rotates along with the first liquid injection and drainage unit and the second liquid injection and drainage unit, a scraping and guiding claw is arranged at the lower part of the hole cylinder and is contacted with the lower wall of the inner wall at the corresponding position of the extraction kettle, the lower wall of the extraction kettle is provided with a downward-concave annular blanking groove, and a crystallization discharge joint is constructed at the lower end of the extraction kettle and the position of the annular blanking groove; the first liquid injection and drainage unit comprises a first guide pipe, one end of the first guide pipe vertically extends into the hole cylinder from the upper end of the extraction kettle, a first piston is communicated with the lower end of the first guide pipe, the first guide pipe is communicated with the interior of the hole cylinder through the first piston, a first conduction joint is rotatably installed on the part, located outside the extraction kettle, of the first guide pipe, a sliding seat is installed at the upper end of the first guide pipe, and the sliding seat is installed on a sliding rail and driven by a first air cylinder to vertically move; the second liquid injection and drainage unit comprises a second guide pipe, one end of the second guide pipe vertically extends into the hole cylinder from the lower end of the extraction kettle, a second piston is communicated with the upper end of the second guide pipe, the second guide pipe is communicated with the inside of the hole cylinder through the second piston, a second conduction joint is rotatably installed on the part, located outside the extraction kettle, of the second guide pipe, and the lower end of the second guide pipe is connected with the power motor.
2. A purification system for the production of chiral drugs according to claim 1, wherein: the aperture top-down of the through-hole that is covered with on the hole section of thick bamboo diminishes in proper order, demountable installation has a drainage impeller on the hole section of thick bamboo outer wall, the drainage impeller is including the fixed disk that has the internal connection edge, the internal connection edge can be dismantled with hole section of thick bamboo outer wall and be connected, in evenly be constructed along its circumference on the fixed disk and have a plurality of drainage blades, in each the both sides of drainage blade are formed with the drainage turn-ups respectively, in the below of drainage impeller and the position department that is close to drainage impeller are provided with the steadying flow dish, the steadying flow dish has the outer joint edge of dismantling the connection with the inner wall of extraction cauldron, has seted up a plurality of passageways that flow over on the steadying flow dish, when the extraction cauldron interior liquid-liquid layering, the drainage blade is corresponding to and flows over passageway department.
3. A purification system for the production of chiral drugs according to claim 1, wherein: the dry cold grinding device is including having the dry cold grinding cauldron that the feeding connects, in dry cold grinding cauldron internal rotation is connected with the rabbling mechanism that adjusts the temperature, in the lower extreme of rabbling mechanism that adjusts the temperature is constructed and is ground the piece, in the lower extreme of dry cold grinding cauldron just is located to grind a department and sets up a plurality of unloading holes that evenly set up along dry cold grinding cauldron's circumference, in dry cold grinding cauldron just is located unloading hole department swing joint outward and is used for opening and close the cover that opens and close of unloading hole.
4. A purification system for the production of chiral drugs according to claim 3, wherein: the stirring mechanism adjusts the temperature is constructed the rotatory assembly body that has medium outlet pipe and medium import pipe respectively including upper and lower both ends, grinding member has the first medium chamber with medium import pipe intercommunication, the upper portion of rotatory assembly body is constructed the second medium chamber with medium outlet pipe intercommunication, installs the stirring pipe that adjusts the temperature in rotatory assembly body outer evenly along its circumference, the stirring pipe that adjusts the temperature is along vertical circuitous extension of buckling, and the both ends of stirring pipe that adjusts the temperature communicate with first medium chamber and second medium chamber respectively, it is connected with medium import adapter and medium export adapter to rotate respectively on the position that dry cryomilling cauldron is stretched out to medium import pipe and medium outlet pipe, installs the drive wheel on medium import pipe.
5. A purification system for the production of chiral drugs according to claim 3, wherein: the lower end of the drying and cold-milling kettle is constructed into a horn-shaped milling shell which is reduced downwards, the milling part is a conical milling body matched with the milling shell, the lower end of the drying and cold-milling kettle is constructed into a connecting cylinder, the lower part of the opening and closing cover is constructed into an adjusting sleeve which is sleeved on the outer wall of the connecting cylinder and is in threaded connection with the connecting cylinder, and a plurality of operating handles are uniformly arranged on the outer wall of the adjusting sleeve along the circumferential direction of the adjusting sleeve.
6. A purification system for the production of chiral drugs according to claim 1, wherein: the self-cleaning centrifugal impurity removing device comprises a centrifugal mechanism which is arranged in a centrifugal kettle in a built-in manner and is rotationally connected with the centrifugal kettle, the centrifugal mechanism comprises a centrifugal net cylinder of which the lower end is rotationally connected with the centrifugal kettle, a discharge joint is constructed at the lower end of the centrifugal kettle, the upper end of the centrifugal net cylinder extends out of the centrifugal kettle and is communicated with a separation liquid outlet through a quick joint, a plurality of annular elastic baffles are arranged in the centrifugal net cylinder along the vertical interval of the centrifugal net cylinder, the outer edge of each annular elastic baffle is fixedly connected with the inner wall of the centrifugal net cylinder, the inner edge of each annular elastic baffle is connected with an adjusting rod through a plurality of connecting rods, the adjusting rod is superposed with the axis of the centrifugal net cylinder, a pipe body extending out of the centrifugal kettle is connected with a pipe adapter extending out of the centrifugal kettle, the position of the pipe body in the centrifugal kettle is communicated with the centrifugal net cylinder, the position of the pipe body extending out of the centrifugal kettle is rotationally connected with a slag discharge, and the lower end of the pipe body is connected with a driving motor, and the driving motor is driven by the second cylinder and can move along the vertical direction.
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| JP6143808B2 (en) * | 2015-05-28 | 2017-06-07 | 曽田香料株式会社 | Extraction method of solute components in aqueous solution |
| CN206853783U (en) * | 2017-06-20 | 2018-01-09 | 青岛嘉德滤料有限公司 | A kind of powdered activated carbon fine grinding device |
| CN208031968U (en) * | 2018-01-24 | 2018-11-02 | 云南博泽林化工有限公司 | A kind of tannic acid equipment for purifying |
| CN111362231B (en) * | 2020-03-16 | 2021-06-04 | 淮北师范大学 | System and method for extracting sulfur from sulfur-containing foam of coking plant |
| CN212594118U (en) * | 2020-05-22 | 2021-02-26 | 广东新达瑞生物科技有限公司 | Multifunctional tank capable of extracting, separating, concentrating, crystallizing and filtering |
| CN111790180A (en) * | 2020-07-09 | 2020-10-20 | 江西德盛精细化学品有限公司 | Device is refined in extraction of acid fixing agent |
| CN112916129A (en) * | 2020-12-29 | 2021-06-08 | 蚌埠市兄弟粮油食品科技有限公司 | Processing technology of selenium-rich glutinous rice flour |
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