CN220918196U - Integrated micromolecular drug recrystallization device - Google Patents
Integrated micromolecular drug recrystallization device Download PDFInfo
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- CN220918196U CN220918196U CN202321968927.5U CN202321968927U CN220918196U CN 220918196 U CN220918196 U CN 220918196U CN 202321968927 U CN202321968927 U CN 202321968927U CN 220918196 U CN220918196 U CN 220918196U
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- container
- suction filtration
- decompression
- crystallization
- reaction
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- 238000001953 recrystallisation Methods 0.000 title claims abstract description 19
- 239000003814 drug Substances 0.000 title claims abstract description 11
- 229940079593 drug Drugs 0.000 title claims abstract description 10
- 238000000967 suction filtration Methods 0.000 claims abstract description 134
- 238000002425 crystallisation Methods 0.000 claims abstract description 76
- 230000008025 crystallization Effects 0.000 claims abstract description 76
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- 230000006837 decompression Effects 0.000 claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000011229 interlayer Substances 0.000 claims abstract description 17
- 238000010992 reflux Methods 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 230000005494 condensation Effects 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229940126586 small molecule drug Drugs 0.000 claims description 5
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000003828 vacuum filtration Methods 0.000 claims 5
- 239000000376 reactant Substances 0.000 abstract description 8
- 230000010354 integration Effects 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 5
- 239000010410 layer Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model discloses an integrated micromolecular drug recrystallization device which comprises a box body, wherein a reaction module, a suction filtration crystallization module and a decompression suction filtration module are arranged in the box body; the reaction module comprises a reaction container, a liquid outlet is arranged below the reaction container, a suction filtration crystallization container is movably arranged below the liquid outlet, filter paper is arranged at the upper part of the suction filtration crystallization container, a second valve is arranged at the outlet of the bottom, an interlayer is arranged at the periphery of the suction filtration crystallization container, and the interlayer is communicated with a low-temperature constant-temperature tank; a decompression suction filtration container is movably arranged below the suction filtration crystallization container, and a filter screen is arranged in the middle of the decompression suction filtration container; the suction filtration crystallization container and the decompression suction filtration container are respectively connected with a lifting module, and the lifting module drives the suction filtration crystallization container and the decompression suction filtration container to move up and down, and the suction filtration crystallization container and the decompression suction filtration container are respectively communicated with a vacuum pump. The utility model has high integration level, effectively shortens the experiment time and is convenient to use; the transfer of reactants is avoided, the loss caused by the transfer of reactants can be avoided, and the yield of the product is greatly improved.
Description
Technical Field
The utility model relates to the technical field of chemical experimental equipment, in particular to an integrated micromolecular drug recrystallization device.
Background
In the fields of chemistry and medicine, for example, filtration is required in the preparation, purification and recrystallization processes of small molecule drugs, and in consideration of the defect that the compound to be purified is crystallized immediately below a certain temperature, a laboratory generally adopts a hot suction filtration method to purify a target substance. The hot suction filtration operation is mostly finished by adopting a combination of a cloth funnel, a suction filter bottle and a vacuum pump at present, and the combination is influenced by the field environment temperature in the hot suction filtration process, a large amount of crystallization residues exist at the upper end of the cloth funnel and in the funnel, the recrystallization yield is seriously influenced, and the operations such as heating and decoloring of recrystallization can not be performed.
The Chinese patent CN214485865U (publication date: 2021.10.26) discloses a constant-temperature and pressure-reducing filter device for a laboratory, which comprises a heat-preserving funnel and a heat-preserving suction filter flask, wherein the heat-preserving funnel comprises a containing bucket, a filter plate, a built-in baffle plate, a containing bucket water inlet and outlet, a connecting pipe and a lower straight pipe, and the connecting pipe is in a structure of a gradually expanding and shrinking pipe and is provided with an extraction opening; the accommodating bucket is of a double-layer structure; hot water can be introduced between the two layers of structures; the funnel filter plate is a structure for filtering and supporting filter paper and blocking solids; the baffle plate arranged in the bucket is arranged at the intersection of the vertical bisector of the connecting line of the bucket water inlet and the bucket water outlet and the bucket double-layer structure, and extends to a position which is about 1.5cm away from the bottom of the inner edge of the lower straight pipe; the latter mainly comprises a suction filtration bottle water inlet, a suction filtration bottle water outlet and an interlayer support block. During hot filtration, experimenters can introduce hot water into the heat preservation funnel, suction filtration is performed according to general suction filtration operation when the temperature is constant, meanwhile, cooling water is introduced into the heat preservation suction filtration bottle, and the flowing filtrate can be crystallized successively. The whole structure materials in the patent are glass, ceramic or quartz, so that the instrument is easy to damage and possible to cause safety accidents; the disassembly is needed before and after the use, and the operation is complicated in the experimental process; the method can only be used for carrying out the operations of decompression suction filtration and recrystallization independently after the reaction is finished, can not be used for filtering and separating after the recrystallization, can not be used for carrying out other experimental steps, and has low integration level.
Disclosure of utility model
In order to solve the defects in the prior art, the utility model provides an integrated micromolecular drug recrystallization device which integrates the reaction, suction filtration, recrystallization and separation operation into a whole, has high integration level, is more convenient to operate, shortens the operation time and improves the working efficiency.
In order to achieve the technical purpose, the utility model adopts the following technical scheme:
An integrated micromolecular drug recrystallization device comprises a box body, wherein a reaction module, a suction filtration crystallization module and a decompression suction filtration module are arranged in the box body; the reaction module comprises a reaction container, a liquid outlet is arranged below the reaction container, a first valve is arranged on the liquid outlet, a suction filtration crystallization module is movably arranged below the liquid outlet of the reaction container, the suction filtration crystallization module comprises a suction filtration crystallization container, filter paper is arranged at the upper part of the suction filtration crystallization container, a second valve is arranged at the outlet at the bottom of the suction filtration crystallization container, an interlayer is arranged at the periphery of the suction filtration crystallization container, and the interlayer is communicated with a low-temperature constant-temperature tank; a decompression suction filtration module is movably arranged below the suction filtration crystallization container, the decompression suction filtration module comprises a decompression suction filtration container, and a filter screen is arranged in the middle of the decompression suction filtration container; the suction filtration crystallization container and the decompression suction filtration container are respectively connected with the lifting module, the lifting module drives the suction filtration crystallization container and the decompression suction filtration container to move up and down, the reaction container is in sealed connection with the suction filtration crystallization container and the decompression suction filtration container, and the suction filtration crystallization container and the decompression suction filtration container are respectively communicated with the vacuum pump.
Further, a temperature control heating interlayer is arranged on the periphery of a reaction container of the reaction module, a condensation reflux device is arranged above the reaction container, and the condensation reflux device is communicated with a low-temperature constant-temperature tank.
Further, a magnetic stirrer is arranged below the reaction vessel.
Further, a rubber gasket is arranged between the liquid outlet of the reaction container and the top inlet of the suction filtration crystallization container, and a rubber gasket is arranged between the bottom outlet of the suction filtration crystallization container and the liquid inlet end of the decompression suction filtration container.
Further, the longitudinal section of the rubber gasket is H-shaped.
Further, the end part of the H-shaped bayonet of the rubber gasket is provided with a 45-degree guiding inclined plane.
Further, the lifting module is a lifting motor.
Further, the lifting module comprises racks and gears, the gears are respectively connected to the two sides of the suction filtration crystallization container and the pressure reduction suction filtration container through connecting rods in a rotating way, the racks are vertically arranged and fixedly arranged on the two sides of the suction filtration crystallization container and the pressure reduction suction filtration container, the gears are connected with the racks in a meshed way, the gears are axially connected with screw knobs penetrating through the box body, and the gears can be driven to ascend or descend along the racks by manually rotating the screw knobs; the gear bolt penetrates through the inside from the outside of the box body and penetrates through the rack, the positions of the two pairs of gear bolts correspond to the highest points of the two groups of gears which are allowed to ascend respectively, and when the gears ascend to the highest positions, the gear bolt is pushed to abut against the lower ends of the gears to prevent the gears from moving downwards.
Compared with the prior art, the utility model has the beneficial effects that:
The reaction module, the suction filtration crystallization module and the decompression suction filtration module are highly integrated, so that the operation time of an experiment is effectively shortened, and the use is more convenient; meanwhile, no reactant is transferred, so that the loss caused by reactant transfer can be avoided, and the yield of the product is greatly improved.
The utility model has the advantages of safety, reliability, more convenient operation and high integration level, and has wide application value in the technical fields of micromolecular drug synthesis and hot suction filtration of drug recrystallization.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic overall structure of an embodiment of the present utility model.
Fig. 2 is a schematic longitudinal section of a rubber gasket.
FIG. 3 is a schematic diagram of one embodiment of a lifting module.
Reference numerals: the device comprises a 1-condensation reflux device, a 2-reaction container, a 3-temperature-control heating interlayer, a 4-magnetic stirrer, a 5-first valve, a 6-rubber gasket, a 61-guiding inclined plane, a 7-interlayer, an 8-vacuum pump, a 9-second valve, a 10-low-temperature constant temperature tank, a 11-lifting module, a 12-filter screen, a 13-water outlet, a 14-box body, a 15-gear, a 16-rack, a 17-gear buckle, a 18-suction filtration crystallization container, a 19-decompression suction filtration container and a 20-connecting rod.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments of the present application. The components of the embodiments of the present application generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the application, as presented in the figures, is not intended to limit the scope of the application, as claimed, but is merely representative of selected embodiments of the application. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
An integrated micromolecular drug recrystallization device is shown in fig. 1, and comprises a box body 14, wherein a reaction module, a suction filtration crystallization module and a decompression suction filtration module are arranged in the box body 14; the reaction module comprises a reaction container 2, a liquid outlet is arranged below the reaction container 2, a first valve 5 is arranged on the liquid outlet, a suction filtration crystallization module is movably arranged below the liquid outlet of the reaction container 2, the suction filtration crystallization module comprises a suction filtration crystallization container 18, filter paper is arranged at the upper part of the suction filtration crystallization container 18, a second valve 9 is arranged at the outlet at the bottom of the suction filtration crystallization container 18, an interlayer 7 is arranged at the periphery of the suction filtration crystallization container 18, and the interlayer 7 is communicated with a low-temperature constant-temperature tank 10; a decompression and suction filtration module is movably arranged below the suction filtration crystallization container 18, the decompression and suction filtration module comprises a decompression and suction filtration container 19, and a filter screen 12 is arranged in the middle of the decompression and suction filtration container 19; the suction filtration crystallization container 18 and the decompression suction filtration container 19 are respectively connected with the lifting module 11, the lifting module 11 drives the suction filtration crystallization container 18 and the decompression suction filtration container 19 to move up and down, the sealed connection between the reaction container 2 and the suction filtration crystallization container 18 and the sealed connection between the suction filtration crystallization container 18 and the decompression suction filtration container 19 are realized, and the suction filtration crystallization container 18 and the decompression suction filtration container 19 are respectively communicated with the vacuum pump 8.
Further, a temperature control heating interlayer 3 is arranged on the periphery of a reaction container 2 of the reaction module, a condensation reflux device 1 is arranged above the reaction container, the condensation reflux device 1 is communicated with a low-temperature constant-temperature tank 10, and a magnetic stirrer 4 is arranged below the reaction container 2; and the reactants are introduced into the reaction container 2, the temperature-control heating interlayer 3 and the magnetic stirrer 4 respectively perform temperature-control heating and stirring on the solution in the reaction container 2, and the condensation reflux device 1 is communicated with the low-temperature constant-temperature tank 10 to perform condensation reflux on the reactants.
Preferably, a rubber gasket 6 is arranged between the liquid outlet of the reaction vessel 2 and the top inlet of the suction filtration crystallization vessel 18, and a rubber gasket 6 is arranged between the bottom outlet of the suction filtration crystallization vessel 18 and the liquid inlet end of the pressure reduction suction filtration vessel 19, so that the reaction vessel 2 is in sealed connection with the suction filtration crystallization vessel 18 and the pressure reduction suction filtration vessel 19, and a negative pressure environment is formed in the suction filtration crystallization vessel 18 or the pressure reduction suction filtration vessel 19 when the vacuum pump 8 pumps. More preferably, the longitudinal section of the rubber gasket 6 is in an "H" shape, as shown in fig. 2, the bayonet at two ends of the "H" of the rubber gasket 6 is respectively clamped at the liquid outlet of the reaction vessel 2 and the top inlet of the suction filtration crystallization vessel 18, the bottom outlet of the suction filtration crystallization vessel 18 and the bottleneck at the liquid inlet end of the pressure reduction suction filtration vessel 19, so that the sealing effect can be further improved. Preferably, the end of the H-shaped bayonet of the rubber gasket 6 is provided with a 45-degree guiding inclined plane 61, so that the bottle mouth of the suction filtration crystallization container 18 and the bottle mouth of the decompression suction filtration container 19 can be smoothly clamped into the rubber gasket in the rising process.
In one embodiment, the lifting module is a lifting motor.
In another preferred embodiment, as shown in fig. 1 and 3, the lifting module includes a rack 16 and a gear 15, two sides of the suction filtration crystallization container 18 and the pressure reduction suction filtration container 19 are respectively connected with the gear 15 through a connecting rod 20 in a rotating manner, the rack 16 is vertically arranged and fixedly arranged at two sides of the suction filtration crystallization container 18 and the pressure reduction suction filtration container 19, the gear 15 is in meshed connection with the rack 16, the gear 15 is axially connected with a screw knob penetrating through the box 14, and the gear 15 can be driven to ascend or descend along the rack 16 by manually rotating the screw knob, so that the height positions of the suction filtration crystallization container 18 and the pressure reduction suction filtration container 19 are adjusted; the device further comprises two pairs of gear bolts 17, the gear bolts 17 penetrate from the outside of the box body 14 to the inside and penetrate through the racks 16, the positions of the two pairs of gear bolts 17 respectively correspond to the highest points of the two groups of gears 15 allowed to ascend, namely, the heights reached by the tight fitting of the suction filtration crystallization container 18 and the condensation reflux device 1 and the tight fitting of the decompression suction filtration device 19 and the suction filtration crystallization device 18, the gear bolts 17 are taken as the preset highest points, and when the gears 15 reach the highest points, the gear bolts 17 are manually pushed in from the outside of the box body 14 so as to support the gears to prevent the gears 15 from shifting. The suction filtration crystallization container 18 and the decompression suction filtration container 19 form a negative pressure environment, so that air leakage caused by loose pressing of rubber gaskets is avoided; the gear bolt 17 penetrates from the outer wall of the box body 14 to the inside, when the container is used, the gear bolt 17 is pulled out from the outside of the box body 14, the gear 15 is lowered, and the suction filtration crystallization container 18 or the decompression suction filtration container 19 can be driven to be lowered.
The whole operation flow of the utility model is as follows: introducing reactants into the reaction container 2, respectively heating and stirring the solution in the reaction container 2 by the temperature control heating interlayer 3 and the magnetic stirrer 4, and condensing and refluxing the reactants by the condensing and refluxing device 1 through the low-temperature constant-temperature tank 10; after the reaction is finished, the height position of a suction filtration crystallization container 18 is adjusted through a lifting module 11, the suction filtration crystallization container is in sealing connection with a reaction container 2, a first valve 5 is opened, a vacuum pump 8 is opened to carry out suction filtration on the solution while the solution is hot, and a condensing agent is introduced into an interlayer 7 of the suction filtration crystallization container 18 through the low-temperature constant-temperature tank 10, so that the filtrate after the filtration while the solution is hot is crystallized; after the filtrate is crystallized, the height positions of a suction filtration crystallization container 18 and a decompression suction filtration container 19 are adjusted through a lifting module 11 to be in sealed connection, a second valve 9 is opened, the crystallized filtrate is introduced above a filter screen 12 of the decompression suction filtration container 19, a vacuum pump 8 is opened, the vacuum pump 8 is used for decompressing and filtering the solution which is subjected to crystallization in the decompression suction filtration container 19, the separation of the filtrate and crystals is completed, a product obtained on the filter screen 12 is a target product, a water outlet 13 is arranged below the decompression suction filtration container 19, and the water outlet 13 at the bottom of the decompression suction filtration container 19 is opened to discharge waste liquid.
Of course, the present utility model is capable of other various embodiments and its several details are capable of modification and variation in light of the present utility model by one skilled in the art without departing from the spirit and scope of the utility model as defined in the appended claims.
Claims (5)
1. An integrated micromolecular drug recrystallization device is characterized in that: the device comprises a box body (14), wherein a reaction module, a suction filtration crystallization module and a decompression suction filtration module are arranged in the box body (14); the reaction module comprises a reaction container (2), a liquid outlet is formed in the lower portion of the reaction container (2), a first valve (5) is arranged on the liquid outlet, a suction filtration crystallization module is movably arranged below the liquid outlet of the reaction container (2), the suction filtration crystallization module comprises a suction filtration crystallization container (18), filter paper is arranged on the upper portion of the suction filtration crystallization container (18), a second valve (9) is arranged at the outlet of the bottom of the suction filtration crystallization container (18), an interlayer (7) is arranged on the periphery of the suction filtration crystallization container (18), and the interlayer (7) is communicated with a low-temperature constant-temperature tank (10); a decompression and suction filtration module is movably arranged below the suction filtration crystallization container (18), the decompression and suction filtration module comprises a decompression and suction filtration container (19), and a filter screen (12) is arranged in the middle of the decompression and suction filtration container (19); the vacuum filtration crystallization container (18) and the decompression filtration container (19) are respectively connected with the lifting module (11), the lifting module (11) drives the vacuum filtration crystallization container (18) and the decompression filtration container (19) to move up and down, so that the reaction container (2) is in sealed connection with the vacuum filtration crystallization container (18), the vacuum filtration crystallization container (18) is in sealed connection with the decompression filtration container (19), and the vacuum filtration crystallization container (18) and the decompression filtration container (19) are respectively communicated with the vacuum pump (8);
A rubber gasket (6) is arranged between a liquid outlet of the reaction container (2) and a top inlet of the suction filtration crystallization container (18), and a rubber gasket (6) is arranged between a bottom outlet of the suction filtration crystallization container (18) and a liquid inlet end of the decompression suction filtration container (19);
The lifting module comprises a rack (16) and a gear (15), wherein the two sides of the suction filtration crystallization container (18) and the decompression suction filtration container (19) are respectively connected with the gear (15) through a connecting rod (20) in a rotating way, the rack (16) is vertically arranged and fixedly arranged on the two sides of the suction filtration crystallization container (18) and the decompression suction filtration container (19), the gear (15) is meshed with the rack (16), the gear (15) is axially connected with a screw knob penetrating through the box body (14), and the gear (15) can be driven to ascend or descend along the rack (16) through manual rotation of the screw knob; the gear box further comprises gear pins (17), the gear pins (17) penetrate through the box body (14) from the outside to the inside and penetrate through racks (16), the positions of the two pairs of the gear pins (17) correspond to the highest points of the two groups of gears (15) which are allowed to ascend respectively, and when the gears (15) ascend to the highest positions, the gear pins (17) are pushed to abut against the lower ends of the gears (15) to prevent the gears (15) from moving downwards.
2. The integrated small molecule drug recrystallization apparatus of claim 1, wherein: the reaction device is characterized in that a temperature control heating interlayer (3) is arranged on the periphery of a reaction container (2) of the reaction module, a condensation reflux device (1) is arranged above the reaction container (2), and the condensation reflux device (1) is communicated with a low-temperature constant-temperature tank (10).
3. The integrated small molecule drug recrystallization apparatus of claim 2, wherein: a magnetic stirrer (4) is arranged below the reaction vessel (2).
4. The integrated small molecule drug recrystallization apparatus of claim 1, wherein: the longitudinal section of the rubber gasket (6) is H-shaped.
5. The integrated small molecule drug recrystallization apparatus of claim 4, wherein: the end part of the H-shaped bayonet of the rubber gasket (6) is provided with a 45-degree guiding inclined plane (61).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321968927.5U CN220918196U (en) | 2023-07-25 | 2023-07-25 | Integrated micromolecular drug recrystallization device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321968927.5U CN220918196U (en) | 2023-07-25 | 2023-07-25 | Integrated micromolecular drug recrystallization device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220918196U true CN220918196U (en) | 2024-05-10 |
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ID=90940070
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202321968927.5U Active CN220918196U (en) | 2023-07-25 | 2023-07-25 | Integrated micromolecular drug recrystallization device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220918196U (en) |
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2023
- 2023-07-25 CN CN202321968927.5U patent/CN220918196U/en active Active
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