Pre-freezing device and pre-freezing method

Abstract

The embodiment of the invention provides a pre-freezing device and a pre-freezing method. The pre-freezing device comprises a box body with an opening and a box cover covering the box body. The box body sequentially comprises a shell, a heat preservation layer and a cold transfer layer from outside to inside, a sample bin is arranged on one side of the cold transfer layer, a liquid nitrogen bin is arranged on the other side of the cold transfer layer, and an injection hole is formed in the cold transfer layer. The liquid nitrogen bin is separated from the sample bin, so that the sample is not in direct contact with the liquid nitrogen, and the risk that the sample is directly polluted by impurities or pollutants in the liquid nitrogen is reduced. The low temperature of the liquid nitrogen is efficiently transferred to the sample in the sample bin through the cold transfer layer, so that the sample can quickly reach an ideal pre-freezing temperature, the pre-freezing time is shortened, and the pre-freezing efficiency and effect are enhanced. Furthermore, the liquid nitrogen bin is provided with a liquid nitrogen leading-out pipe and an observation window, and the liquid nitrogen leading-out pipe is used for recycling the residual liquid nitrogen in the liquid nitrogen bin for secondary utilization, so that the repeated utilization rate of the liquid nitrogen is increased.

Description

Technical Field

[0001] The embodiments of the present application relate to but are not limited to the field of pre-freezing technology, and in particular to a pre-freezing device and a pre-freezing method. Background Art

[0002] During the drug pre-freezing stage, the pre-freezing temperature needs to be strictly controlled (usually a few degrees lower than the eutectic point of the drug). If the pre-freezing temperature is not low enough, the drug may not be completely frozen and will expand and bubble during vacuum sublimation; if the pre-freezing temperature is too low, it will not only increase unnecessary energy consumption, but also reduce the survival rate of some biological drugs after freeze-drying.

[0003] At present, liquid nitrogen is usually used to prefreeze samples in laboratory environments. In order to achieve the ideal prefreezing temperature, if the experimenter directly immerses the sample in liquid nitrogen, the reuse rate of liquid nitrogen will be reduced, which may seriously cause sample contamination. Another method is to place the sample in an ultra-low temperature refrigerator for prefreezing, but this method often takes too long to prefreeze. Summary of the invention

[0004] The following is a summary of the subject matter described in detail herein. This summary is not intended to limit the scope of the claims.

[0005] The embodiments of the present application provide a pre-freezing device and a pre-freezing method, wherein the pre-freezing device can improve the reuse rate of liquid nitrogen and reduce the risk of sample contamination during the pre-freezing process, thereby enhancing the pre-freezing efficiency and effect.

[0006] In a first aspect, an embodiment of the present application provides a pre-freezing device, comprising: a box body provided with an opening and a box cover covering the box body, the box body comprising an outer shell, a heat-insulating layer and a cold transfer layer from the outside to the inside; a sample bin is provided on one side of the cold transfer layer, and a liquid nitrogen bin is provided on the other side, and an injection hole is provided on the cold transfer layer; the liquid nitrogen bin is provided with a liquid nitrogen outlet pipe and an observation window, and the liquid nitrogen outlet pipe is used to recover the remaining liquid nitrogen in the liquid nitrogen bin.

[0007] In combination with the first aspect, in a possible implementation manner of the first aspect, a door is provided on the housing, and the door corresponds to a position of the sample chamber.

[0008] In combination with the first aspect, in a possible implementation of the first aspect, one end of the liquid nitrogen outlet pipe is passed through the outer shell and the insulation layer and is located inside the liquid nitrogen tank; a push-type valve is provided in the liquid nitrogen outlet pipe, and the push-type valve is used to open and close the flow of liquid nitrogen.

[0009] In combination with the first aspect, in a possible implementation of the first aspect, the observation window is provided through a side wall of the liquid nitrogen bin and the outer shell, and the observation window is used to observe a remaining amount of liquid nitrogen in the liquid nitrogen bin.

[0010] In combination with the first aspect, in a possible implementation manner of the first aspect, a temperature sensor is provided on the cold transfer layer, a display screen is provided on the housing, and the temperature sensor is connected to the display screen.

[0011] In combination with the first aspect, in a possible implementation of the first aspect, an outer wall of the cooling layer abuts against an inner wall of the heat preservation layer, and the sample chamber is located inside the cooling layer.

[0012] In combination with the first aspect, in a possible implementation manner of the first aspect, a silicone layer is disposed on the injection hole.

[0013] In combination with the first aspect, in a possible implementation of the first aspect, the box door and the box cover are made of stainless steel and polyurethane foam.

[0014] In combination with the first aspect, in a possible implementation of the first aspect, the thermal insulation layer is made of polyurethane foam.

[0015] In the second aspect, an embodiment of the present application provides a pre-freezing method, which is applied to the pre-freezing device as described above, including: injecting liquid nitrogen into the liquid nitrogen bin from the injection hole; when the displayed temperature reaches the preset temperature, placing the sample in the sample bin for pre-cooling until the state of the sample meets the preset state, thereby obtaining a pre-frozen sample.

[0016] A pre-freezing device provided in an embodiment of the present application comprises a box body with an opening and a box cover covering the box body. The box body comprises an outer shell, a heat-insulating layer and a cold transfer layer from outside to inside, wherein a sample bin is provided on one side of the cold transfer layer, a liquid nitrogen bin is provided on the other side, and an injection hole is provided on the cold transfer layer. Due to the separation design of the liquid nitrogen bin and the sample bin, the sample does not directly contact the liquid nitrogen, but heat is transferred through the cold transfer layer, thereby avoiding the risk of direct contamination of the sample by impurities or contaminants in the liquid nitrogen, and ensuring the purity of the sample. At the same time, the low temperature of the liquid nitrogen is efficiently transferred to the sample in the sample bin through the cold transfer layer. Compared with the traditional ultra-low temperature refrigerator pre-freezing method, this method can reach the ideal pre-freezing temperature more quickly, thereby shortening the pre-freezing time. The liquid nitrogen bin is provided with a liquid nitrogen outlet pipe and an observation window, and the liquid nitrogen outlet pipe can recycle the remaining liquid nitrogen in the liquid nitrogen bin. Compared with the traditional method of directly immersing the sample in liquid nitrogen, this method significantly reduces the waste of liquid nitrogen, improves the reuse rate of liquid nitrogen, and reduces the experimental cost. In addition, the observation window enables the experimenter to visually observe the liquid nitrogen situation in the liquid nitrogen tank, including the remaining amount of liquid nitrogen and the pre-freezing progress, thereby improving the experimental efficiency. In addition, the box body includes an outer shell, a heat preservation layer and a cold transfer layer from the outside to the inside. This multi-layer structure design effectively reduces heat loss, ensures the stability of the low-temperature environment during the pre-freezing process, and improves the pre-freezing effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 is a side structural schematic diagram of a pre-freezing device provided in an embodiment of the present application;

[0018] Figure 2 is a front view structural schematic diagram of a pre-freezing device provided in an embodiment of the present application;

[0019] Figure 3 is a schematic diagram of the top view of the pre-freezing device provided in an embodiment of the present application;

[0020] Reference numerals: box body 110 ; box cover 120 ; outer shell 121 ; heat-insulating layer 122 ; cooling layer 123 ; sample chamber 124 ; liquid nitrogen chamber 125 ; injection hole 10 ; liquid nitrogen outlet pipe 130 ; observation window 140 ; ​​push-type valve 20 ; box door 210 ; temperature sensor 30 ; display screen 150 ; silicone layer 310 . DETAILED DESCRIPTION

[0021] In order to make the purpose, technical solution and advantages of the present application more clearly understood, the present application is further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and are not used to limit the present application.

[0022] It should be noted that, although the logical order is shown in the flowchart, in some cases, the steps shown or described can be performed in a different order from that in the flowchart. The terms "first", "second", etc. in the specification, claims and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequence. It should be noted that the structures, proportions, sizes, etc. illustrated in the drawings of this specification are only used to match the contents disclosed in the specification for people familiar with this technology to understand and read, and are not used to limit the limiting conditions that the present invention can be implemented, so they have no technical substantive significance. Any modification of the structure, change of the proportional relationship or adjustment of the size, without affecting the effects that the present invention can produce and the purposes that can be achieved, should still fall within the scope of the technical content disclosed by the present invention. At the same time, the terms such as "upper", "lower", "left", "right", "middle" and "one" quoted in this specification are only for the convenience of narration, and are not used to limit the scope of the implementation of the present invention. The change or adjustment of the relative relationship should also be regarded as the scope of the implementation of the present invention without substantially changing the technical content.

[0023] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application belongs. The terms used herein are only for the purpose of describing the embodiments of this application and are not intended to limit this application.

[0024] Vacuum freeze-drying technology is a drying technology that freezes wet materials or solutions into a solid state at a relatively low temperature (-10℃~-50℃), and then sublimates the water in the solution into a gaseous state without passing through the liquid state under vacuum (1.3~13 Pa), and finally dehydrates the material. The process includes three stages: freezing, sublimation and re-drying. During the vacuum freeze-drying process, the material does not have the problem of surface hardening, and a porous sponge is formed inside, so it has excellent rehydration properties and can be restored to the state before drying in a short time. At present, vacuum freeze-drying technology has been applied to many occasions.

[0025] Since the drying process is carried out at a very low temperature and is basically isolated from the air, it effectively inhibits the biological, chemical or physical changes of heat-sensitive substances, and better preserves the active substances in the raw materials, as well as the color of the raw materials. In the vacuum pre-freeze drying process, the dried medicine needs to be pre-frozen first, and then the water is directly changed from ice to gas under vacuum to dry the medicine. During the entire sublimation stage, the medicine must be kept in a frozen state, otherwise a product with good properties cannot be obtained.

[0026] During the drug pre-freezing stage, the pre-freezing temperature must be strictly controlled (usually a few degrees lower than the eutectic point of the drug). If the pre-freezing temperature is not low enough, the drug may not be completely frozen and will expand and bubble during vacuum sublimation; if the pre-freezing temperature is too low, it will not only increase unnecessary energy consumption, but also reduce the survival rate of some biological drugs after freeze-drying. At present, liquid nitrogen is commonly used to pre-freeze samples in laboratory environments, but if the samples are directly immersed in liquid nitrogen, the reuse rate of liquid nitrogen will be reduced, which may seriously cause sample contamination. Another pre-freezing method is to place the sample in a constant temperature pre-freezing ultra-low temperature refrigerator for pre-freezing, but this method often takes too long to pre-freeze.

[0027] In view of this, the embodiment of the present application provides a pre-freezing device and a pre-freezing method, the pre-freezing device includes a box body with an opening and a box cover covering the box body. The box body includes an outer shell, a heat preservation layer and a cold transfer layer from the outside to the inside, wherein a sample bin is provided on one side of the cold transfer layer, a liquid nitrogen bin is provided on the other side, and an injection hole is provided on the cold transfer layer. Due to the separation design of the liquid nitrogen bin and the sample bin, the sample does not directly contact the liquid nitrogen, but heat is transferred through the cold transfer layer, thereby avoiding the risk of the sample being directly contaminated by impurities or contaminants in the liquid nitrogen, and ensuring the purity of the sample. At the same time, the low temperature of the liquid nitrogen is efficiently transferred to the sample in the sample bin through the cold transfer layer. Compared with the traditional ultra-low temperature refrigerator pre-freezing method, this method can reach the ideal pre-freezing temperature more quickly, thereby shortening the pre-freezing time. The liquid nitrogen bin is provided with a liquid nitrogen outlet pipe and an observation window, and the liquid nitrogen outlet pipe can recycle the remaining liquid nitrogen in the liquid nitrogen bin. Compared with the traditional method of directly immersing the sample in liquid nitrogen, this method significantly reduces the waste of liquid nitrogen, improves the reuse rate of liquid nitrogen, and reduces the experimental cost. In addition, the observation window enables the experimenter to visually observe the liquid nitrogen situation in the liquid nitrogen tank, including the remaining amount of liquid nitrogen and the pre-freezing progress, so that the experimenter can adjust the experimental conditions in time and improve the experimental efficiency. The box body includes the outer shell, the insulation layer and the cold transfer layer from the outside to the inside. This multi-layer structure design effectively reduces the heat loss, ensures the stability of the low temperature environment during the pre-freezing process, and improves the pre-freezing effect.

[0028] The embodiments of the present application are further described below in conjunction with the accompanying drawings.

[0029] See also Figure 1 , Figure 1: is an overall structural diagram of the pre-freezing device provided in an embodiment of the present application. The pre-freezing device includes a box body 110 provided with an opening and a box cover 120 covering the box body 110 to ensure the sealing of the pre-freezing process. The internal structure of the box body 110 is clearly layered, and includes an outer shell 121, an efficient heat-insulating insulation layer 122 and a cold transfer layer 123 from the outside to the inside, which together create a stable and low-temperature pre-freezing environment. A sample bin 124 for placing the sample to be pre-frozen is provided on one side of the cold transfer layer 123, and a liquid nitrogen bin 125 for storing liquid nitrogen and effectively transferring the low-temperature energy of liquid nitrogen is provided on the other side. By separating the liquid nitrogen bin 125 from the sample bin 124, the sample does not directly contact the liquid nitrogen, but is heat transferred through the cold transfer layer 123, thereby avoiding the risk of the sample being directly contaminated by impurities or contaminants in the liquid nitrogen, and ensuring the purity of the sample. At the same time, the low temperature of liquid nitrogen is efficiently transferred to the sample in the sample bin 124 through the cold transfer layer 123. Compared with the traditional ultra-low temperature refrigerator pre-freezing method, this method can reach the ideal pre-freezing temperature more quickly, thereby shortening the pre-freezing time. An injection hole 10 is provided on the cold transfer layer 123, through which liquid nitrogen can be easily injected into the liquid nitrogen bin 125 to achieve a fast and uniform pre-freezing effect. Furthermore, the liquid nitrogen bin 125 is provided with a liquid nitrogen outlet pipe 130 and an observation window 140. The liquid nitrogen outlet pipe 130 is used to recycle the remaining liquid nitrogen in the liquid nitrogen bin 125, thereby reducing the waste of liquid nitrogen and improving the reuse rate of liquid nitrogen.

[0030] In a feasible embodiment, one end of the liquid nitrogen outlet pipe 130 penetrates into the liquid nitrogen bin 125, and the other end passes through the outer shell 121 and the insulation layer 122, so as to facilitate the safe recovery and reuse of the remaining liquid nitrogen. The push-type valve 20 built into the liquid nitrogen outlet pipe 130 can realize the opening and closing of the liquid nitrogen flow, recover the liquid nitrogen for secondary use, and thus improve the reuse rate of the liquid nitrogen.

[0031] In a feasible embodiment, the observation window 140 is provided through the side wall of the liquid nitrogen bin 125 and the outer shell 121, allowing the user (experimenter) to directly observe the remaining amount of liquid nitrogen in the liquid nitrogen bin 125 without opening the pre-freezing device, providing an important reference for experimental preparation. Exemplarily, the observation window 140 can be made of transparent materials such as glass, so that the liquid nitrogen injection, remaining amount, etc. can be observed from the outer shell 121, which greatly improves the convenience of operation and the visualization of the experimental process.

[0032] In a feasible embodiment, the outer wall of the cold transfer layer 123 abuts against the inner wall of the heat preservation layer 122, forming an effective heat isolation and transfer interface, which not only reduces the heat loss, but also ensures that the cold transfer layer 123 can quickly and evenly transfer the low temperature to its core area (sample chamber 124). The sample chamber 124 is built into the cold transfer layer 123, so that the sample can be directly affected by the low temperature environment, thereby achieving a fast and efficient pre-freezing effect. The entire structure is compact and efficient, providing an ideal solution for laboratory sample storage and pre-freezing work.

[0033] In a possible embodiment, if Figure 2 As shown, the housing 121 is provided with a door 210, and the position of the door 210 corresponds to the position of the sample chamber 124. The user can open and close the door 210 at any time to place and take out the sample.

[0034] In a feasible embodiment, a temperature sensor 30 is provided on the cold transfer layer 123, and the temperature sensor 30 is embedded in the bottom of the sample chamber 124, and can detect and feedback the temperature change in the pre-freezing process in real time. A display screen 150 is provided on the housing 121, and the wire of the temperature sensor 30 passes through the insulation layer 122 and is connected to the display screen 150 (such as a liquid crystal display screen). The display screen 150 is responsible for receiving and displaying the temperature information transmitted by the temperature sensor 30, so that the user can observe the temperature of the sample chamber 124 in real time.

[0035] In a possible embodiment, if Figure 3 As shown, a silicone layer 310 is provided on the injection hole 10, which not only enhances the sealing performance but also facilitates the opening and closing of the injection of liquid nitrogen.

[0036] In a feasible embodiment, the door 210 and the cover 120 adopt a composite structure of stainless steel and polyurethane foam, wherein the inner layer is a durable stainless steel, which effectively resists external impact and corrosion; and the middle layer is filled with high-quality polyurethane foam, which not only enhances the thermal insulation performance of the structure, but also improves the overall buffering and shock absorption effect. In addition, the shell 121 can be made of high-strength, corrosion-resistant materials such as acrylonitrile-butadiene-styrene (ABS) and polymethyl methacrylate (PMMA) to meet the needs of different experimental environments. The cold transfer layer 123 can be made of materials with excellent thermal conductivity and acid-base resistance, such as stainless steel, to ensure the efficient transfer of low-temperature energy and the long-term stable operation of the equipment. In addition, the thermal insulation layer 122 can be made of insulating materials with low thermal conductivity, such as polyurethane foam, etc. as its preparation material, which effectively blocks the penetration of external heat and ensures the low-temperature environment of the pre-freezing device during long-term use. It is worth noting that the materials used in the pre-freezing device provided in the embodiment of the present application (ABS, stainless steel, polyurethane foam, silicone, glass, etc.) are all low-priced, widely used, and have a relatively mature production system, which is conducive to large-scale production. It should be noted that the embodiment of the present application does not set strict restrictions on the preparation materials of the box door 210, the box cover 120, the shell 121, and the insulation layer 122, which means that in actual applications, flexible selection and optimization can be made according to various factors such as experimental conditions, performance requirements, and cost considerations to achieve the best pre-freezing effect and economic benefits.

[0037] In addition, an embodiment of the present application provides a pre-freezing method, which can be applied to the pre-freezing device described in the previous embodiment. The pre-freezing method includes but is not limited to steps 410 to 420.

[0038] Step 410: injecting liquid nitrogen into the liquid nitrogen tank 125 from the injection hole 10;

[0039] Step 420: When the display temperature of the display screen 150 reaches the preset temperature, the sample is placed in the sample chamber 124 for precooling until the state of the sample meets the preset state, thereby obtaining a pre-frozen sample.

[0040] The following is a specific example to illustrate the use of the pre-freezing method.

[0041] Step 1: Open the box cover 120, open the liquid nitrogen injection hole 10, inject liquid nitrogen into the liquid nitrogen bin 125, and observe the injection amount of liquid nitrogen through the observation window 140 until the liquid nitrogen bin 125 is completely filled; Step 2: Observe the temperature displayed on the display screen 150 until the temperature reaches the ideal temperature value; Step 3: Open the box door 210, place the sample at the bottom of the sample bin 124, and close the box door 210. Let it stand for 10 minutes (if the sample volume is large, the standing time can be increased); Step 4: The box door 210 can be opened at any time during the pre-freezing process to observe the sample status; Step 5: After the sample is frozen, immediately take out the sample and transfer it to the freeze-drying equipment for vacuum freeze drying; Step 6: Press the push valve 20 of the liquid nitrogen outlet pipe 130 to export and recycle the remaining liquid nitrogen.

[0042] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present application. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A pre-freezing device, characterized in that: include: A box body with an opening and a box cover covering the box body are provided, and the box body includes an outer shell, a heat-insulating layer and a cold transfer layer from the outside to the inside; a sample bin is provided on one side of the cold transfer layer, and a liquid nitrogen bin is provided on the other side, and an injection hole is provided on the cold transfer layer; the liquid nitrogen bin is provided with a liquid nitrogen outlet pipe and an observation window, and the liquid nitrogen outlet pipe is used to recover the remaining liquid nitrogen in the liquid nitrogen bin.

2. A pre-freezing device according to claim 1, characterized in that: The housing is provided with a box door, and the box door corresponds to the position of the sample chamber.

3. A pre-freezing device according to claim 1, characterized in that: One end of the liquid nitrogen outlet pipe is passed through the outer shell and the insulation layer and is located inside the liquid nitrogen warehouse; a push-type valve is provided in the liquid nitrogen outlet pipe, and the push-type valve is used to open and close the flow of liquid nitrogen.

4. A pre-freezing device according to claim 1, characterized in that: The observation window is arranged through the side wall of the liquid nitrogen bin and the outer shell, and the observation window is used to observe the remaining amount of liquid nitrogen in the liquid nitrogen bin.

5. A pre-freezing device according to claim 1, characterized in that: A temperature sensor is arranged on the cold transfer layer, a display screen is arranged on the shell, and the temperature sensor is connected to the display screen.

6. A pre-freezing device according to claim 1, characterized in that: The outer wall of the cooling layer abuts against the inner wall of the heat preservation layer, and the sample chamber is located inside the cooling layer.

7. A pre-freezing device according to claim 1, characterized in that: A silica gel layer is arranged on the injection hole.

8. A pre-freezing device according to claim 2, characterized in that: The box door and the box cover are made of stainless steel and polyurethane foam.

9. A pre-freezing device according to claim 1, characterized in that: The thermal insulation layer is made of polyurethane foam.

10. A prefreezing method, characterized in that: The pre-freezing device according to any one of claims 1 to 9, wherein the pre-freezing method comprises: Inject liquid nitrogen into the liquid nitrogen tank from the injection hole; When the displayed temperature reaches the preset temperature, the sample is placed in the sample compartment for precooling until the state of the sample meets the preset state, thereby obtaining a prefrozen sample.

Images