CN114230476A - Preparation method and device of small-particle pregabalin - Google Patents

Preparation method and device of small-particle pregabalin Download PDF

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Publication number
CN114230476A
CN114230476A CN202111672660.0A CN202111672660A CN114230476A CN 114230476 A CN114230476 A CN 114230476A CN 202111672660 A CN202111672660 A CN 202111672660A CN 114230476 A CN114230476 A CN 114230476A
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China
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liquid storage
storage tank
pregabalin
solution
screen
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CN202111672660.0A
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CN114230476B (en
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郑伯州
赵智勇
曹倩
詹小军
胡霞
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Shanghai Guochuang Pharmaceutical Co ltd
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Shanghai Guochuang Pharmaceutical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification
    • C07C227/42Crystallisation

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  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)

Abstract

The invention discloses a preparation device of small-particle pregabalin, which comprises the following components: a liquid storage tank, wherein pregabalin crystal precipitate and solution are placed in the liquid storage tank; the support is used for supporting the liquid storage tank, and a cover plate is arranged at the top of the liquid storage tank; the screen is placed inside the liquid storage tank, the screen separates the solution from the crystals, a pipeline for pumping the solution at the top of the screen is arranged at the bottom of the cover plate, and the pipeline is connected with external negative pressure suction equipment; the turnover mechanism is arranged between the liquid storage tank and the support, and the turnover mechanism turns over and discharges the liquid tank after the solution at the top of the screen is absorbed by the pipeline, so that the solution in the liquid storage tank flows back to the cover plate position and is absorbed again by the pipeline.

Description

Preparation method and device of small-particle pregabalin
Technical Field
The invention relates to the technical field of preparation of small-particle pregabalin, in particular to a preparation method and a device of small-particle pregabalin.
Background
The chemical name of Pregabalin is (S) -3-aminomethyl-5-methylhexanoic acid, the molecular formula is C8H17NO2, the Pregabalin is an antiepileptic drug and is mainly used for clinically treating postherpetic neuralgia, Pregabalin (Pregabalin) is a novel gamma-aminobutyric acid (GABA) receptor antagonist developed by the company Pespern, is mainly used for treating anxiety disorder, neuropathic pain, epileptic seizure and other diseases, and has the advantages of small administration dosage, quick response, long duration, few toxic side effects and the like.
In recent years, the rapid development of controlled release and sustained release technology of the preparation puts forward higher quality requirements on the granularity of raw material medicines. Formulation aspects would like to address the particle size distribution of the product from the API source to meet their particular needs. For pregabalin products, the particle size problem is also urgently needed to be solved. Although a large number of documents and patents report the preparation of pregabalin, API product particles obtained by these preparation methods are often large, and the average particle diameter D (50) is 700 to 1000 μm. For preparing the small-particle pregabalin, the large-particle product needs to be crushed and sieved for multiple times to reach the small-particle size range required by the preparation, such as: the average particle diameter D (50) is 100 to 300 μm. The complicated crushing and sieving process is not only long in time consumption and low in efficiency, but also inconvenient in operation and not beneficial to industrial production.
In the existing preparation method of small-particle pregabalin with patent application number 201510068646.8, a certain amount of pregabalin crude product is added into a mixed solution of alcohol and water, and the mixture is heated to 80-90 ℃ and stirred to be dissolved clearly; then cooling to 60-68 ℃, and adding pregabalin seed crystal into the solution at the temperature; and slowly cooling, crystallizing, filtering and drying to obtain a small-particle pregabalin product with the average particle size D (50) of 100-300 mu m, wherein after the small-particle pregabalin is precipitated, the small-particle pregabalin product needs to be sieved by a 100-300-mesh screen, during specific operation, a container after the crystals are precipitated is moved to a filtering device, and then the solution and the crystals are poured into the filtering device for filtering, but a large amount of manpower and material resources are consumed in the process of moving the container and the crystals to the filtering device, so that the preparation of the small-particle pregabalin is inconvenient.
Disclosure of Invention
The invention aims to provide a preparation method and a device of small-particle pregabalin, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation facilities of small granule pregabalin includes:
a liquid storage tank, wherein pregabalin crystal precipitate and solution are placed in the liquid storage tank;
the support is used for supporting the liquid storage tank, and a cover plate is arranged at the top of the liquid storage tank;
the screen is placed inside the liquid storage tank, the screen separates the solution from the crystals, a pipeline for pumping the solution at the top of the screen is arranged at the bottom of the cover plate, and the pipeline is connected with external negative pressure suction equipment;
and the turnover mechanism is arranged between the liquid storage tank and the support, and turns over and discharges the liquid storage tank after the solution at the top of the screen is absorbed by the pipeline, so that the solution in the liquid storage tank is sucked by the pipeline again after flowing back to the cover plate position.
Preferably, the turnover mechanism comprises a jacking mechanism installed inside the support, the outer side of the liquid storage tank is provided with two rails, the two rails are provided with turnover grooves, the side face of the support is provided with a rotating column inserted into the turnover grooves, and the jacking mechanism jacks up the liquid storage tank and then enables the liquid storage tank to turn over by rotating the rotating column.
Preferably, the jacking mechanism comprises an air cylinder installed on the support, and a top plate for jacking the bottom of the liquid storage tank is arranged at the top of the air cylinder.
Preferably, orbital inside is equipped with two positioning mechanism of supplementary rotation post location, and two positioning mechanism are located orbital both ends respectively, positioning mechanism include with track pivoted rotor plate, the rotor plate is connected through pivot and track rotation, be equipped with the torsional spring between rotor plate and the pivot, the one end butt of rotor plate is in the outside of rotating the post, one side of rotor plate is equipped with along the inside gliding locating plate of track, the rotor plate is along with the rail displacement to rotating post position after, the locating plate is fixed a position the rotor plate after sliding down for the rotation post is fixed a position by the rotor plate.
Preferably, the rotating plate comprises a first part abutting against the outer side of the rotating column, a second part is arranged on one side of the first part, and the second part is in contact with the positioning plate.
Preferably, the liquid storage pot outside is equipped with the spacing stop gear to the screen cloth, stop gear is including installing the screw rod in the liquid storage pot outside, the outside of screw rod is equipped with the electro-magnet to the screen cloth attraction, the tip of screw rod is equipped with and promotes screw rod pivoted and rotates the piece.
Preferably, the rotating part comprises a handle arranged outside the screw rod, and the handle is fixedly connected with the screw rod.
Preferably, the rotating part comprises a distance sensor arranged at the bottom of the cover plate, the end part of the screw rod is fixedly connected with a motor, and along with the change of the distance between the distance sensor and the screen, the motor pushes the screw rod to rotate, so that the electromagnet can attract the outer side of the screen.
Preferably, the bottom of the liquid storage tank is provided with a moving part for sealing the liquid storage tank, the moving part comprises a sliding column in sliding connection with the liquid storage tank, and two sides of the sliding column are respectively provided with a sealing gasket for sealing the liquid storage tank and a boss for opening the sealing tank.
A preparation method of small-particle pregabalin comprises the following steps:
step one, pouring crude pregabalin into a container for dissolving;
screening impurities of the dissolved pregabalin solution by using screening equipment, and placing the screened solution in a liquid storage tank;
step three, separating out small particle pregabalin crystals after the solution is cooled, and adsorbing the upper layer solution by using a pipeline immediately after the screen is arranged from the top of the liquid storage tank until the surface layer solution is completely adsorbed;
step four, turning over the liquid storage tank by using a turning mechanism, and continuously using a pipeline to extract redundant solution;
and step five, placing the liquid storage tank and the leaching in a drying box for drying, and finishing the preparation.
The invention has at least the following beneficial effects:
the solution at the top of the screen is extracted through the pipeline, and then the liquid storage tank is turned through the turning mechanism and then the liquid is continuously extracted, compared with the prior art that a large amount of manpower and material resources are consumed in the process that the container and the crystals are moved to the filtering equipment, and the preparation of the small-particle pregabalin is inconvenient.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a partial cross-sectional view of a fluid reservoir of the present invention;
FIG. 3 is a partial cross-sectional view of a stent according to the present invention;
FIG. 4 is an enlarged view of area A of FIG. 3;
FIG. 5 is an enlarged view of area B of FIG. 3;
FIG. 6 is a partial view of a fluid reservoir of the present invention;
FIG. 7 is an enlarged view of area C of FIG. 6;
FIG. 8 is an enlarged view of area D of FIG. 6;
FIG. 9 is a partial cross-sectional view of the present invention;
FIG. 10 is an enlarged view of area E of FIG. 9;
FIG. 11 is a diagram of a second embodiment of the present invention.
In the figure: 1-a liquid storage tank; 2-a scaffold; 3-cover plate; 4-a pipeline; 5-screening the screen; 6-turning over mechanism; 61-track; 62-overturning the groove; 63-rotating the column; 7-a jacking mechanism; 71-a cylinder; 72-a top plate; 8-a positioning mechanism; 81-rotating the plate; 82-torsion spring; 83-a positioning plate; 9-a rotating member; 91-a handle; 92-a distance sensor; 93-a motor; 10-a stationary ring; 11-placing a ring; 12-a limiting mechanism; 121-screw rod; 122-an electromagnet; 13-a movable member; 131-a sliding column; 132-a gasket; 133-boss.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-11, the present invention provides a technical solution: in one embodiment, a device for preparing small-particle pregabalin includes:
a liquid storage tank 1, wherein pregabalin crystal sediment and solution are placed in the liquid storage tank 1;
the liquid storage tank 1 is arranged on the support 2, the support 2 supports the liquid storage tank 1, a cover plate 3 is arranged at the top of the liquid storage tank 1, the cover plate 3 provides a pipeline 4 supporting function, the cover plate 3 is fixedly connected with the liquid storage tank 1 and can be detached relative to the liquid storage tank 1, and the support 2 is used for installing the liquid storage tank 1 to facilitate the overturning of the liquid storage tank 1;
the liquid storage tank comprises a screen 5, the screen 5 is placed inside a liquid storage tank 1, a fixing ring 10 for fixing the screen 5 is arranged on the outer side of the screen 5, the fixing ring 10 of the screen 5 is in contact with the inner wall of the liquid storage tank 1, the screen 5 separates a solution from a crystal, a pipeline 4 for extracting the solution at the top of the screen 5 is arranged at the bottom of a cover plate 3, a placing ring 11 is fixedly connected to the end of the pipeline 4, the pipeline 4 is placed at the top of the screen 5 through the placing ring 11, a groove is formed in the inner wall of the cover plate 3, the placing ring 11 is matched with the groove, the pipeline 4 and the cover plate 3 are conveniently sealed through the placing ring 11 after the liquid storage tank 1 is turned over, and then the liquid in the liquid storage tank 1 can be more conveniently extracted, the pipeline 4 is connected with external negative pressure suction equipment, the negative pressure equipment is a water pump, and the liquid in the liquid storage tank 1 can be extracted through the pipeline 4;
the turnover mechanism 6 is arranged between the liquid storage tank 1 and the support 2, the turnover mechanism 6 turns over and dumps the liquid storage tank 1 after the solution at the top of the screen 5 is absorbed by the pipeline 4 after the pipeline 4, so that the solution in the liquid storage tank 1 flows back to the position of the cover plate 3 and is sucked by the pipeline 4 again, before the turnover mechanism 6 turns over, the pipeline 4 completely extracts the solution at the top of the screen 5 in the liquid storage tank 1, at the moment, partial solution is still in the crystal at the bottom of the screen 5, at the moment, the crystal and the screen 5 are turned over by the turnover mechanism 6, and then the solution in the crystal is further extracted, the subsequent drying of the crystal is more convenient, so that the manpower and material resources of the solution and the sediment during the transfer are reduced, the preparation time of the small-particle pregabalin is saved, in addition, the screen 5 reaches the surface of the sediment after entering the solution from the upper part of the solution, and does not need to directly pour the solution and the sediment into the surface of the screen 5, on one hand, the possibility that the screen 5 is blocked by sediment is reduced, on the other hand, the solution does not need to flow down after passing through the screen 5 and the small-particle pregabalin crystals, the solution is directly pumped out by the pipeline 4 after passing through the screen 5, the screen 5 only screens out the solution from the small-particle pregabalin crystals after being overturned, the screening time of the crystals and the screen 5 is shortened, the preparation efficiency of the small-particle pregabalin is improved, in addition, when the small-particle pregabalin crystals are transported along with a container and poured into the top of the screen 5, collision can occur between the crystals and between the crystals and the container, further the crystals are crushed, when the screen 5 is used for screening, part of the small-particle crystals directly flow out along with the screen 5, the overturning mechanism 6 does not need to transport the small-particle pregabalin and the solution, only needs to overturn the liquid storage tank 1, and the possibility of collision between the crystals or between the crystals and the inner wall of the liquid storage tank 1 is reduced, thereby ensuring the total preparation amount of the small-particle pregabalin, reducing the waste of the small-particle pregabalin and saving the cost.
Tilting mechanism 6 is including installing at the inside jack-up mechanism 7 of support 2, the outside of liquid storage pot 1 is equipped with two tracks 61, and two tracks 61 are the symmetric distribution, two tracks 61 all with liquid storage pot 1 fixed connection, two track 61 all is equipped with upset groove 62, the side of support 2 is equipped with the rotation post 63 that inserts in upset groove 62, rotates post 63 and support 2 fixed connection, rotates post 63 and can pass through the bolt with support 2 and dismantle, jack-up mechanism 7 is with 1 jack-up back of liquid storage pot to rotate post 63 and make 1 upset of liquid storage pot for rotating, jack-up mechanism 7 cooperation tilting mechanism 6 overturns, and then reduces the center of overturning, and the convenience is to the upset of liquid storage pot 1, and liquid storage pot 1 can overturn along rotating post 63 under self action of gravity.
The jacking mechanism 7 comprises an air cylinder 71 arranged on the support 2, the air cylinder 71 is fixedly connected with the support 2, the top of the air cylinder 71 is provided with a top plate 72 jacking the bottom of the liquid storage tank 1, the top plate 72 is contacted with the bottom of the liquid storage tank 1, the air cylinder 71 is fixedly connected with the top plate 72, the air cylinder 71 can drive the top plate 72 to jack up when jacking, so as to further push the rotating column 63 to slide in the overturning groove 62, after sliding to the position of the screen 5, the rotating column 63 is positioned at the bottom of the overturning groove 62, the air cylinder 71 is recovered, the liquid storage tank 1 rotates along the rotating column 63 under the action of the self gravity of the liquid storage tank 1, so as to overturn the liquid storage tank 1, the pipeline 4 is a hose, the pipeline 4 slides along the cover plate 3 when overturning, the placing ring 11 slides into the groove, so as to further seal the liquid storage tank 1 and the cover plate 3, and can pump out air in the liquid storage tank 1 when the pipeline 4 pumps out liquid, further facilitating the liquid to flow from one side of the screen 5 to the other side, and further facilitating the extraction of the liquid in the liquid storage tank 1.
The inside of track 61 is equipped with two positioning mechanism 8 of supplementary rotation post 63 location, and two positioning mechanism 8 are located the both ends of track 61 respectively, positioning mechanism 8 include with track 61 pivoted rotating plate 81, rotating plate 81 rotates with track 61 through the pivot and is connected, pivot and track 61 fixed connection, rotating plate 81 rotates with the pivot to be connected, be equipped with torsional spring 82 between rotating plate 81 and the pivot, the both ends of torsional spring 82 respectively with pivot and rotating plate 81 fixed connection, one end butt of rotating plate 81 is in the outside of rotation post 63, one side of rotating plate 81 is equipped with along the inside gliding locating plate 83 of track 61, after rotating plate 81 moves to rotation post 63 position along with track 61, locating plate 81 location after the locating plate 83 slides down for rotation post 63 is fixed a position by rotating plate 81, after pipeline 4 absorbs the solution at the top of screen cloth 5 completely, at this time, the cylinder 71 is ejected, the cylinder 71 drives the top plate 72 to push the liquid storage tank 1 to move upwards, the rotating column 63 slides in the overturning groove 62, the rotating column 63 firstly disengages from the rotating plate 81 at the top, the rotating plate 81 at the top rotates, the torsion spring 82 rotates, after the rotating column 63 disengages from the rotating plate 81 at the top, the torsion spring 82 resets, when the rotating column 63 moves to the rotating plate 81 at the top, the rotating column 63 drives the rotating plate 81 to rotate, the torsion spring 82 is twisted, after the rotating column 63 is arranged at one side of the rotating plate 81, the positioning plate 83 is at the other side of the rotating plate 81 due to the action of gravity, when the cylinder 71 retracts, the rotating column 63 abuts against one side of the rotating plate 81, the positioning plate 83 limits the other side of the rotating plate 81, so that the rotating column 63 cannot slide in the overturning groove 62, the rotating position of the rotating column 63 on the rail 61 is ensured, and the liquid storage tank 1 is convenient to rotate along the rotating column 63 direction, further promote and rotate post 63 pivoted stability, when liquid storage pot 1 rotates to the top, locating plate 83 slides in track 61 under the effect of gravity this moment, remove the restriction to rotor plate 81, and then make things convenient for the upset once more of liquid storage pot 1, in addition rotate post 63 to overturn behind screen cloth 5 one side position again, further make things convenient for throwing away of the interior solution of tiny particle pregabalin crystal, and still reduce the collision that tiny particle pregabalin crystal produced when the upset, reduce the broken possibility of tiny particle pregabalin crystal, make things convenient for the filtration of tiny particle pregabalin.
The rotating plate 81 comprises a first part abutted to the outer side of the rotating column 63, a second part is arranged on one side of the first part and integrally formed with the first part, and the second part is in contact with the positioning plate 83, so that the first part is more conveniently positioned through the second part and the positioning plate 83.
The outer side of the liquid storage tank 1 is provided with a limiting mechanism 12 for limiting the screen 5, the limiting mechanism 12 comprises a screw rod 121 arranged on the outer side of the liquid storage tank 1, the screw rod 121 is rotatably connected with the liquid storage tank 1, the outer side of the screw rod 121 is provided with an electromagnet 122 for attracting the screen 5, the electromagnet 122 is in threaded connection with the screw rod 121, the fixing ring 10 is a steel ring and can be adsorbed by the electromagnet 122, and the end part of the screw rod 121 is provided with a rotating part 9 for pushing the screw rod 121 to rotate.
The rotating member 9 comprises a handle 91 arranged outside the screw rod 121, the handle 91 is fixedly connected with the screw rod 121, when the screen 5 falls to the surface of the small-particle pregabalin crystal along with the self gravity, the position of the screen 5 can be observed through the transparent liquid storage tank 1, at the moment, the handle 91 is rotated, the handle 91 drives the electromagnet 122 to move to a position slightly higher than the screen 5, the electromagnet 122 is started, the electromagnet 122 attracts the fixing ring 10 on the outer side of the screen 5, the screen 5 is fixed on the inner wall of the liquid storage tank 1, thereby convenient subsequent upset reduces the possibility that the granule pregabalin crystal removed, reduces the possibility of collision between granule pregabalin crystal and the liquid storage pot 1, in addition, more convenient the extraction of pipeline 4 to the solution that is located screen cloth 5 one side after the upset, and pipeline 4 is kept away from to screen cloth 5, makes things convenient for pipeline 4 directly to absorb the solution.
The bottom of the liquid storage tank 1 is provided with a movable piece 13 which seals the liquid storage tank 1, the movable piece 13 comprises a sliding column 131 which is connected with the liquid storage tank 1 in a sliding way, the two sides of the sliding column 131 are respectively provided with a sealing gasket 132 for sealing the liquid storage tank 1 and a boss 133 for opening the sealing tank, the sealing gasket 132 and the boss 133 are respectively fixedly connected with the sliding column 131, when the liquid storage tank 1 is turned over, under the action of the gravity of the movable member 13 and the pressure of the solution and the crystal, the sealing gasket 132 is attached to the bottom of the liquid storage tank 1, thereby facilitating the sealing of the liquid storage tank 1, after being turned over, the gasket 132 is separated from the tank 1, and air can enter the tank 1, when the pipeline 4 at the bottom is bled, outside air gets into in the liquid storage pot 1 simultaneously to pass through the filter screen with liquid and impress apron 3 department from the interior little granule pregabalin crystal, and then convenient more quick taking out of little granule pregabalin crystal interior solution.
According to the above embodiment, referring to fig. 11, in the present invention, there is a second embodiment, the rotating member 9 includes a distance sensor 92 installed at the bottom of the cover plate 3, the distance sensor 92 is fixedly connected to the cover plate 3, an end of the screw rod 121 is fixedly connected to a motor 93, the motor 93 is electrically connected to the distance sensor 92, the motor 93 is fixedly connected to the screw rod 121, the motor 93 pushes the screw rod 121 to rotate with a change in distance between the distance sensor 92 and the screen 5, so that the electromagnet 122 attracts the outer side of the screen 5, when the screen 5 descends to the surface of the crystal, the distance sensor 92 emits a signal to measure the distance between the screen 5, the motor 93 is controlled to rotate, the motor 93 drives the screw rod 121 to rotate, the electromagnet 122 rotates to the upper portion of the screen 5, the electromagnet 122 is energized to attract the screen 5, and the screen 5 moves upward by a small distance, thereby contain some liquid in the crystal, when the upset, to playing lubricated effect between crystal and the liquid storage pot 1, reduce the broken possibility of crystal, make things convenient for the sifting out of crystal, can the moving position of direct control electro-magnet 122 through distance sensor 92 in addition, and then more convenient locking to screen cloth 5, make things convenient for subsequent upset.
A preparation method of small-particle pregabalin comprises the following steps:
step one, pouring crude pregabalin into a container for dissolving;
screening impurities of the dissolved pregabalin solution by using screening equipment, and placing the screened solution in a liquid storage tank 1;
step three, separating out small particle pregabalin crystals after the solution is cooled, and adsorbing the upper layer solution by using a pipeline 4 after a screen 5 is arranged from the top of the liquid storage tank 1 until the surface layer solution is completely adsorbed;
step four, the liquid storage tank 1 is turned over by using the turning mechanism 6, and the pipeline 4 is continuously used for extracting the redundant solution;
and step five, placing the liquid storage tank 1 and the leaching in a drying box for drying, and finishing the preparation.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. A preparation facilities of small granule pregabalin includes:
the device comprises a liquid storage tank (1), wherein pregabalin crystal precipitates and a solution are placed in the liquid storage tank (1);
the method is characterized in that:
the liquid storage tank (1) is mounted on the support (2), the support (2) supports the liquid storage tank (1), and a cover plate (3) is arranged at the top of the liquid storage tank (1);
the liquid storage tank is characterized by comprising a screen (5), the screen (5) is placed inside the liquid storage tank (1), the screen (5) separates the solution from the crystals, a pipeline (4) for pumping the solution at the top of the screen (5) is arranged at the bottom of the cover plate (3), and the pipeline (4) is connected with external negative pressure suction equipment;
tilting mechanism (6), tilting mechanism (6) are installed between liquid storage pot (1) and support (2), tilting mechanism (6) absorb the solution at screen cloth (5) top at pipeline (4) back dump liquid pot (1), make solution refluence in liquid storage pot (1) is sucked by pipeline (4) once more behind apron (3) position.
2. The device of small particle pregabalin of claim 1, wherein: tilting mechanism (6) are including installing jacking mechanism (7) in support (2) inside, the outside of liquid storage pot (1) is equipped with two tracks (61), two track (61) all are equipped with upset groove (62), the side of support (2) is equipped with rotation post (63) of inserting in upset groove (62), jacking mechanism (7) make liquid storage pot (1) upset for rotating post (63) after with liquid storage pot (1) jack-up.
3. The device of small particle pregabalin of claim 2, characterized in that: the jacking mechanism (7) comprises an air cylinder (71) arranged on the support (2), and a top plate (72) for jacking the bottom of the liquid storage tank (1) is arranged at the top of the air cylinder (71).
4. The device of small particle pregabalin of claim 2, characterized in that: the inside of track (61) is equipped with two positioning mechanism (8) of supplementary rotation post (63) location, and two positioning mechanism (8) are located the both ends of track (61) respectively, positioning mechanism (8) include with track (61) pivoted rotor plate (81), rotor plate (81) rotate with track (61) through the pivot and are connected, be equipped with torsional spring (82) between rotor plate (81) and the pivot, the one end butt of rotor plate (81) is in the outside of rotating post (63), one side of rotor plate (81) is equipped with along track (61) inside gliding locating plate (83), rotor plate (81) are moving to rotation post (63) position along with track (61) after, locating plate (83) slide down back with rotor plate (81) location for rotation post (63) is fixed a position by rotor plate (81).
5. The device of small particle pregabalin of claim 4, wherein: the rotating plate (81) comprises a first component which is abutted against the outer side of the rotating column (63), one side of the first component is provided with a second component, and the second component is in contact with the positioning plate (83).
6. The device of small particle pregabalin of claim 2, characterized in that: liquid storage pot (1) outside is equipped with spacing stop gear (12) to screen cloth (5), stop gear (12) are including installing screw rod (121) in liquid storage pot (1) outside, the outside of screw rod (121) is equipped with electro-magnet (122) to screen cloth (5) attraction, the tip of screw rod (121) is equipped with and promotes screw rod (121) pivoted and rotates piece (9).
7. The device of small particle pregabalin of claim 6, wherein: the rotating part (9) comprises a handle (91) arranged on the outer side of the screw rod (121), and the handle (91) is fixedly connected with the screw rod (121).
8. The device of small particle pregabalin of claim 6, wherein: the rotating piece (9) comprises a distance sensor (92) arranged at the bottom of the cover plate (3), the end part of the screw rod (121) is fixedly connected with a motor (93), and along with the change of the distance between the distance sensor (92) and the screen (5), the motor (93) pushes the screw rod (121) to rotate, so that the electromagnet (122) can attract the outer side of the screen (5).
9. The device of small particle pregabalin of claim 1, wherein: the bottom of liquid storage pot (1) is equipped with moving part (13) sealed to liquid storage pot (1), moving part (13) include with liquid storage pot (1) sliding connection's slip post (131), the both sides of slip post (131) are equipped with sealed pad (132) sealed to liquid storage pot (1) and boss (133) that will seal the jar and open respectively.
10. A method for preparing small-particle pregabalin applied to the preparation device of claim 1, characterized in that: the method comprises the following steps:
step one, pouring crude pregabalin into a container for dissolving;
screening impurities of the dissolved pregabalin solution by using screening equipment, and placing the screened solution in a liquid storage tank (1);
step three, separating out small-particle pregabalin crystals after the solution is cooled, and adsorbing the upper-layer solution by using a pipeline (4) from the top of the liquid storage tank (1) by using a screen (5) until the surface-layer solution is completely adsorbed;
step four, the liquid storage tank (1) is turned over by using a turning mechanism (6), and the pipeline (4) is continuously used for extracting the redundant solution;
and step five, placing the liquid storage tank (1) and the leaching in a drying box for drying, and finishing the preparation.
CN202111672660.0A 2021-12-31 2021-12-31 Preparation method and device of small-particle pregabalin Active CN114230476B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202111672660.0A CN114230476B (en) 2021-12-31 2021-12-31 Preparation method and device of small-particle pregabalin

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Application Number Priority Date Filing Date Title
CN202111672660.0A CN114230476B (en) 2021-12-31 2021-12-31 Preparation method and device of small-particle pregabalin

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Publication number Priority date Publication date Assignee Title
GB349466A (en) *
US20020139003A1 (en) * 1999-10-19 2002-10-03 Bryan David E. Centrifugal pellet dryer
CN104649919A (en) * 2015-02-10 2015-05-27 浙江华海药业股份有限公司 Preparation method of small-particle pregabalin
CN111170879A (en) * 2020-01-21 2020-05-19 石药集团中奇制药技术(石家庄)有限公司 Small-particle-size pregabalin and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB349466A (en) *
US20020139003A1 (en) * 1999-10-19 2002-10-03 Bryan David E. Centrifugal pellet dryer
CN104649919A (en) * 2015-02-10 2015-05-27 浙江华海药业股份有限公司 Preparation method of small-particle pregabalin
CN111170879A (en) * 2020-01-21 2020-05-19 石药集团中奇制药技术(石家庄)有限公司 Small-particle-size pregabalin and preparation method thereof

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