CN112808188A - Controllable phase separation device of material transfer speed - Google Patents
Controllable phase separation device of material transfer speed Download PDFInfo
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- CN112808188A CN112808188A CN202110175174.1A CN202110175174A CN112808188A CN 112808188 A CN112808188 A CN 112808188A CN 202110175174 A CN202110175174 A CN 202110175174A CN 112808188 A CN112808188 A CN 112808188A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
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Abstract
本发明公开了一种物料转移速度可控的相分离装置，包括油相釜、二甲基硅油釜、固化釜、高剪切乳化机以及分筛机，油相釜加料口通过第二蠕动泵与乳化机第二进料口连通，乳化机出料口与油相釜第一进料口连接；二甲基硅油釜出料口通过隔膜计量泵与油相釜第二进料口连接；油相釜出料口通过第一隔膜泵与固化釜第一进料口连接；固化釜出料口通过第三隔膜泵与分筛机进料口连接。本发明实现了物料转移的自动化，并能对物料转移速度进行严格控制，减少了工艺误差，同时扩大了设备的工艺产能。
The invention discloses a phase separation device with controllable material transfer speed, comprising an oil phase kettle, a dimethyl silicone oil kettle, a curing kettle, a high shear emulsifier and a sieving machine. The feeding port of the oil phase kettle passes through a second peristaltic pump It is connected with the second feed port of the emulsifier, and the discharge port of the emulsifier is connected with the first feed port of the oil phase kettle; the discharge port of the dimethyl silicone oil kettle is connected with the second feed port of the oil phase kettle through a diaphragm metering pump; The outlet of the phase kettle is connected with the first inlet of the curing kettle through the first diaphragm pump; the outlet of the curing kettle is connected with the inlet of the screening machine through the third diaphragm pump. The invention realizes the automation of material transfer, can strictly control the material transfer speed, reduces the process error, and at the same time expands the process capacity of the equipment.
Description
Technical Field
The invention relates to the technical field of microsphere preparation equipment by a phase separation method, in particular to a phase separation device with controllable material transfer speed.
Background
In the microsphere preparation process adopting the phase separation method, the water phase or the solid phase and the oil phase need to be emulsified firstly, and then the raw materials and the emulsified liquid are added into a curing kettle for reaction. In the existing microsphere preparation process adopting a phase separation method, the transfer of materials needs to be carried out manually, so that the labor cost is increased and the capacity is limited; on the other hand, the feeding speed is difficult to control, and in some processes requiring strict control of the feeding time and speed, errors are generated due to human factors, so that the accuracy of the process is influenced. In addition, the existing equipment cannot be simultaneously applied to the liquid-liquid phase separation method and the liquid-solid phase separation method, so that the equipment cost of enterprises is increased.
Disclosure of Invention
The invention aims to provide a phase separation device with a controllable material transfer speed, which aims to effectively expand the process capacity, realize the automation of material transfer in the process and reduce errors.
In order to achieve the above purpose, the invention provides the following technical scheme: a phase separation apparatus with controlled material transfer rates, comprising:
the high-shear emulsifying machine is provided with a first feeding hole of the emulsifying machine, a second feeding hole of the emulsifying machine and a discharging hole of the emulsifying machine, and the first feeding hole of the emulsifying machine is used for adding a water phase or a solid phase into the high-shear emulsifying machine;
the oil phase kettle is provided with an oil phase kettle first material transferring port, an oil phase kettle second material transferring port, an oil phase kettle pumping port and an oil phase kettle discharging port;
the dimethyl silicone oil kettle is provided with a discharge hole of the dimethyl silicone oil kettle;
the curing kettle is provided with a first curing kettle material transferring port, a curing kettle material feeding port and a curing kettle material discharging port; and
the screening machine is provided with a screening machine feeding hole;
the material pumping port of the oil phase kettle is communicated with a second feeding port of the emulsifying machine through a second peristaltic pump, and the discharging port of the emulsifying machine is connected with the first material rotating port of the oil phase kettle; the discharge port of the dimethyl silicone oil kettle is connected with the second material transferring port of the oil phase kettle through a diaphragm metering pump; the discharge port of the oil phase kettle is connected with the first rotating port of the curing kettle through a first diaphragm pump; and the discharge hole of the curing kettle is connected with the feed inlet of the screening machine through a third diaphragm pump.
Further, the first feed inlet of emulsion machine is used for adding the aqueous phase to high shear emulsion machine, the phase separation device still includes the aqueous phase cauldron, the aqueous phase cauldron is equipped with aqueous phase cauldron pump outlet, the aqueous phase cauldron is pumped the material mouth and is connected with the first feed inlet of emulsion machine through first peristaltic pump.
Further, still include reserve cauldron, reserve cauldron is equipped with reserve cauldron discharge gate, reserve cauldron discharge gate is passed through the second diaphragm pump and is connected with solidification cauldron second commentaries on classics material mouth.
Further, the curing kettle, the dimethyl silicone oil kettle, the standby kettle and the oil phase kettle are all of a double-layer structure, the inner layer is a reaction cavity, and the outer layer is a cooling liquid circulation cavity; and a cooling liquid inlet and a cooling liquid outlet are respectively arranged on two opposite sides of the cooling liquid circulating cavity.
Further, still include the coolant liquid circulating pump, the coolant liquid circulating pump is equipped with liquid outlet and inlet, the liquid outlet is connected with the coolant liquid import in coolant liquid circulation chamber, the inlet is connected with the coolant liquid export in coolant liquid circulation chamber.
Further, the temperature control point of the cooling liquid circulating pump is 3 ℃.
Further, stirring paddles are respectively arranged in reaction cavities of the curing kettle, the n-heptane kettle and the oil phase kettle.
Further, the flow rates of the first diaphragm pump, the second diaphragm pump and the third diaphragm pump are all 5-20L/min.
Compared with the prior art, the invention has the advantages that: according to the invention, through the reaction kettles with different specifications and the peristaltic pumps and the diaphragm pumps which are used for mutually transferring materials, the automation of material transfer is realized, the material transfer speed can be strictly controlled, the process error is reduced, and the process capacity of the equipment is expanded; in addition, the invention can be applied to two processes of a liquid-liquid phase separation method and a liquid-solid phase separation method, and only the reaction kettle needs to be replaced during preparation.
Drawings
Fig. 1 is a schematic view of the overall structure of the present invention.
FIG. 2 is a schematic view of the arrangement of the tank cover of the aqueous phase tank of the present invention.
FIG. 3 is a schematic view of the layout of the cover of the oil phase tank of the present invention.
FIG. 4 is a schematic view of the layout of the cover of the dimethylsilicone kettle of the present invention.
FIG. 5 is a schematic view of the layout of the cover of the curing oven of the present invention.
FIG. 6 is a schematic view of the arrangement of the cover of the n-heptane vessel in the present invention.
In the figure: 1. a water phase kettle 101 and a water phase kettle material pumping port; 2. an oil phase kettle, 201, a first material transferring port of the oil phase kettle, 202, a second material transferring port of the oil phase kettle, 203 and a material pumping port of the oil phase kettle; 3. a dimethyl silicone oil kettle 301 and a dimethyl silicone oil kettle feed inlet; 4. the curing kettle comprises a curing kettle body 401, a curing kettle body charging port 402, a curing kettle body first material transferring port 403 and a curing kettle body second material transferring port; 5. an n-heptane kettle, 501, a feed inlet of the n-heptane kettle; 6. a first peristaltic pump; 7. a second peristaltic pump; 8. a diaphragm metering pump; 9. a first diaphragm pump; 10. a second diaphragm pump; 11. a third diaphragm pump; 12. a coolant circulation pump; 13. a high shear emulsifier; 14. a screening machine.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further specifically described below by way of embodiments in combination with the accompanying drawings.
Example 1
In this embodiment, taking preparation of microspheres by a polypeptide liquid-liquid phase separation method as an example, as shown in fig. 1-6, a n-heptane kettle is used as a spare kettle, and the device includes a 1L water phase kettle 1, a 10L oil phase kettle 2, a 5L dimethyl silicone oil kettle 3, a 50L n-heptane kettle 5, a 100L curing kettle 4, a high shear emulsifying machine 13 and a sieving machine 14; wherein:
the top of the water phase kettle 1 is provided with a water phase kettle pumping port 101 for pumping out the raw materials in the water phase kettle.
The top of the oil phase kettle 2 is provided with an oil phase kettle first material transferring port 201, an oil phase kettle second material transferring port 202 and an oil phase kettle material pumping port 203; the bottom is provided with an oil phase kettle discharge hole.
The top of the dimethyl silicone oil kettle 3 is provided with a dimethyl silicone oil kettle feeding hole 301 for feeding materials into the dimethyl silicone oil kettle; the bottom is provided with a dimethyl silicone oil kettle discharge hole.
The top of the n-heptane kettle 5 is provided with an n-heptane kettle feeding hole 501 for feeding materials into the n-heptane kettle; the bottom is provided with a discharge hole of the normal heptane kettle.
The top of the curing kettle 4 is provided with a curing kettle feed port 401, a curing kettle first material transferring port 402 and a curing kettle second material transferring port 403; the bottom is provided with a discharge hole of the curing kettle.
The high shear emulsifying machine 13 is provided with a first feeding hole of the emulsifying machine, a second feeding hole of the emulsifying machine and a discharging hole of the emulsifying machine.
The screening machine 14 is provided with a screening machine feed inlet.
In this embodiment, the high-shear emulsifying machine 13 and the screening machine 14 may be any machine that can meet the use requirements in the market.
The water phase kettle pumping port 101 is connected with a first feeding port of the emulsifying machine through a first peristaltic pump 6 and is used for transferring the raw materials in the water phase kettle 1 into a high-shear emulsifying machine 13 through the first peristaltic pump 6; specifically, the first peristaltic pump 6 is connected with the water phase kettle material pumping port 101 and the first feeding port of the emulsifying machine respectively by a silicone tube, and the flow rate is controlled to be about 3.12 mL/min.
The oil phase kettle pumping port 203 is communicated with a second feeding port of the emulsifying machine through a second peristaltic pump 7 and is used for transferring the raw materials in the oil phase kettle 2 into a high-shear emulsifying machine 13 through the second peristaltic pump 7; specifically, the second peristaltic pump 7 is connected to the oil phase kettle pumping port 203 and the second feeding port of the emulsifying machine through a tetrafluoro pipe.
The discharge port of the emulsifying machine is connected with the first material transferring port 201 of the oil phase kettle, and the emulsified material can flow into the oil phase kettle 2.
A discharge port of the simethicone kettle is connected with a second material transferring port 202 of the oil phase kettle through a diaphragm metering pump 8 and is used for transferring the simethicone into the oil phase kettle 2 through the diaphragm metering pump 8; specifically, the diaphragm metering pump 8 is connected with the discharge port of the simethicone kettle and the second material transferring port 202 of the oil phase kettle respectively by a silicone tube, and the flow rate is controlled to be about 3L/min.
The discharge port of the oil phase kettle is connected with the first material transferring port 402 of the curing kettle through a first diaphragm pump 9, and is used for transferring the material to the curing kettle 4 through the first diaphragm pump 9, and the flow rate of the first diaphragm pump 9 is 10L/min.
The discharge port of the n-heptane kettle is connected with a second material transferring port 403 of the curing kettle through a second diaphragm pump 10, and is used for transferring n-heptane into the curing kettle 4 through the second diaphragm pump 10, wherein the flow rate of the second diaphragm pump 10 is 10L/min.
The discharge hole of the curing kettle is connected with the feed inlet of the screening machine through a third diaphragm pump 11, and is used for transferring liquid or small-particle-size materials in the curing kettle 4 to the screening machine 14, and the flow rate of the third diaphragm pump 11 is 10L/min.
In the structure, the solidification kettle 4, the dimethyl silicon oil kettle 3, the n-heptane kettle 5 and the oil phase kettle 2 are of double-layer structures, the inner layer is a reaction cavity, the outer layer is a cooling liquid circulation cavity, the two opposite sides of the cooling liquid circulation cavity are respectively provided with a cooling liquid inlet and a cooling liquid outlet, and the cooling liquid inlet and the cooling liquid outlet are respectively located at the bottom and the top of the cooling liquid circulation cavity. In the embodiment, two cooling liquid circulating pumps 12 are provided, one of which provides a cold source for the curing kettle 4 and the dimethyl silicone oil kettle 3, and the temperature control point is 3 ℃; the other provides cold sources for the n-heptane kettle 5 and the oil phase kettle 2, and the temperature control point is 3 ℃. Specifically, the coolant circulation pump 12 is provided with a liquid outlet and a liquid inlet, the liquid outlet is connected to a coolant inlet of the corresponding coolant circulation chamber, and the liquid inlet is connected to a coolant outlet of the corresponding coolant circulation chamber.
In this embodiment, the reaction cavities of the curing kettle 4, the n-heptane kettle 5 and the oil phase kettle 2 are respectively provided with stirring paddles driven by a motor.
In this embodiment, first, the corresponding raw materials are added into each reaction kettle, for example, PLGA (polylactic acid-glycolic acid copolymer) or PLA (polylactic acid) dissolved by dichloromethane is added into the oil phase kettle 2, and raw materials such as n-heptane are added into the curing kettle 4. Then the first peristaltic pump 6 and the second peristaltic pump 7 start to work, the raw materials in the water phase kettle 1 and the raw materials in the oil phase kettle 2 are transferred into a high-shear emulsifying machine 13 for emulsification, the emulsified materials flow into the oil phase kettle 2 again, and full emulsification is completed through circulation; then a diaphragm metering pump 8 works, the dimethyl silicone oil in the dimethyl silicone oil kettle 3 is transferred into the oil phase kettle 2, and the mixture is stirred uniformly; then the first diaphragm pump 9 works, the materials in the oil phase kettle 2 are transferred to the curing kettle 4, and are mixed with the raw materials in the curing kettle 4 to react, after the reaction lasts for a period of time, in order to ensure that the reaction is complete, the normal heptane in the normal heptane kettle 5 is transferred to the curing kettle 4 through the second diaphragm pump 10 to supplement the normal heptane; at the same time, the third diaphragm pump 11 discharges the liquid or small-particle-size material in the curing kettle 4 to the sieving machine 14.
If the liquid-solid phase separation method is adopted for preparing the microspheres, only the water phase kettle 1 is removed, and the solid phase raw materials are directly added into the emulsifying machine through the first feed inlet of the emulsifying machine.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202110175174.1A CN112808188A (en) | 2021-02-07 | 2021-02-07 | Controllable phase separation device of material transfer speed |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110175174.1A CN112808188A (en) | 2021-02-07 | 2021-02-07 | Controllable phase separation device of material transfer speed |
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|---|---|---|---|---|
| US5827909A (en) * | 1995-01-10 | 1998-10-27 | The Procter & Gamble Company | Recirculating a portion of high internal phase emulsions prepared in a continuous process |
| US20050084536A1 (en) * | 2001-10-26 | 2005-04-21 | Van Buitenen Adrianus F.G. | Method for the preparation of purified microparticles |
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| CN210906036U (en) * | 2019-08-27 | 2020-07-03 | 安疗生命科学（武汉）有限公司 | Electrostatic spray collection device |
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-
2021
- 2021-02-07 CN CN202110175174.1A patent/CN112808188A/en active Pending
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