阅读说明：本技术 一种生物医药制备用析晶方法 (Crystallization method for biological medicine preparation ) 是由 不公告发明人 于 2021-08-25 设计创作，主要内容包括：本发明公开了生物医药制备用析晶方法技术领域的一种生物医药制备用析晶方法,该方法的具体步骤为：步骤一：量取需要进行析晶的生物医药溶剂；步骤二：取出足够的冷水备用；步骤三：将生物医药溶剂和冷水分别加入生物医药制备用析晶设备中；步骤四：将析晶完成后的溶液和晶体排出,收集晶体；本发明使用生物医药制备用析晶设备进行药物析晶能使得析晶筒内的溶剂快速且均匀的析出,加快析晶的效率。(The invention discloses a crystallization method for biological medicine preparation, which belongs to the technical field of crystallization methods for biological medicine preparation, and comprises the following specific steps: the method comprises the following steps: measuring a biological medicine solvent which needs to be crystallized; step two: taking out enough cold water for standby; step three: adding a biological medicine solvent and cold water into crystallization equipment for biological medicine preparation respectively; step four: discharging the solution and the crystals after the crystallization is finished, and collecting the crystals; according to the invention, the crystallization equipment for biological medicine preparation is used for medicine crystallization, so that the solvent in the crystallization cylinder can be quickly and uniformly precipitated, and the crystallization efficiency is accelerated.)

1. A crystallization method for biomedical preparation, characterized in that: the method comprises the following specific steps:

the method comprises the following steps: measuring a biological medicine solvent which needs to be crystallized;

step two: taking out enough cold water for standby;

step three: adding the biological medicine solvent and cold water into crystallization equipment respectively;

step four: discharging the solution and the crystals after the crystallization is finished, and collecting the crystals;

wherein, in the third step, the crystallization device comprises a supporting base (1), the top of the supporting base (1) is fixedly connected with a supporting frame, a crystallization reaction kettle (4) is arranged on the supporting frame, the top and the bottom of the crystallization reaction kettle (4) are respectively provided with a feeding pipe (5) and a discharging pipe (6) which are used for feeding and discharging, the top of the crystallization cylinder (4) is fixedly connected with a water storage tank (7), the bottom of the crystallization cylinder (4) and the bottom of the water storage tank (7) are jointly and rotatably connected with a rotating shaft (8), the rotating shaft (8) is positioned at the central position of the crystallization cylinder (4), the bottom end of the rotating shaft (8) penetrates through the crystallization cylinder (4) and is fixedly connected with a driving motor (9), the driving motor (9) is fixedly connected with the top of the supporting base (1), and the outer surface of the rotating shaft (8) is fixedly connected with a plurality of first connecting blocks (10), a plurality of first connecting block (10) outer end common fixedly connected with vortex siphunculus (11), set up a plurality of groups of water outlets (12) of longitudinal symmetry on vortex siphunculus (11) surface, crystallization section of thick bamboo (4) lean on the upper portion inside wall on fixedly connected with first collar (13), first collar (13) top fixedly connected with is a plurality of along first collar (13) circumference array first kicking block (14), crystallization section of thick bamboo (4) lean on the lower part inside wall on fixedly connected with second collar (15), second collar (15) bottom fixedly connected with a plurality of second kicking block (16), second kicking block (16) and first kicking block (14) staggered position, a plurality of same group delivery port (12) inboard is equipped with first slide bar (17) jointly, first slide bar (17) surface on fixedly connected with a plurality of groups of sealing block (18), a plurality of equal fixedly connected with in both ends pushes away and draws piece (19) about first slide bar (17), the top is a plurality of push away and draw piece (19) all to be located the top of first collar (13), the bottom is a plurality of push away and draw piece (19) all to be located the bottom of second collar (15), the bottom is a plurality of push away and draw the equal fixedly connected with telescopic link (20) in piece (19) bottom, fixedly connected with support frame (21) on axis of rotation (8) surface, a plurality of equal fixed connection is at the top of support frame (21) in telescopic link (20), vortex siphunculus (11) top intercommunication has rotating tube (22), rotating tube (22) are connected with the rotation intercommunication mechanism that is used for communicating storage water tank (7).

2. The crystallization method for biomedical preparation according to claim 1, wherein: the rotating communication mechanism comprises a sealing sleeve (23), a mounting groove (24) is formed in the bottom of the water storage tank (7), the sealing sleeve (23) is rotatably connected to the inner side wall of the mounting groove (24), the top end of the rotating pipe (22) penetrates through the sealing sleeve (23) and is fixedly connected with the sealing sleeve, and the rotating shaft (8) is fixedly connected with the sealing sleeve (23).

3. The crystallization method for biomedical preparation according to claim 1, wherein: the support frame includes four support post (2), four the equal fixed connection of support post (2) is at unable adjustment base (1) top, four two fixed disks (3), two of the common fixedly connected with of support post (2) fixed disk (3) inside wall and crystallization reation kettle (4) fixed connection.

4. The crystallization method for biomedical preparation according to claim 1, wherein: every group sealed piece (18) bottom all is equipped with and rotates shunting block (25) of connection on first slide bar (17) surface, and is a plurality of shunting block (25) is all the same apart from sealed piece (18) of its top apart from equal, a plurality of equal fixedly connected with agitator disk (26) on shunting block (25) bottom lateral wall, and is a plurality of equal fixedly connected with thrust plate (27) on shunting block (25) top surface, thrust plate (27) are used for being strikeed by cold water and drive shunting block (25) and rotate.

5. The crystallization method for biomedical preparation according to claim 4, wherein: the utility model discloses a crystallization device, including axis of rotation (8), axis of rotation (8) outer surface is gone up fixedly connected with a plurality of groups and is followed stirring rod (28) that axis of rotation (8) vertical direction linear array arranged, and three stirring rod (28) are a set of, the group number of stirring rod (28) is the same with the quantity of head rod (10), and every stirring rod of group (28) and head rod (10) all use axis of rotation (8) center pin to arrange on axis of rotation (8) lateral wall as central circular array, the inside wall contact of stirring piece (28) outer end and crystallization cylinder (4).

6. The crystallization method for biomedical preparation according to claim 5, wherein: the top and the below are with organizing common the first support ring of common fixedly connected with (29), two between stirring piece (28) rotate jointly between first support ring (29) and be connected with a plurality of first bull stick (30), and is a plurality of equal fixedly connected with keeps off dish (31) on first bull stick (30) bottom surface, keep off dish (31) bottom fixedly connected with torsional spring (32), torsional spring (32) bottom fixed connection is at first support ring (29) top, and is a plurality of equal fixedly connected with dials board (33) on first bull stick (30) surface, dial board (33) and agitator disk (26) contact.

7. The crystallization method for biomedical preparation according to claim 1, wherein: every group top the equal fixedly connected with of sealed piece (18) top divides shell (34), divide shell (34) with sealed piece (18) is inside to have seted up water spray through-hole (35), water spray through-hole (35) inboard is all pegged graft and is had sealed slide bar (36), and is a plurality of the solid fixed ring (37) of the common fixedly connected with in sealed slide bar (36) bottom, gu all fixedly connected with L type link (38) on fixed ring (37) exterior wall, the equal fixed connection of L type link (38) is on the inside wall of vortex siphunculus (11).

Technical Field

The invention relates to the technical field of crystallization methods for biological medicine preparation, in particular to a crystallization method for biological medicine preparation.

Background

For the biological medicine prepared step by solution reaction, after the reaction is finished, the solution needs to be cooled and crystallized until a corresponding product is obtained, two different effects can be obtained by adopting two modes generally, firstly, when cold water or ice water is used for rapidly cooling and the solution is stirred vigorously, crystals with small particles can be obtained; the other is to let the hot solution stand at an air temperature to slowly cool the solution, so as to obtain a uniform and large product.

The prior art discloses an invention patent in the aspect of a crystallization method for preparing a part of biological medicines, and a Chinese patent with the patent application number of CN201922322976.1, and discloses a crystallization device for preparing the biological medicines, which comprises the following steps: the reaction component is used for preparing a cavity during crystallization by using the biological medicine; the lifting mechanism is arranged on the reaction assembly; the water storage component is positioned right above the reaction component, arranged on the lifting mechanism and used for storing cooling water for crystallization; the rotating mechanism is arranged on the water storage component, so that the cooling water in the water storage component is dripped into the reaction component, and the biological medicine in the reaction component is stirred when the cooling water is dripped.

In the prior art, when crystallization equipment for preparing the biological medicine is used for crystallization, cold water is slowly dripped into the crystallization equipment from the top of the crystallization equipment, the cold water can be firstly contacted with a solvent at the top in the crystallization equipment and cannot be quickly and uniformly mixed with the solvent in the crystallization equipment, so that the crystallization is carried out at the top, the phenomenon of nonuniform crystallization of a reaction product is easy to occur, and the crystallization preparation of the biological medicine is influenced.

Based on this, the invention designs a crystallization method for preparing biological medicine, so as to solve the problems.

Disclosure of Invention

The invention aims to provide a crystallization method for preparing a biological medicine, and aims to solve the problems that in the prior art, when crystallization equipment for preparing the biological medicine is used for crystallization treatment, cold water is slowly dripped into the crystallization equipment from the top of the crystallization equipment, the cold water can be contacted with a solvent at the top in the crystallization equipment firstly, cannot be quickly and uniformly mixed with the solvent in the crystallization equipment, so that the crystallization is carried out at the top firstly, the phenomenon of nonuniform crystallization of a reaction product is easy to occur, and the crystallization preparation of the biological medicine is influenced.

In order to achieve the purpose, the invention provides the following technical scheme: a crystallization method for preparing biological medicine comprises the following specific steps:

the method comprises the following steps: measuring a biological medicine solvent which needs to be crystallized;

step two: taking out enough cold water for standby;

step three: adding the biological medicine solvent and cold water into crystallization equipment respectively;

step four: discharging the solution and the crystals after the crystallization is finished, and collecting the crystals;

wherein, in the third step, the crystallization device comprises a supporting base, the top of the supporting base is fixedly connected with a supporting frame, the supporting frame is provided with a crystallization reaction kettle, the top and the bottom of the crystallization reaction kettle are respectively provided with a feeding pipe and a discharging pipe for feeding and discharging, the top of the crystallization cylinder is fixedly connected with a water storage tank, the bottom of the crystallization cylinder and the bottom of the water storage tank are jointly and rotatably connected with a rotating shaft, the rotating shaft is positioned at the central position of the crystallization cylinder, the bottom end of the rotating shaft penetrates through the crystallization cylinder and is fixedly connected with a driving motor, the driving motor is fixedly connected with the top of the supporting base, the outer surface of the rotating shaft is fixedly connected with a plurality of first connecting blocks, the outer ends of the first connecting blocks are jointly and fixedly connected with a vortex through pipe, the outer surface of the vortex through pipe is provided with a plurality of groups of vertically symmetrical water outlets, and the inner side wall of the upper portion of the crystallization cylinder is fixedly connected with a first mounting ring, the top of the first mounting ring is fixedly connected with a plurality of first ejector blocks along a first mounting ring circumferential array, the devitrification cylinder is fixedly connected with a second mounting ring on the inner side wall of the lower portion, the bottom of the second mounting ring is fixedly connected with a plurality of second ejector blocks, the second ejector blocks and the first ejector blocks are staggered, a plurality of groups of the inner sides of the water outlets are jointly provided with a first slide bar, the outer surface of the first slide bar is fixedly connected with a plurality of groups of sealing blocks, the upper end and the lower end of the first slide bar are fixedly connected with push-pull blocks, the top of the push-pull blocks are all positioned at the top of the first mounting ring, the bottom of the push-pull blocks are all positioned at the bottom of the second mounting ring, the bottom of the push-pull blocks are all fixedly connected with telescopic rods, the outer surface of the rotating shaft is fixedly connected with a support frame, and the telescopic rods are all fixedly connected at the top of the support frame, the top of the vortex through pipe is communicated with a rotating pipe, and the rotating pipe is connected with a rotating communication mechanism for communicating a water storage tank;

the rotary communication mechanism comprises a sealing sleeve, a mounting groove is formed in the bottom of the water storage tank, the sealing sleeve is rotatably connected to the inner side wall of the mounting groove, the top end of the rotary pipe penetrates through the sealing sleeve and is fixedly connected with the sealing sleeve, and the rotary shaft is fixedly connected with the sealing sleeve;

the support frame comprises four support stand columns, the four support stand columns are all fixedly connected to the top of the fixed base, the four support stand columns are jointly and fixedly connected with two fixed discs, and the inner side walls of the two fixed discs are fixedly connected with the crystallization reaction kettle;

when the device works, because cold water is slowly dripped into the crystallization device from the top of the crystallization device when the crystallization device for biological medicine preparation is used for crystallization treatment in the prior art, the cold water can be firstly contacted with a solvent at the top in the crystallization device and can not be quickly and uniformly mixed with the solvent in the crystallization device, so that crystallization is carried out at the top first, the phenomenon of nonuniform crystallization of a reaction product is easy to occur, and the crystallization preparation of the biological medicine is influenced. The rotating shaft is driven to rotate, the rotating shaft drives the vortex through pipe to rotate together through the first connecting block, meanwhile, the rotating pipe drives the sealing sleeve to rotate, so that the sealing sleeve rotates in the water storage tank, the rotating pipe is always communicated with the water storage tank, cold water in the water storage tank can continuously flow into the vortex through pipe, the supply of the cold water is guaranteed, in addition, when the vortex through pipe rotates, the first sliding rod and the plurality of groups of sealing blocks are driven to rotate simultaneously through the supporting frame and the telescopic rod, the push-pull blocks at the upper end and the lower end of the first sliding rod respectively rotate along the top of the first mounting ring and the bottom of the second mounting ring, the first jacking block and the second jacking block are arranged in a staggered mode, when the push-pull block at the top is slowly lifted up in contact with the first jacking block, the push-pull block at the bottom is separated from the second jacking block in advance, the first sliding rod and the sealing blocks are driven to slowly lift up, the telescopic rod is stretched, so that the two sealing blocks are separated from the water outlet, the water outlet is opened, cold water in the vortex through pipe begins to be discharged from the water outlet crystallization cylinder, a plurality of water outlets arranged along the surface of the vortex through pipe extend out of the interior of a reagent to be treated, when the cold water flows out of the water outlets, the cold water can be rapidly and uniformly distributed in a solvent to be treated under the action of the vortex through pipe which rotates ceaselessly and water outlets at different positions, the solvent in the crystallization cylinder is rapidly stirred by utilizing the first connecting block, the first sliding rod and the vortex through pipe to accelerate the cold water to flow to all parts in the solvent, so that the solvents with different heights in the solvent can be uniformly contacted with the cold water, the phenomenon that partial areas are contacted with the cold water in advance to crystallize is avoided, the crystallization speed of the solvent is accelerated, when the push-pull block at the top moves on the first top block for a certain distance, and after the water outlet discharges the cold water for a certain time, the push-pull block at the top is separated from the first top block, the push-pull block at the bottom starts to contact with the second top block at the bottom, so that the first slide rod and the sealing block slide downwards again, the sealing block seals the water outlet of the vortex communicating pipe again, water is prevented from continuously flowing out from the water outlet, cold water can be mixed into a solvent for enough time, a certain crystallization time is given to a solution, the phenomenon that the crystallization cylinder is filled with the cold water due to too fast addition is avoided, sufficient crystallization time is given, the solution can be crystallized more completely, the first slide rod and the sealing block move up and down along with the continuous rotation of the rotating shaft, the sealing block alternately opens and seals the water outlet, the solution in the crystallization cylinder is crystallized rapidly and uniformly, after the crystallization is completed, the discharge valve is opened, the precipitated crystals and the liquid are discharged, the crystals are collected and the crystallization is completed, and therefore, when the crystallization method is required to be used for preparing the biological medicines each time, the vortex-type crystallization device is characterized in that a vortex of a vortex through pipe is arranged in a crystallization cylinder, a plurality of water outlets are formed in the outer surface of the vortex through pipe, the water outlets at different positions on the vortex through pipe are utilized, a first top block, a second top block, a push-pull block, a first slide bar and a sealing block are matched to open and close the water outlets in a staggered mode, cold water in the vortex through pipe is rapidly and uniformly distributed at each part in the crystallization cylinder, and a solvent in the crystallization cylinder is driven to flow rapidly when the first connecting block, the first slide bar and the vortex through pipe rotate to be separated out rapidly and uniformly, so that the solvent in the crystallization cylinder is separated out rapidly and uniformly, the crystallization efficiency is accelerated, and the phenomenon that the solvent in a part of area is cooled and crystallized in advance and is not uniform is avoided.

As a further scheme of the invention, the bottom of each group of sealing blocks is provided with a shunting block rotatably connected to the outer surface of the first sliding rod, the distance between the plurality of shunting blocks and the sealing block above the shunting blocks is the same, the outer side wall of the bottom of each shunting block is fixedly connected with a stirring disc, the outer surface of the top of each shunting block is fixedly connected with a flow pushing plate, and the flow pushing plate is used for being impacted by cold water to drive the shunting blocks to rotate; when the device works, because the cold water flowing out of the water outlet at each time is directly discharged into the crystallization cylinder, the discharged cold water is collected and is not beneficial to the rapid and uniform distribution of the cold water in a solvent, the flow splitting block is fixedly connected with the bottom of the sealing block, when the sealing block at the bottom is driven to slide into the vortex through pipe, the flow splitting block is driven to simultaneously move to the bottom of the water outlet, the cold water is discharged downwards from the water outlet and impacts the flow pushing plate, so that the flow pushing plate and the flow splitting block rotate to drive the stirring disc at the bottom of the flow splitting block to rotate, the discharged cold water is directly guided and dispersed by the rotating flow splitting block and rapidly diffused to the periphery of the solvent, and the dispersed cold water is rapidly mixed with the solution by the rotating stirring disc to accelerate the mixing and melting of the cold water into the solvent, thereby realizing the rapid dispersion of the cold water after the cold water is discharged from the water outlet of the vortex through pipe, and rapid and uniform mixing with the solvent, is beneficial to the uniform and rapid crystallization of the solvent and improves the crystallization efficiency.

As a further scheme of the invention, a plurality of groups of stirring rods which are linearly arranged in an array along the vertical direction of the rotating shaft are fixedly connected to the outer surface of the rotating shaft, the number of the groups of the three stirring rods is the same as that of the first connecting rods, each group of the stirring rods and one first connecting rod are circularly arranged on the side wall of the rotating shaft in an array by taking the central shaft of the rotating shaft as the center, and the outer end of each stirring block is contacted with the inner side wall of the crystallization cylinder; the during operation, because when crystallization at every turn, need carry out quick stirring to the solvent, it is quick to be used for accelerating cold water, evenly and melt into the solvent, through a plurality of stirring pieces of fixedly connected with on the axis of rotation surface, and the outer end of stirring piece contacts with the inside wall of crystallization section of thick bamboo, furthest's the scope of expansion stirring, and the stirring piece that arranges from top to bottom can not interfere with vortex siphunculus and first connecting block, make the stirring piece, first connecting block and vortex siphunculus can be quick, more thorough stirs the solvent, the biggest spacing quickening cold water mixes with the solvent, make the crystal of appearing more even.

As a further scheme of the invention, a first support ring is fixedly connected between the uppermost and lowermost stirring blocks in the same group, a plurality of first rotating rods are rotatably connected between the two first support rings, the outer surfaces of the bottoms of the first rotating rods are fixedly connected with baffle discs, the bottoms of the baffle discs are fixedly connected with torsional springs, the bottom ends of the torsional springs are fixedly connected to the tops of the first support rings, the outer surfaces of the first rotating rods are fixedly connected with stirring plates, and the stirring plates are in contact with the stirring discs; when the stirring plate is separated from the stirring plate, the torsion spring enables the baffle plate, the first rotating rod and the stirring plate to reset and to be contacted with the stirring plate again, and the stirring plate continuously rotates along with the continuous rotation of the stirring plate, so that the stirring plate continuously swings to accelerate the mixing of cold water and a solvent at the center of the crystallization barrel, and the quick and uniform crystallization of the solvent is facilitated.

As a further scheme of the invention, the top of the sealing block above each group is fixedly connected with a shunting shell, water spraying through holes are formed in the shunting shell and the sealing block, sealing slide bars are inserted into the inner sides of the water spraying through holes, the bottom ends of the sealing slide bars are fixedly connected with a fixing ring together, the outer surface wall of the fixing ring is fixedly connected with an L-shaped connecting frame, and the L-shaped connecting frames are fixedly connected on the inner side wall of the vortex through pipe; when the device works, because the cold water flowing out of the water outlet at the top of the vortex through pipe is also in a gathering state and cannot be quickly mixed into the solvent, the cold water passes through the diversion shell fixedly connected with the top of the sealing block at the top, when the first slide bar drives the sealing block to move upwards, the sealing block drives the diversion shell to be separated from the vortex through pipe, so that the water spraying through hole in the sealing block is separated from the sealing slide bar, the sealing slide bar is fixedly connected with the vortex through pipe through an L-shaped connecting frame and does not move, so that the water spraying through hole is opened, the cold water sprayed out of the water outlet is partially dispersed by the diversion shell and diffused to the periphery of the crystallization cylinder, and partially flows out of the water spraying through hole and is directly discharged upwards, so that the distributed cold water is more dispersed and can cover more solvents, when the sealing block slides down to seal the water outlet after water is discharged, the sealing slide bar is inserted into the water spraying through hole again to seal the water spraying through hole, the sealing effect of the sealing block is ensured, so that cold water discharged from the top can be rapidly dispersed, and the crystallization speed is accelerated in a solvent needing crystallization, so that the crystallization is more uniform.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, when the crystallization method is required to be used for preparing the biological medicine each time, the vortex of the vortex through pipe is arranged in the crystallization cylinder, the outer surface of the vortex through pipe is provided with a plurality of water outlets, the water outlets at different positions on the vortex through pipe are used, and the first top block, the second top block, the push-pull block, the first slide bar and the sealing block are matched to open and close the water outlets in a staggered manner, so that cold water in the vortex through pipe is rapidly and uniformly distributed at each part in the crystallization cylinder, and the first connecting block, the first slide bar and the vortex through pipe are used for driving the solvent in the crystallization cylinder to rapidly flow when the vortex rotates, so that the solvent in the crystallization cylinder is rapidly and uniformly separated out, the crystallization efficiency is accelerated, and the phenomena of premature cooling crystallization of the solvent in partial areas and non-uniform crystallization of the solvent are avoided.

2. According to the invention, the diversion block is fixedly connected to the bottom of the sealing block, when the sealing block at the bottom is driven to slide into the vortex through pipe, the diversion block is driven to move at the bottom of the water outlet, cold water is discharged downwards from the water outlet, the diversion block is impacted to rotate the diversion plate and the diversion block, the stirring disc at the bottom of the diversion block is driven to rotate, the discharged cold water is directly guided and dispersed by the rotating diversion block and quickly diffused to the periphery of the solvent, and the dispersed cold water is quickly mixed with the solution by utilizing the rotating stirring disc, so that the cold water is quickly mixed and melted into the solvent, and therefore, the cold water can be quickly dispersed after being discharged from the water outlet of the vortex through pipe, and is quickly and uniformly mixed with the solvent, the uniform and quick crystallization of the solvent is facilitated, and the crystallization efficiency is improved.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a flow chart of the steps of the crystallization method of the present invention;

FIG. 2 is a first perspective view of the overall construction of the present invention;

FIG. 3 is a second perspective cross-sectional view of the general construction of the invention;

FIG. 4 is a sectional view showing the internal structure of a crystallization cylinder according to the present invention;

FIG. 5 is an enlarged view of the structure at A in FIG. 4;

FIG. 6 is a schematic view of a second mounting ring and support bracket configuration of the present invention;

FIG. 7 is an enlarged view of the structure at B in FIG. 6;

FIG. 8 is a schematic view of the vortex through pipe and the water outlet according to the present invention;

fig. 9 is an enlarged view of the structure at C in fig. 8.

In the drawings, the components represented by the respective reference numerals are listed below:

the device comprises a supporting base 1, a supporting upright post 2, a fixed disc 3, a crystallization barrel 4, a feeding pipe 5, a discharge valve 6, a water storage tank 7, a rotating shaft 8, a driving motor 9, a first connecting block 10, a vortex through pipe 11, a water outlet 12, a first mounting ring 13, a first top block 14, a second mounting ring 15, a second top block 16, a first sliding rod 17, a sealing block 18, a push-pull block 19, a telescopic rod 20, a supporting frame 21, a rotating pipe 22, a sealing sleeve 23, a mounting groove 24, a shunting block 25, a stirring disc 26, a push-flow plate 27, a stirring block 28, a first supporting ring 29, a first rotating rod 30, a baffle disc 31, a torsion spring 32, a poking plate 33, a shunting shell 34, a water spraying through hole 35, a sealing sliding rod 36, a fixing ring 37 and an L-shaped connecting frame 38.

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. 1-9, the present invention provides a technical solution: a crystallization method for preparing biological medicine comprises the following specific steps:

the method comprises the following steps: measuring a biological medicine solvent which needs to be crystallized;

step two: taking out enough cold water for standby;

step three: adding the biological medicine solvent and cold water into crystallization equipment respectively;

step four: discharging the solution and the crystals after the crystallization is finished, and collecting the crystals;

wherein, the crystallization device in the third step comprises a supporting base 1, the top of the supporting base 1 is fixedly connected with a supporting frame, a crystallization reaction kettle 4 is arranged on the supporting frame, the top and the bottom of the crystallization reaction kettle 4 are respectively provided with a feeding pipe 5 and a discharging pipe 6 for feeding and discharging, the top of the crystallization cylinder 4 is fixedly connected with a water storage tank 7, the bottom of the crystallization cylinder 4 and the bottom of the water storage tank 7 are jointly and rotatably connected with a rotating shaft 8, the rotating shaft 8 is positioned at the central position of the crystallization cylinder 4, the bottom end of the rotating shaft 8 penetrates through the crystallization cylinder 4 and is fixedly connected with a driving motor 9, the driving motor 9 is fixedly connected with the top of the supporting base 1, the outer surface of the rotating shaft 8 is fixedly connected with a plurality of first connecting blocks 10, the outer ends of the first connecting blocks 10 are jointly and fixedly connected with a vortex communicating pipe 11, the outer surface of the vortex 11 is provided with a plurality of groups of vertically symmetrical water outlets 12, the inner side wall of the upper portion of the crystallization cylinder 4 is fixedly connected with a first mounting ring 13, the top of the first mounting ring 13 is fixedly connected with a plurality of first ejector blocks 14 arrayed along the circumference of the first mounting ring 13, the inner side wall of the lower part of the crystallizer 4 is fixedly connected with a second mounting ring 15, the bottom of the second mounting ring 15 is fixedly connected with a plurality of second ejector blocks 16, the second ejector blocks 16 and the first ejector blocks 14 are staggered, a plurality of groups of water outlets 12 are provided with a first slide bar 17 together, the outer surface of the first slide bar 17 is fixedly connected with a plurality of groups of sealing blocks 18, the upper and lower ends of the first slide bars 17 are fixedly connected with push-pull blocks 19, a plurality of push-pull blocks 19 at the top are all positioned at the top of the first mounting ring 13, a plurality of push-pull blocks 19 at the bottom are all positioned at the bottom of the second mounting ring 15, the bottoms of a plurality of push-pull blocks 19 at the bottom are all fixedly connected with telescopic rods 20, the outer surface of the rotating shaft 8 is fixedly connected with a support frame 21, and a plurality of telescopic rods 20 are all fixedly connected at the top of the support frame 21, the top of the vortex through pipe 11 is communicated with a rotating pipe 22, and the rotating pipe 22 is connected with a rotating communicating mechanism for communicating the water storage tank 7;

the rotary communication mechanism comprises a sealing sleeve 23, the bottom of the water storage tank 7 is provided with a mounting groove 24, the sealing sleeve 23 is rotatably connected to the inner side wall of the mounting groove 24, the top end of the rotary pipe 22 penetrates through the sealing sleeve 23 and is fixedly connected with the sealing sleeve 23, and the rotary shaft 8 is fixedly connected with the sealing sleeve 23;

the support frame comprises four support columns 2, the four support columns 2 are all fixedly connected to the top of the fixed base 1, the four support columns 2 are jointly and fixedly connected with two fixed discs 3, and the inner side walls of the two fixed discs 3 are fixedly connected with the crystallization reaction kettle 4;

when the device works, because cold water is slowly dripped into the crystallization device from the top of the crystallization device when the crystallization device for biological medicine preparation is used for crystallization treatment in the prior art, the cold water can be firstly contacted with a solvent at the top in the crystallization device and can not be quickly and uniformly mixed with the solvent in the crystallization device, so that crystallization is carried out at the top first, the phenomenon of nonuniform crystallization of a reaction product is easy to occur, and the crystallization preparation of biological medicines is influenced, the invention provides a technical scheme for solving the above problems, when the device is used, a medicament needing crystallization treatment is firstly added into a crystallization barrel 4 from a feeding pipe 5, and cold water is added into a water outlet tank, at the moment, a water outlet 12 on the outer surface of a vortex through pipe 11 is sealed by a sealing block 18, the cold water added into a water storage tank 7 flows into the vortex through pipe 11 through a rotating pipe 22 and is filled in the vortex through pipe 11, then, a driving motor 9 is started to drive a rotating shaft 8 to rotate, the rotating shaft 8 drives a vortex through pipe 11 to rotate together through a first connecting block 10, meanwhile, a rotating pipe 22 drives a sealing sleeve 23 to rotate, the sealing sleeve 23 rotates in a water storage tank 7, the rotating pipe 22 is ensured to be communicated with the water storage tank 7 all the time, cold water in the water storage tank 7 can continuously flow into the vortex through pipe 11, the supply of the cold water is ensured, when the vortex through pipe 11 rotates, a first sliding rod 17 and a plurality of groups of sealing blocks 18 are driven to rotate simultaneously through a supporting frame 21 and a telescopic rod 20, push-pull blocks 19 at the upper end and the lower end of the first sliding rod 17 respectively rotate along the top of a first mounting ring 13 and the bottom of a second mounting ring 15, the first top block 14 and the second top block 16 are arranged in a staggered mode, when the push-pull block 19 at the top is in contact with the first top block 14 and is slowly lifted, the push-pull block 19 at the bottom is separated from the second top block 16 in advance, the first sliding rod 17 and the sealing blocks 18 are driven to slowly rise, the telescopic rod 20 is stretched to separate the two sealing blocks 18 from the water outlet 12, the water outlet 12 is opened, cold water in the vortex through pipe 11 begins to be discharged from the crystal separation barrel 4 of the water outlet 12, a plurality of water outlets 12 arranged along the surface of the vortex through pipe 11 extend out of the reagent to be treated, when the cold water flows out of the water outlet 12, the cold water can be rapidly and uniformly distributed in the solvent to be treated under the action of the vortex through pipe 11 which rotates ceaselessly and the water outlets 12 which are different in position, the solvent in the crystal separation barrel 4 is rapidly stirred by using the first connecting block 10, the first sliding rod 17 and the vortex through pipe 11 which rotate ceaselessly, cold water is accelerated to flow to each position in the solvent, so that the solvents with different heights in the solvent can uniformly contact with the cold water, and the phenomenon that partial areas are not uniformly crystallized by contacting the cold water in advance is avoided, accelerating the crystallization speed of the solvent, after the top push-pull block 19 moves a certain distance on the first top block 14, the water outlet 12 discharges cold water for a certain time, the top push-pull block 19 is separated from the first top block 14, the bottom push-pull block 19 starts to contact with the bottom second top block 16, so that the first sliding rod 17 and the sealing block 18 slide downwards again, the sealing block 18 seals the water outlet 12 of the vortex through pipe 11 again, the water outlet 12 is prevented from continuously discharging water, the cold water can be mixed into the solvent for a sufficient time, the solution is given a certain crystallization time, the phenomenon that the crystallization cylinder 4 is filled with the cold water due to too fast addition is avoided, the sufficient crystallization time is given, the solution can be more completely crystallized, and similarly, the first sliding rod 17 and the sealing block 18 continuously move up and down along with the continuous rotation of the rotating shaft 8, so that the sealing block 18 alternately opens and seals the water outlet 12, the method comprises the steps of carrying out rapid and uniform crystallization on a solution in a crystallization barrel 4, opening a discharge valve 6 after crystallization is finished, discharging precipitated crystals and liquid, collecting the crystals, and finishing crystallization, so that when the crystallization method is required to be used for preparing the biological medicine each time, a vortex through pipe 11 is arranged in the crystallization barrel 4 in a vortex manner, a plurality of water outlets 12 are formed in the outer surface of the vortex through pipe 11, the water outlets 12 at different positions on the vortex through pipe 11 are utilized, a first top block 14, a second top block 16, a push-pull block 19, a first slide bar 17 and a sealing block 18 are matched to open and close the water outlets 12 in a staggered manner, cold water in the vortex through pipe 11 is rapidly and uniformly distributed at each part in the crystallization barrel 4, and a solvent in the crystallization barrel 4 is driven to rapidly flow when a first connecting block 10, a first slide bar 17 and the vortex through pipe 11 rotate, so that the solvent in the crystallization barrel 4 is rapidly and uniformly precipitated, the crystallization efficiency is accelerated, and the phenomena that the solvent is cooled and crystallized in advance in partial areas and the solvent is not uniformly crystallized are avoided.

As a further scheme of the invention, the bottom of each group of sealing blocks 18 is provided with a shunting block 25 which is rotatably connected to the outer surface of the first sliding rod 17, the distance between the plurality of shunting blocks 25 and the sealing block 18 above the shunting blocks is the same, the outer side walls of the bottoms of the plurality of shunting blocks 25 are fixedly connected with stirring discs 26, the outer surfaces of the tops of the plurality of shunting blocks 25 are fixedly connected with thrust plates 27, and the thrust plates 27 are used for driving the shunting blocks 25 to rotate by being impacted by cold water; when the device works, because the cold water flowing out of the water outlet 12 at each time is directly discharged into the crystallization cylinder 4, the discharged cold water is collected and is not beneficial to the rapid and uniform distribution of the cold water in a solvent, the diversion block 25 is fixedly connected to the bottom of the sealing block 18, when the sealing block 18 at the bottom is driven to slide into the vortex through pipe 11, the diversion block 25 is driven to move at the bottom of the water outlet 12 at the same time, the cold water is discharged downwards from the water outlet 12, the diversion block 27 is impacted, the diversion block 27 and the diversion block 25 rotate to drive the stirring disc 26 at the bottom of the diversion block 25 to rotate, the rotating diversion block 25 enables the discharged cold water to be directly guided and dispersed to be rapidly diffused to the periphery of the solvent, the dispersed cold water is rapidly mixed with the solution by the rotating stirring disc 26 to accelerate the mixing and melting of the cold water into the solvent, and the rapid dispersion of the cold water after the cold water is discharged from the water outlet 12 of the vortex through pipe 11 is realized, the solvent is quickly and uniformly mixed with the solvent, so that the uniform and quick crystallization of the solvent is facilitated, and the crystallization efficiency is improved.

As a further scheme of the invention, a plurality of groups of stirring rods 28 which are arranged in a linear array along the vertical direction of the rotating shaft 8 are fixedly connected on the outer surface of the rotating shaft 8, three stirring rods 28 form one group, the number of the groups of the stirring rods 28 is the same as that of the first connecting rods 10, each group of the stirring rods 28 and one first connecting rod 10 are arranged on the side wall of the rotating shaft 8 in a circular array by taking the central shaft of the rotating shaft 8 as the center, and the outer end of each stirring block 28 is contacted with the inner side wall of the crystallization cylinder 4; the during operation, because when crystallization at every turn, need carry out quick stirring to the solvent, it is quick to be used for accelerating cold water, even and melt into the solvent, through a plurality of stirring pieces 28 of fixedly connected with on 8 surfaces of axis of rotation, and the outer end of stirring piece 28 contacts with the inside wall of crystallization barrel 4, furthest's scope of expanding the stirring, and the stirring piece 28 that arranges from top to bottom can not interfere with vortex siphunculus 11 and first connecting block 10, make stirring piece 28, first connecting block 10 and vortex siphunculus 11 can be quick, more thorough stirs the solvent, the biggest spacing acceleration cold water and solvent mix, make the crystal of appearing more even.

As a further scheme of the invention, the first supporting rings 29 are fixedly connected between the same group of stirring blocks 28 at the top and the bottom together, a plurality of first rotating rods 30 are rotatably connected between the two first supporting rings 29 together, the outer surfaces of the bottoms of the first rotating rods 30 are fixedly connected with baffle discs 31, the bottoms of the baffle discs 31 are fixedly connected with torsional springs 32, the bottom ends of the torsional springs 32 are fixedly connected to the tops of the first supporting rings 29, the outer surfaces of the first rotating rods 30 are fixedly connected with stirring plates 33, and the stirring plates 33 are contacted with the stirring discs 26; during operation, only the stirring blocks 28 which are alternately arranged up and down exist at the central position close to the rotating shaft 8 in the crystallization cylinder 4 for stirring, cold water cannot rapidly reach the central position of the crystallization cylinder 4, when the cold water is discharged to drive the shunting blocks 25 and the stirring disc 26 to rotate, the stirring disc 26 is driven to rotate, the stirring plate 33 is pushed to enable the first rotating rod 30 to rotate, the torsion spring 32 is twisted, the stirring plate 33 is finally rotated, the cold water flowing out of the shunting blocks 25 is stirred towards the center of the crystallization cylinder 4, the cold water is accelerated to enter the central position of the crystallization cylinder 4, after the stirring plate 33 is separated from the stirring disc 26, the torsion spring 32 enables the blocking disc 31, the first rotating rod 30 and the stirring plate 33 to reset and to be contacted with the stirring disc 26 again, the stirring plate 33 continuously swings along with the continuous rotation of the stirring disc 26, the mixing of the cold water and a solvent at the center of the crystallization cylinder 4 is accelerated, and the rapid solvent is facilitated, Uniform crystallization.

As a further scheme of the invention, the top of each group of upper sealing blocks 18 is fixedly connected with a shunt shell 34, the interior of the shunt shell 34 and the interior of the sealing blocks 18 are provided with water spraying through holes 35, the inner sides of the water spraying through holes 35 are all inserted with sealing slide bars 36, the bottom ends of the sealing slide bars 36 are jointly and fixedly connected with a fixing ring 37, the outer surface wall of the fixing ring 37 is fixedly connected with an L-shaped connecting frame 38, and the L-shaped connecting frames 38 are all fixedly connected on the inner side wall of the vortex through pipe 11; when the device works, because the cold water flowing out from the water outlet 12 at the top of the vortex through pipe 11 is also in a gathering state and cannot be quickly mixed into the solvent, the cold water passes through the diversion shell 34 fixedly connected with the top of the sealing block 18 at the top, when the first slide bar 17 drives the sealing block 18 to move upwards, the sealing block 18 drives the diversion shell 34 to be separated from the vortex through pipe 11, so that the water spraying through hole 35 in the sealing block 18 is separated from the sealing slide bar 36, the sealing slide bar 36 is fixedly connected with the vortex through pipe 11 through the L-shaped connecting frame 38 and does not move, so that the water spraying through hole 35 is opened, part of the cold water sprayed out from the water outlet 12 is scattered by the diversion shell 34 and is diffused to the periphery of the crystallization cylinder 4, part of the cold water flows out from the water spraying through hole 35 and is directly discharged upwards, so that the distributed cold water is more dispersed, and more solvent can be covered, when the sealing block 18 slides down to the sealed water outlet 12 after water outlet is finished, the sealing slide rod 36 is inserted into the water spraying through hole 35 again to seal the water spraying through hole 35, so that the sealing effect of the sealing block 18 is ensured, cold water discharged from the top can be rapidly dispersed, the crystallization speed is accelerated in a solvent needing crystallization, and the crystallization is more uniform.

The working principle is as follows: when the invention is used, firstly, the medicament to be subjected to crystallization treatment is added into the crystallization barrel 4 from the feeding pipe 5, and cold water is added into the water outlet tank, at the moment, the water outlet 12 on the outer surface of the vortex through pipe 11 is sealed by the sealing block 18, the cold water added into the water storage tank 7 flows into the vortex through pipe 11 through the rotating pipe 22 to fill the vortex through pipe 11, then the driving motor 9 is started to drive the rotating shaft 8 to rotate, the rotating shaft 8 drives the vortex through pipe 11 to rotate together through the first connecting block 10, meanwhile, the rotating pipe 22 drives the sealing sleeve 23 to rotate, so that the sealing sleeve 23 rotates in the water storage tank 7, the rotating pipe 22 is ensured to be always communicated with the water storage tank 7, the cold water in the water storage tank 7 can continuously flow into the vortex through pipe 11, the supply of the cold water is ensured, and when the vortex through pipe 11 rotates, the first sliding rod 17 and the groups of sealing blocks 18 are driven to rotate simultaneously through the supporting frame 21 and the telescopic rod 20, the push-pull blocks 19 at the upper end and the lower end of the first slide bar 17 respectively rotate along the top of the first mounting ring 13 and the bottom of the second mounting ring 15, the first top block 14 and the second top block 16 are arranged in a staggered manner, when the push-pull block 19 at the top is contacted with the first top block 14 and is slowly lifted, the push-pull block 19 at the bottom is separated from the second top block 16 in advance, the first slide bar 17 and the sealing block 18 are driven to slowly lift, the telescopic rod 20 is stretched, the two sealing blocks 18 are separated from the water outlet 12, the water outlet 12 is opened, cold water in the vortex through pipe 11 starts to be discharged from the crystallization cylinder 4 at the water outlet 12, a plurality of water outlets 12 arranged along the surface of the vortex through pipe 11 extend out of a reagent to be processed, when the cold water flows out from the water outlet 12, the cold water can be rapidly and uniformly distributed into the solvent to be processed under the action of the vortex through pipe 11 which continuously rotates and the water outlets 12 at different positions, and the first connecting block 10, the first slide bar 17 and the vortex through pipe 11 are utilized to rotate ceaselessly to quickly stir the solvent in the crystallization cylinder 4, so that cold water flows to all parts in the solvent, the solvents with different heights in the solvent can be uniformly contacted with the cold water, the phenomenon that partial areas are contacted with the cold water in advance for crystallization in advance to generate non-uniformity is avoided, the crystallization speed of the solvent is accelerated, when the push-pull block 19 at the top moves for a certain distance on the first top block 14, the push-pull block 19 at the top is separated from the first top block 14 after the cold water at a certain time is discharged from the water outlet 12, the push-pull block 19 at the bottom starts to be contacted with the second top block 16 at the bottom, the first slide bar 17 and the sealing block 18 slide downwards again, the sealing block 18 seals the water outlet 12 of the vortex through pipe 11 again, the continuous water outlet 12 water is avoided, the cold water can be mixed into the solvent for a certain crystallization time, the phenomenon that the crystallization cylinder 4 is filled with the excessive cold water is avoided, the more thorough crystallization of the solution can be ensured, similarly, the first sliding rod 17 and the sealing block 18 continuously move up and down along with the continuous rotation of the rotating shaft 8, so that the sealing block 18 alternately opens and seals the water outlet 12, the solution in the crystallization cylinder 4 is rapidly and uniformly crystallized, after the crystallization is finished, the discharge valve 6 is opened, the precipitated crystals and the liquid are discharged, the crystals are collected, and the crystallization is finished.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.