CN219415446U - Low-temperature freeze dryer - Google Patents

Abstract

The application relates to the field of freeze-drying technology, specifically provides a low temperature freeze dryer, include: the freeze-drying bottle is used for placing the material to be freeze-dried; n low-temperature bins, N being a positive integer greater than or equal to 2, wherein each low-temperature bin has a chamber for accommodating one of the lyophilization vials, and the temperature within the chamber can be reduced to a temperature required for lyophilizing the material in the lyophilization vial; and the control panel is used for regulating and controlling the temperature in the low-temperature bin. The freeze-drying bottle in this application need not to shift the material after freezing in advance to avoid the temperature rapid change or the material that produce because of shifting receives the problem of pollution.

Description

Low-temperature freeze dryer

Technical Field

The application relates to the field of freeze-drying technology, in particular to a low-temperature freeze dryer.

Background

Freeze drying is a technology of drying by utilizing the principle of vacuum sublimation, which is to freeze water-containing materials into solid rapidly at low temperature, and then sublimate ice directly into water vapor without passing through liquid phase under the condition of low temperature and low pressure, thereby dehydrating the materials at low temperature to achieve the aim of drying. The freeze-drying process comprises three steps: freezing the material, namely freezing the material into solid; sublimation drying is carried out, and ice crystals in the material are removed in a sublimation mode; and (3) analyzing and drying, and evaporating the water remained in the material at a higher temperature to enable the residual water to meet the preset requirement. The freeze-drying technology is widely applied in the fields of biological medicine, pharmaceutical preparations, blood materials, foods and the like. Cryogenic freeze-dryer for biological medicine experiments is increasingly favored by people by virtue of the incomparable advantages of the drying method.

However, the existing cryofreeze dryer for biomedical experiments has the following disadvantages when in use: the freeze-drying bottle is required to be placed in a cold trap for pre-freezing, the freeze-drying bottle is required to be transferred to a freeze-drying bin or an external multi-manifold during drying, the temperature can be rapidly changed in the transfer process, and the materials are easy to be polluted, so that the freeze-drying deterioration risk of the materials is caused.

Disclosure of Invention

In order to solve the above-mentioned problem, provide a low temperature freeze dryer in the embodiment of this application, the freeze-drying bottle in this application need not to shift the material after freezing in advance and accomplish to avoid the temperature rapid change or the material that produce because of shifting receive the problem of pollution.

For this reason, the following technical solutions are adopted in the embodiments of the present application:

a cryofreeze dryer, comprising: the freeze-drying bottle is used for placing the material to be freeze-dried; n low-temperature bins, N being a positive integer greater than or equal to 2, wherein each low-temperature bin has a chamber for accommodating one of the lyophilization vials, and the temperature within the chamber can be reduced to a temperature required for lyophilizing the material in the lyophilization vial; and the control panel is used for regulating and controlling the temperature in the cavity.

In the embodiment, the freeze-drying bottle is placed in the low-temperature bin to freeze the materials, the materials do not need to be transferred after prefreezing, and the freeze dryer is directly started to freeze the materials, so that rapid temperature change or pollution of the materials in the transfer process is avoided; meanwhile, the freeze-drying bottle is continuously placed in the low-temperature bin, so that the difference between the internal temperature and the external temperature of the bottle caused by different placement modes can be avoided, the analysis and drying process of unstable biological medical chemicals is influenced, and the quality of material products is guaranteed.

As one possible implementation, a cooling coil is disposed in the cryogenic compartment, and the control panel controls the temperature within the chamber by controlling the cooling coil.

As an implementation manner, a temperature control probe is arranged in the low-temperature bin and is used for monitoring the temperature in the cavity.

As one implementation, the temperature of the chamber may be up to-80 degrees celsius.

As an implementation manner, the method further includes: and the cold trap system is communicated with the freeze-drying bottle and is used for capturing water and organic solvent generated in the material freeze-drying process.

As an implementation manner, the cold trap system is internally provided with a cold trap coil and a cold trap coil temperature control probe.

As one implementation, the N is 2, and the cold trap system is located at the midpoint of the line connecting the 2 cold bins.

As an implementation manner, the control panel is arranged on the cold trap system, the temperatures in the chambers of the two low-temperature cabins are different or the same, and the control panel is provided with a detection display screen which is used for displaying and observing the temperatures of the cold trap system and the chambers in the low-temperature cabins.

As an implementation manner, the method further includes: and the inert gas steel bottle is communicated with the freeze-drying bottle and is used for introducing inert gas into the freeze-drying bottle.

As an implementation manner, the method further includes: the three-way valve is provided with a piston, an inert gas steel bottle interface, a cold trap system interface and a freeze-drying bottle interface respectively; the inert gas steel cylinder connector is communicated with an inert gas steel cylinder; the cold trap system interface is communicated with a cold trap system; the freeze-drying bottle interface is communicated with the freeze-drying bottle.

In summary, the present application has the following beneficial effects:

1. the freeze-drying bottle is placed in the low-temperature bin to freeze materials, the materials do not need to be transferred after prefreezing, and the freeze-drying machine is directly started to freeze the materials, so that rapid temperature change or pollution of the materials in the transfer process is avoided;

2. by continuously placing the freeze-dried bottles in the low-temperature bin, the difference between the internal temperature and the external temperature of the bottles caused by different placing modes can be avoided, the material analysis and drying process is influenced, and the material quality is ensured;

3. the freeze-drying temperature can be adjusted at will within the range of-80 ℃ to 0 ℃ by placing the freeze-drying bottle in the low-temperature bin, so as to realize the fumbling of the unstable biomedical chemical low-temperature freeze-drying process;

4. the freeze-drying bottle is connected with the inert gas steel bottle, inert gas is introduced through the three-way valve before the material is taken down, and then the material is stored in a sealing mode, so that the problem that unstable biological medical chemicals are degraded due to contact with water vapor or oxygen in the air can be avoided.

Drawings

In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present application, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.

The various regions, shapes and relative sizes, positional relationships between them shown in the drawings are merely exemplary, may in practice deviate due to manufacturing tolerances or technical limitations, and one skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions as actually required.

Like elements are denoted by like reference numerals throughout the various figures. For clarity, various parts in the drawings are not drawn to scale, and certain features may be exaggerated or omitted to more clearly illustrate and explain the present application.

Fig. 1 is a schematic structural diagram of a cryofreeze dryer provided in an embodiment of the present application;

fig. 2 is a schematic diagram of an internal structure of a cryofreeze dryer provided in an embodiment of the present application;

fig. 3 is a schematic structural diagram of a three-way valve according to an embodiment of the present application.

In the figure; 1. a cold trap system; 11. a cold trap coil; 12. a cold trap coil temperature control probe; 2. a first cryogenic bin; 21. a first cooling coil; 22. a first temperature control probe; 3. an inert gas cylinder; 4. a pipe; 5. a three-way valve; 51. a piston; 52. an inert gas cylinder port; 53. a cold trap system interface; 54. a freeze-drying bottle interface; 6. freeze-drying the bottle; 7. a second low temperature bin; 71. a second cooling coil; 72. a second temperature control probe; 8. and a control panel.

Detailed Description

The technical solutions in the embodiments of the present application will be described below with reference to the drawings in the embodiments of the present application.

In the description of the present application, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," etc. indicate orientations or positional relationships based on the orientations or positional relationships illustrated in the drawings, are merely for convenience in describing the present application and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be configured and operated in a particular orientation, and therefore should not be construed as limiting the present application.

Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present application, the meaning of "plurality" is at least two, such as two, three, etc., unless explicitly defined otherwise.

In this application, unless specifically stated and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.

In this application, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be the first and second features in direct contact, or the first and second features in indirect contact via an intervening medium. Moreover, a first feature being "above," "over" and "on" a second feature may be a first feature being directly above or obliquely above the second feature, or simply indicating that the first feature is level higher than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is less level than the second feature.

In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means 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 present application. In this specification, schematic representations of the above terms are not necessarily directed 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. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.

When the existing low-temperature freeze dryer for biological medicine experiments is used, a freeze-drying bottle is required to be placed in a cold trap for pre-freezing, the freeze-drying bottle is required to be transferred to a freeze-drying bin or an external multi-manifold during drying, and the temperature can be rapidly changed or the materials can be polluted in the transfer process, so that the freeze-drying deterioration risk of the materials is caused; different placement modes of the freeze-drying bottle often cause different temperatures inside and outside the bottle, and influence the analysis and drying process of unstable biological medical chemicals, thereby influencing the quality of freeze-drying material products; after the material is freeze-dried, the material is required to be taken out from a bin and then stored in a sealing cover, and in the process, unstable biomedical chemicals are degraded due to contact with water vapor or oxygen in the air.

In order to avoid the above technical problems, the present application provides a lyophilization apparatus to overcome the above drawbacks of the prior art. The two low-temperature bins of the low-temperature freeze dryer not only solve the problem that freeze drying is easy to deteriorate due to temperature change, but also can meet the fumbling of different low-temperature freeze drying processes; in addition, the inert gas steel cylinder is connected with the three-way valve to provide inert gas protection for the freeze-dried material product, and the inert gas is introduced before the material is taken down for sealing and preserving, so that the problem of quality degradation of the material caused by contact with water vapor or oxygen can be avoided

1-2, a cryofreeze dryer disclosed as an embodiment of the present application, comprising: cold trap system 1, low temperature storehouse, inert gas steel bottle 3, pipeline 4, three-way valve 5, freeze-drying bottle 6 and control panel 8.

Wherein the freeze-drying bottle 6 is respectively communicated with the inert gas steel bottle 3 and the pipeline 4 of the cold trap system 1 through a three-way valve 5.

Fig. 3 is a schematic structural diagram of the three-way valve 5 provided in the embodiment of the present application. Referring to fig. 3, specifically, the three-way valve 5 is provided with a piston 51, an inert gas cylinder port 52, a cold trap system port 53 and a freeze-drying cylinder port 54. The inert gas cylinder connector 52 is detachably and hermetically connected with the inert gas cylinder 3; the cold trap system interface 53 is detachably and hermetically connected with the cold trap system 1; the freeze-drying bottle interface 54 is detachably and sealingly connected with the freeze-drying bottle 6.

The freeze-drying bottle 6 is selectively communicated with or closed by a piston 51 of the three-way valve 5 and the inert gas cylinder 3 or the cold trap system 1. The operator can switch between the different channels by rotating the piston 51 of the three-way valve 5. Wherein, when the freeze-drying bottle 6 and the cold trap system 1 are communicated with each other, the cold trap system 1 can be used for capturing water and organic solvent generated in the material freeze-drying process, and in particular, the cold trap system 1 captures the sublimated or evaporated water and organic solvent gas of the freeze-drying bottle 6 on the cooling surface in a condensation manner. When the inert gas steel bottle 3 is communicated with the freeze-drying bottle 6, inert gas is introduced before the material is taken down, and then the material is sealed and stored, so that the problem of quality degradation of the material caused by contact with water vapor or oxygen can be avoided.

In a specific embodiment, referring to fig. 2, a cold trap coil 11 and a cold trap coil temperature control probe 12 are disposed within the cold trap system 1. The control panel 8 is installed on the cold trap system 1, and the cold trap coil temperature control probe 12 and the control panel 8 are mutually and electrically connected, the temperature of the cold trap coil 11 detected by the cold trap coil temperature control probe 12 can be transmitted to the control panel 8, and an operator can accurately control the temperature of the cold trap coil 11 through the control panel 8 so as to conveniently capture water and organic solvents in the freeze-drying bottle 6.

Some examples provide that the cryogenic bins are N, N being a positive integer greater than or equal to 2, each having a chamber containing one lyophilization flask 6, and the temperature within the chamber can be reduced to the temperature required to freeze dry the material in the lyophilization flask 6. The number of the low-temperature bins can be increased by an operator according to the requirement, for example, the number of the low-temperature bins can be 2, 3 and 4. While the shape of the low-temperature bin can be a hollow rectangle or a hollow cylinder, and the application is not limited herein. A cooling coil is further arranged at the edge of the low-temperature bin chamber, and the cooling coil is spirally coiled and fully distributed on the circumferential side wall of the low-temperature bin chamber; the cooling coil is circulated with a cooling medium for regulating the temperature in the chamber, wherein the cooling medium may be a refrigerant such as freon or other liquid with relatively high heat exchange efficiency, and the application is not limited herein. The temperature control probe is arranged in the chamber of the low-temperature bin, is vertically arranged in the chamber and is in contact with the cooling coil, and is used for detecting the temperature in the low Wen Cangqiang chamber and feeding back to the control panel 8, so that an operator can conveniently control the cooling coil to regulate and control the temperature in the chamber through the control panel 8.

By way of example, the temperature in the chamber may be precisely controlled between-80 degrees celsius and 0 degrees celsius under the control of the cooling coil, e.g. the temperature in the chamber may be-80 ℃, -75 ℃, -70 ℃, -65 ℃, -60 ℃, -55 ℃, -50 ℃, -45 ℃, -40 ℃, -35 ℃, -30 ℃, -25 ℃, -20 ℃, -15 ℃, -10 ℃, -5 ℃ and 0 ℃.

Meanwhile, the low-temperature bin superimposes the pre-freezing, the analysis, the drying and the temperature control functions of the materials, so that operators can conveniently find out the low-temperature freeze-drying process of unstable biological medical chemicals.

Illustratively, the labile biomedical chemical may be a sensitive material such as a biologic, blood product, gene drug, or the like.

In a specific embodiment, two cryogenic chambers are provided, including a first cryogenic chamber 2 and a second cryogenic chamber 7, where the first cryogenic chamber 2 and the second cryogenic chamber 7 are symmetrically disposed with respect to the cold trap system 1, i.e. the cold trap system 1 is located at a midpoint of a connection line between the 2 cryogenic chambers. A first cooling coil 21 and a first temperature control probe 22 are arranged in a cavity in the first low-temperature bin 2; a second cooling coil 71 and a second temperature control probe 72 are arranged in the second low-temperature bin 7. The first temperature control probe 22 and the second temperature control probe 72 can monitor the temperatures in the chambers of the first cryogenic chamber 2 and the second cryogenic chamber 7, respectively, in real time. The first cooling coil 21 and the second cooling coil 71 precisely control the temperature within the chambers of the first cryogenic chamber 2 and the second cryogenic chamber 7, respectively. The temperature of the chambers in the first low-temperature bin 2 and the second low-temperature bin 7 can reach-80 ℃, and the freeze-drying temperature of the freeze-drying bottle 6 can be adjusted at will between-80 ℃ and 0 ℃ and can be controlled accurately.

In addition, it should be noted that the first temperature control probe 22 and the second temperature control probe 72 are electrically connected with the control panel 8, the temperatures monitored by the first temperature control probe 22 and the second temperature control probe 72 are fed back to the control panel 8 in real time, the operator can respectively control the temperatures in the first low temperature chamber 2 and the second low temperature chamber 7 through the control panel 8, and the first low temperature chamber 2 and the second low temperature chamber 7 can respectively set the same or different temperatures through the control panel 8.

In addition, a detection display screen is arranged on the control panel 8, and the detection display screen is used for displaying temperature data of the cold trap system 1 and each low-temperature bin in visual observation.

It should be noted that, how the control panel 8 regulates and controls the temperatures of the plurality of cold-storage bins and the cold trap system 1 respectively is in the prior art, for example, the control panel 8 may be a programmable logic controller PLC, the first cooling coil 21 and the second cooling coil 71 may be connected with cooling pumps for providing power respectively, and the control panel 8 controls the two different cooling pumps to pump cooling medium into the first cooling coil 21 and the second cooling coil 71 and circulate respectively, which is not described herein again.

For a more complete understanding of this application, the following examples are set forth. These examples are provided to illustrate embodiments of the present application in detail and should not be construed as limiting the scope of the present application in any way.

Example 1

Referring to fig. 1, a cryofreeze dryer comprises a control panel 8, a cold trap system 1, a first cryochamber 2, a second cryochamber 7 and an inert gas cylinder 3 connected with a three-way valve 5; wherein the control panel (8) is connected with a cold trap coil temperature control probe 12 for respectively regulating and controlling the cold trap system, a first temperature control probe 22 for regulating and controlling the temperature of the first low-temperature bin chamber and a second temperature control probe 72 for regulating and controlling the temperature of the second low-temperature bin chamber; the cold trap system 1 is used for capturing water and organic solvents; the chambers of the first low-temperature bin 2 and the second low-temperature bin 7 are used for placing a freeze-drying bottle 6 for containing sample materials; the inert gas steel cylinder 3 is connected with the three-way valve 5 and can provide inert gas protection for the freeze-dried material product.

The implementation principle of the cryofreeze dryer disclosed in embodiment 1 of the application is as follows: firstly, setting a cold trap system 1 and low-temperature bins (2 and 7) to be at a target temperature of-80 ℃ through a control panel 8, and placing a freeze-drying bottle 6 filled with a biological medicine solution to be freeze-dried into the low-temperature bins (2 and 7) for pre-freezing treatment after the target temperature is reached; rotating the three-way valve piston 51 after the pre-freezing beam so as to enable the cold trap system 1 to be communicated with the freeze-drying bottle 6; starting the freeze dryer to freeze dry, and simultaneously respectively adjusting the temperature of the low-temperature bins (2 and 7) to be target temperature through the control panel 8 (different temperatures can be respectively set for the low-temperature bins (2 and 7); after the drying is finished, the three-way valve piston 51 is rotated to enable the freeze-drying bottle 6 to be communicated with the inert gas steel bottle 3, and inert gas is introduced to preserve materials in the inert gas atmosphere; the three-way valve piston 51 is rotated to close the three-way valve 5, and after the pipeline is disassembled, the freeze-dried materials are taken out of the low-temperature bins (2 and 7) and are rapidly placed in a set preservation environment.

The positional relationship, the number, the structural shape, the gas circulation direction and the like of each part of the low-temperature freeze dryer provided by the embodiment of the application are not limited to the above embodiment, and all technical schemes realized under the principle of the application are within the protection scope of the scheme. Any one or more embodiments or illustrations in the specification, combined in a suitable manner, are within the scope of the present disclosure.

Finally, the above embodiments are only used to illustrate the technical solutions of the present application. It will be appreciated by those skilled in the art that, although the present application has been described in detail with reference to the foregoing embodiments, various modifications may be made to the technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof. Such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.

Claims (10)

1. A cryofreeze dryer, comprising:

a freeze-drying bottle (6) for placing the material to be freeze-dried;

n low-temperature bins, N being a positive integer greater than or equal to 2, wherein each low-temperature bin has a chamber accommodating one of the lyophilization vials (6), and the temperature within the chamber can be reduced to the temperature required to freeze-dry the material in the lyophilization vial (6);

and a control panel (8) for regulating the temperature in the chamber.

2. The cryofreeze dryer of claim 1 wherein a cooling coil is disposed within the cryobin, the control panel controlling the temperature within the chamber by controlling the temperature of the cooling coil.

3. The lyophilization machine according to claim 1, wherein a temperature control probe is disposed in the low temperature chamber for monitoring the temperature in the chamber.

4. The lyophilizer of claim 1, wherein the chamber is at a temperature of up to-80 degrees celsius.

5. The cryofreeze dryer of any one of claims 1-4, further comprising:

and the cold trap system (1) is communicated with the freeze-drying bottle (6) and is used for capturing water and organic solvent generated in the material freeze-drying process.

6. A cryofreeze dryer according to claim 5 wherein the cold trap system (1) is internally provided with a cold trap coil (11) and a cold trap coil temperature control probe (12).

7. The lyophilizer according to claim 5, wherein N is 2 and the cold trap system (1) is located at the midpoint of the line connecting the 2 cold bins.

8. The cryofreeze dryer according to claim 7, wherein the control panel (8) is arranged on the cold trap system (1), the temperatures in the chambers of the two cold traps are different or the same, and a detection display screen is arranged on the control panel (8) and is used for displaying and observing the temperatures of the cold trap system (1) and the chambers in each cold trap.

9. The cryofreeze dryer of any one of claims 1-4, further comprising:

and the inert gas steel bottle (3) is communicated with the freeze-drying bottle (6) and is used for introducing inert gas into the freeze-drying bottle (6).

10. The cryofreeze dryer of any one of claims 1-4, further comprising:

the three-way valve (5) is respectively provided with a piston (51), an inert gas steel cylinder interface (52), a cold trap system interface (53) and a freeze-drying bottle interface (54); the inert gas steel cylinder interface (52) is communicated with an inert gas steel cylinder (3); the cold trap system interface (53) is communicated with a cold trap system (1); the freeze-drying bottle interface (54) is communicated with the freeze-drying bottle (6).