Vacuum freeze-drying apparatus and method of operation thereof

Abstract

The application provides a vacuum freeze-drying device and a working method thereof. The vacuum freeze-drying device comprises a first drying chamber, a flash chamber in communication with the first drying chamber, a sprayer arranged in the flash chamber, a second drying chamber in communication with the flash chamber, a freezing system in communication with the first drying chamber, the flash chamber and the second drying chamber, a vacuum exhaust system in communication with the first drying chamber, the flash chamber, the freezing system and the second drying chamber and performing vacuum exhaust, and a conveying device arranged in the first drying chamber. The freezing chamber is vacuumized, the flash chamber in communication with the freezing chamber is also in a low-pressure state, the material original solution sprayed from the sprayer in a high-pressure state enters the low-pressure flash chamber, the first drying is completed in the flash chamber, the second drying is completed in the first drying chamber, and the material original solution in the frozen particle state after the second drying is conveyed to the second drying chamber under the action of the conveying device.

Description

Technical Field

[0001] This invention relates to the technical field of vacuum freeze drying, and more specifically, to a vacuum freeze drying apparatus and its operating method. Background Technology

[0002] When producing pharmaceutical freeze-dried agents, the pharmaceutical product needs to be liquefied and then frozen. Sublimation heat is then supplied under vacuum to cause the water in the original liquid material to sublimate, thus achieving drying. This process must be carried out in a vacuum freeze-drying device.

[0003] Chinese invention patent application CN117980680A discloses a freeze-drying apparatus, including a freezing unit for producing a frozen substance by spraying a raw material solution and a drying unit for drying the frozen substance while conveying it; the drying unit includes a tubular section maintained under vacuum, which extends linearly in the horizontal direction in a tube shape.

[0004] The aforementioned freeze-drying equipment has some problems: for example, the freeze-drying time is relatively long, and if more sublimation heat is provided to shorten the freeze-drying time, it may cause the raw material liquid that forms frozen particles to melt and stick together. At the same time, there is also the problem of insufficient drying. In subsequent processing, the raw material liquid of the frozen particles is not uniform, which affects subsequent processing. Summary of the Invention

[0005] In view of this, and in order to solve the above problems, the present invention provides a vacuum freeze-drying device and its working method, the specific technical solution of which is as follows: On the one hand, a vacuum freeze-drying apparatus includes: First drying chamber; A flash chamber is connected to the first drying chamber. A sprayer is installed in the flash chamber and is used to spray the raw material liquid into the flash chamber. The second drying chamber is connected to the flash chamber; A refrigeration system is connected to the first drying chamber, the flash chamber, and the second drying chamber. The refrigeration system is used to capture water vapor and discharge the water vapor. A vacuum exhaust system is connected to the first drying chamber, the flash evaporation chamber, the refrigeration system, and the second drying chamber, respectively. The vacuum exhaust system is used to exhaust the vacuum from the first drying chamber, the flash evaporation chamber, the second drying chamber, and the refrigeration system. A transport device is installed in the first drying chamber, and the output port of the transport device is connected to the second drying chamber.

[0006] The aforementioned vacuum freeze-drying equipment, by evacuating the freezing chamber, also lowers the pressure of the flash chamber connected to it. When the high-pressure raw material liquid sprayed from the atomizer enters the low-pressure flash chamber, the water in the raw material liquid undergoes flash evaporation, turning into water vapor. Simultaneously, due to the continuous evacuation of the freezing chamber by the vacuum exhaust system, the water vapor appearing in the flash chamber is attracted into the freezing chamber. The low surface temperature of the first freezer causes the water vapor to condense on its surface, thus capturing the water vapor. One drying cycle is completed in the flash chamber. At the same time, the temperature of the freezing chamber is also transferred to the flash chamber, freezing the raw material liquid into frozen particles that fall into the first drying chamber. At this point, the temperature controller adjusts the temperature of the transport device to provide sublimation heat, ensuring that the raw material liquid frozen into frozen granules does not melt while allowing the water in it to sublimate into water vapor and be captured by the second freezer. This completes the second drying in the first drying chamber. Simultaneously, under the operation of the transport device, the raw material liquid in the frozen granule state that has completed the second drying is transported to the second drying chamber. Through vibration and stirring, the raw material liquid in the frozen granule state generates sublimation heat through self-collision and friction, expelling the internal water and forming water vapor, which is then captured by the third freezer. Thus, the drying is completed again during the stirring process.

[0007] Furthermore, it also includes a temperature control device, which includes a first temperature controller disposed in the first drying chamber and a second temperature controller disposed in the second drying chamber. The first temperature controller is used to control the temperature of the first drying chamber, and the second temperature controller is used to control the temperature of the second drying chamber.

[0008] Furthermore, the bottom of the flash chamber is connected to the top of the first drying chamber, the bottom of the flash chamber has a bucket-shaped structure, the center line of the sprayer nozzle coincides with the center line of the flash chamber, and the raw material liquid sprayed by the sprayer moves from the sprayer nozzle to the first drying chamber.

[0009] Furthermore, the output port of the transport device is located above the second drying chamber; the second drying chamber is provided with an inlet, a second drying space and a discharge port from top to bottom, the inlet is connected to the output port of the transport device, and a vibration stirring device is provided in the second drying space.

[0010] Furthermore, the refrigeration system includes a freezing chamber, a first freezer, a second freezer, and a third freezer; the first freezer is disposed in the freezing chamber, and the freezing chamber is connected to the flash chamber; the vacuum exhaust system is provided with an exhaust passage connected to the freezing chamber; the second freezer is disposed in the first drying chamber, and the third freezer is disposed in the second drying chamber.

[0011] Furthermore, the connection between the vacuum exhaust system and the second drying chamber, as well as the third freezer, are both located inside and above the second drying chamber.

[0012] Furthermore, it also includes a feeding device disposed at the discharge port, the feeding device being used to uniformly convey the stirred frozen particles.

[0013] On the other hand, a vacuum freeze-drying method and a vacuum freeze-drying apparatus include the following steps: The vacuum exhaust system is activated to exhaust air from the first drying chamber, the flash chamber, the second drying chamber, and the refrigeration system. The vacuum exhaust system is activated to dry the freezing chamber, the first drying chamber, and the second drying chamber in sequence. The temperature of the conveying device in the first drying chamber is controlled between the first temperature and the temperature of the second freezer. The first temperature is the melting temperature at which the raw material liquid is frozen into frozen particles.

[0014] Start the first freezer to dry the freezer compartment; The second freezer is started to dry the first drying chamber; The third freezer is started to dry the second drying chamber.

[0015] Start the oscillating and stirring device to oscillate and dry the raw material liquid that has been frozen into frozen granules in the second drying chamber. Attached Figure Description

[0016] The invention will be further understood from the following description taken in conjunction with the accompanying drawings. The components in the drawings are not necessarily drawn to scale, but rather the emphasis is on illustrating the principles of the embodiments. In different views, the same reference numerals designate corresponding parts.

[0017] Figure 1 This is a simplified structural diagram of the vacuum freeze-drying equipment according to an embodiment of the present invention; Figure 2 yes Figure 1 Enlarged view of the structure at point A in the middle; Figure 3 This is a schematic diagram of the feeding device according to an embodiment of the present invention; Figure 4 This is a structural cross-sectional view of the feeding device according to an embodiment of the present invention.

[0018] Explanation of reference numerals in the attached figures: 10. First drying chamber; 20. Flash chamber; 30. Second drying chamber; 50. Vacuum exhaust system; 60. Conveying device; 70. Temperature control device; 80. Feeding device; 21. Sprayer; 31. Discharge port; 32. First motor; 33. Stirring rod; 34. Support; 35. Support spring; 36. Second motor; 37. Vibrating cam; 41. Freezer compartment; 42. First freezer; 43. Second freezer; 44. Third freezer; 81. Feeding frame; 82. Intermediate hopper; 83. Rotating material tray; 84. Feeding hopper; 85. Feeding motor; 801. Storage cavity; 802. Discharge cavity opening. Detailed Implementation

[0019] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to its embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the scope of protection of the invention.

[0020] It should be noted that when an element is referred to as being "fixed to" another element, it can be directly attached to the other element or there may be an intervening element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or there may be an intervening element. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only possible implementation.

[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0022] In this invention, "first" and "second" do not represent a specific quantity or order, but are merely used to distinguish names.

[0023] On the one hand, such as Figure 1 As shown, a vacuum freeze-drying apparatus according to one embodiment of the present invention includes: First drying chamber 10; Flash chamber 20 is connected to first drying chamber 10. A sprayer 21 is installed in flash chamber 20. Sprayer 21 is used to spray the raw material liquid into flash chamber 20. The second drying chamber 30 is connected to the flash chamber 20; A refrigeration system is connected to the first drying chamber 10, the flash chamber 20, and the second drying chamber 30. The refrigeration system is used to capture water vapor and discharge the water vapor. The vacuum exhaust system 50 is connected to the first drying chamber 10, the flash evaporation chamber 20, the refrigeration system, and the second drying chamber 30, respectively. The vacuum exhaust system 50 is used to exhaust the vacuum from the first drying chamber 10, the flash evaporation chamber 20, the second drying chamber 30, and the refrigeration system. The transport device 60 is installed inside the first drying chamber 10, and the output port of the transport device 60 is connected to the second drying chamber 30.

[0024] The aforementioned vacuum freeze-drying equipment, by evacuating the freezing chamber 41, also brings the flash chamber 20, which is connected to the freezing chamber 41, into a low-pressure state. When the high-pressure raw material liquid sprayed from the sprayer 21 enters the low-pressure flash chamber 20, the water in the raw material liquid will flash evaporate and turn into water vapor. At the same time, due to the continuous evacuation of the freezing chamber 41 by the vacuum exhaust system 50, the water vapor appearing in the flash chamber 20 is attracted into the freezing chamber 41. The low surface temperature of the first freezer 42 causes the water vapor to condense on its surface, thus capturing the water vapor. One drying cycle is completed in the flash chamber 20. Simultaneously, the temperature of the freezing chamber 41 is also transferred to the flash chamber 20, causing the raw material liquid to freeze into frozen particles and fall into the first freezer 42. In the drying chamber 10, the temperature controller adjusts the temperature of the conveyor device 60 to provide sublimation heat, ensuring that the raw material liquid frozen into frozen granules does not melt, while allowing the water in it to sublimate into water vapor and be captured by the second freezer 43, thus completing the second drying in the first drying chamber 10. At the same time, under the operation of the conveyor device 60, the raw material liquid in the frozen granule state that has completed the second drying is transported to the second drying chamber 30. Through vibration and stirring, the raw material liquid in the frozen granule state generates sublimation heat through self-collision and friction, expelling the internal water again to form water vapor, which is then captured by the third freezer 44, thus completing the third drying process simultaneously during the stirring process.

[0025] In one embodiment, a temperature control device 70 is also included. The temperature control device 70 includes a first temperature controller disposed in the first drying chamber 10 and a second temperature controller disposed in the second drying chamber 30. The first temperature controller is used to control the temperature of the first drying chamber 10, and the second temperature controller is used to control the temperature of the second drying chamber 30.

[0026] In one embodiment, the bottom of the flash chamber 20 is connected to the top of the first drying chamber 10. The bottom of the flash chamber 20 has a bucket-shaped structure. The center line of the nozzle of the sprayer 21 coincides with the center line of the flash chamber 20. The raw material liquid sprayed by the sprayer 21 moves from the nozzle of the sprayer 21 to the first drying chamber 10.

[0027] In one embodiment, the output port of the transport device 60 is located above the second drying chamber 30; the second drying chamber 30 is provided with an inlet, a second drying space and a discharge port 31 from top to bottom, the inlet is connected to the output port of the transport device 60, and a vibration stirring device is provided in the second drying space.

[0028] like Figure 1 and Figure 2 As shown, in one embodiment, the oscillating stirring device includes a stirring mechanism and an oscillation mechanism. The stirring mechanism includes a first motor 32 disposed outside the second drying chamber 30 and a stirring rod 33 disposed inside the second drying chamber 30. The first motor 32 drives the stirring rod 33. The oscillation mechanism is disposed at the bottom of the second drying chamber 30 and includes a bracket 34, a support spring 35, a second motor 36, and an oscillating cam 37. The bracket 34 is disposed on the outer periphery of the second drying chamber 30 and connected to the second drying chamber 30 through the support spring 35. The second motor 36 is disposed on the bracket 34 and connected to the hub of the oscillating cam 37. Thus, the second motor 36 drives the oscillating cam 37 to rotate, and the outer diameter surface of the oscillating cam 37 contacts the bracket 34. The distance between the output shaft center of the second motor 36 and the bracket 34 changes periodically, causing the second drying chamber 30 to oscillate up and down on one side of the second motor 36, thereby causing the frozen particles inside the second drying chamber 30 to fall off.

[0029] In one embodiment, the refrigeration system includes a freezer chamber 41, a first freezer 42, a second freezer 43, and a third freezer 44. The first freezer 42 is disposed in the freezer chamber 41, which is connected to the flash chamber 20. The vacuum exhaust system 50 has an exhaust passage connected to the freezer chamber 41. The second freezer 43 is disposed in the first drying chamber 10, and the third freezer 44 is disposed in the second drying chamber 30. Thus, by drying the freezer chamber 41 with the first freezer 42, drying the first drying chamber 10 with the second freezer 43, and drying the second drying chamber 30 with the third freezer 44, the freezing rates of the first drying chamber 10, the freezer chamber 41, and the second drying chamber 30 can be adjusted according to technical requirements.

[0030] In one embodiment, the connection between the vacuum exhaust system 50 and the second drying chamber 30, as well as the third freezer 44, are both located above the interior of the second drying chamber 30.

[0031] In one embodiment, a feeding device 80 is also provided at the discharge port 31, which is used to uniformly convey the stirred frozen particles.

[0032] like Figure 3 and Figure 4As shown, in one embodiment, the feeding device 80 includes a feeding frame 81, an intermediate funnel 82 disposed on the feeding frame 81, a rotating material tray 83, a feeding funnel 84, and a feeding motor 85 that drives the rotating material tray 83 to rotate. The rotating material tray 83 has four storage cavities 801, and the feeding funnel 84 has two feeding openings 802. Thus, the frozen particles are guided into the four storage cavities 801 through the intermediate funnel 82. The feeding motor 85 drives the rotating material tray 83 to rotate, thereby aligning two of the four storage cavities 801 with the two feeding openings 802, and causing a fixed amount of frozen particles to fall from the feeding openings 802 to the designated conveying position.

[0033] On one hand, a vacuum freeze-drying method according to an embodiment of the present invention, applied to the aforementioned vacuum freeze-drying equipment, includes the following steps: S1. Start the vacuum exhaust system 50 to exhaust the vacuum from the first drying chamber 10, flash chamber 20, second drying chamber 30, and refrigeration system; S2. Start the vacuum exhaust system 50 to dry the freezing chamber 41, the first drying chamber 10 and the second drying chamber 30 in sequence; control the temperature of the conveying device 60 in the first drying chamber 10 between the first temperature and the temperature of the second freezer 43, where the first temperature is the melting temperature of the raw material liquid when it is frozen into frozen particles.

[0034] S21. Start the first freezer 42 to dry the freezer compartment 41; S22. Start the second freezer 43 to dry the first drying chamber 10; S23. Start the third freezer 44 to dry the second drying chamber 30.

[0035] S3. Start the vibration and stirring device to vibrate and stir the raw material liquid that has been frozen into frozen granules in the second drying chamber 30 for drying.

[0036] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0037] The above embodiments merely illustrate several implementation methods of the present invention, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A vacuum freeze-drying method, applied to a vacuum freeze-drying equipment, characterized in that, The vacuum freeze-drying equipment includes: First drying chamber (10); A flash chamber (20) is connected to the first drying chamber (10). A sprayer (21) is provided in the flash chamber (20). The sprayer (21) is used to spray the raw material liquid into the flash chamber (20). The second drying chamber (30) is connected to the flash chamber (20); A refrigeration system is connected to the first drying chamber (10), the flash chamber (20), and the second drying chamber (30), and the refrigeration system is used to capture water vapor and discharge the water vapor; A vacuum exhaust system (50) is connected to the first drying chamber (10), the flash chamber (20), the refrigeration system, and the second drying chamber (30), respectively. The vacuum exhaust system (50) is used to exhaust the vacuum from the first drying chamber (10), the flash chamber (20), the second drying chamber (30), and the refrigeration system. A transport device (60) is installed in the first drying chamber (10), and the output port of the transport device (60) is connected to the second drying chamber (30); It also includes a temperature control device, which includes a first temperature controller disposed in the first drying chamber (10) and a second temperature controller disposed in the second drying chamber (30). The first temperature controller is used to control the temperature of the first drying chamber (10), and the second temperature controller is used to control the temperature of the second drying chamber (30). The bottom of the flash chamber (20) is connected to the top of the first drying chamber (10). The bottom of the flash chamber (20) has a bucket-shaped structure. The center line of the nozzle of the sprayer (21) coincides with the center line of the flash chamber (20). The raw material liquid sprayed by the sprayer (21) moves from the nozzle of the sprayer (21) to the first drying chamber (10). The output port of the transport device (60) is located above the second drying chamber (30); The second drying chamber (30) is provided with an inlet, a second drying space and a discharge port (31) from top to bottom. The inlet is connected to the output port of the transport device (60). A vibration stirring device is provided in the second drying space. The refrigeration system includes a freezer chamber (41), a first freezer (42), a second freezer (43), and a third freezer (44); the first freezer (42) is disposed in the freezer chamber (41), and the freezer chamber (41) is connected to the flash chamber (20); the vacuum exhaust system (50) is provided with an exhaust channel connected to the freezer chamber (41); the second freezer (43) is disposed in the first drying chamber (10), and the third freezer (44) is disposed in the second drying chamber (30); It also includes a feeding device (80) provided at the discharge port (31), the feeding device (80) being used to uniformly convey the stirred frozen particles; the feeding device (80) includes a feeding frame (81), an intermediate funnel (82) provided on the feeding frame (81), a rotating material plate (83), a feeding funnel (84), and a feeding motor (85) for driving the rotating material plate (83) to rotate, the rotating material plate (83) being provided with four material storage cavities (801), and the feeding funnel (84) being provided with two feeding openings (802); The oscillating stirring device includes a stirring mechanism and an oscillating mechanism. The stirring mechanism includes a first motor (32) located outside the second drying chamber (30) and a stirring rod (33) located inside the second drying chamber (30). The first motor (32) drives the stirring rod (33). The oscillating mechanism is located at the bottom of the second drying chamber (30). The oscillating mechanism includes a bracket (34), a support spring (35), a second motor (36), and an oscillating cam (37). The bracket (34) is located on the outer periphery of the second drying chamber (30) and connected to the second drying chamber (30) through the support spring (35). The second motor (36) is located on the bracket (34) and connected to the hub of the oscillating cam (37). It also includes the following steps: The vacuum exhaust system (50) is activated to exhaust the vacuum from the first drying chamber (10), the flash chamber (20), the second drying chamber (30), and the refrigeration system. The vacuum exhaust system (50) is activated to sequentially dry the freezing chamber (41), the first drying chamber (10), and the second drying chamber (30); Start the shaking and stirring device to shake and stir the raw material liquid that has been frozen into frozen granules in the second drying chamber (30) for drying; The temperature of the conveying device (60) in the first drying chamber (10) is controlled between the first temperature and the temperature of the second freezer (43), where the first temperature is the melting temperature of the raw material liquid frozen into frozen particles; The step involves activating the vacuum exhaust system (50) to sequentially dry the freezing chamber (41), the first drying chamber (10), and the second drying chamber (30), specifically including the following steps: Start the first freezer (42) to dry the freezer compartment (41); The second freezer (43) is started to dry the first drying chamber (10); Start the third freezer (44) to dry the second drying chamber (30).

2. The vacuum freeze-drying method according to claim 1, characterized in that, The connection between the vacuum exhaust system (50) and the second drying chamber (30) and the third freezer (44) are both located above the interior of the second drying chamber (30).

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