A continuous slurry nitrogen production machine

By designing a continuous slurry nitrogen preparation machine and utilizing the alternating use of vacuum barrels and the vacuum control of a Stirling refrigerator, the problem of low efficiency in slurry nitrogen preparation was solved, and efficient and continuous preservation of biological samples through freezing was achieved.

CN116907115BActive Publication Date: 2026-04-14UNIV OF SHANGHAI FOR SCI & TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-07-12
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

Existing slurry nitrogen preparation processes require frequent vacuuming, resulting in low efficiency and long processing times, which cannot meet the needs of continuous biological sample preservation.

Method used

A continuous slurry nitrogen preparation machine was designed. By setting up two sets of vacuum tanks with pumping pipes and control valves, the vacuum tanks can be used alternately. Combined with the vacuuming and repressurization control of the Stirling refrigerator and the condensation chamber, the efficiency of biological sample freezing is improved.

Benefits of technology

This achieves efficient and continuous biological sample freezing process, reduces waiting time, and improves sample preservation efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to the technical fields of slurry nitrogen preparation, and discloses a continuous slurry nitrogen preparation machine, which comprises a workbench, one side of the top of the workbench is provided with a Stirling refrigerator, the middle of the top of the workbench is provided with a vacuumizing mechanism, the other side of the top of the workbench is provided with a vacuum insulation barrel mechanism, and the bottom of the vacuum insulation barrel mechanism is provided with an air pipe catheter mechanism connected with the vacuumizing mechanism; the two groups of vacuum barrels are communicated with the vacuumizing mechanism through the air pipe catheter mechanism, and the opening and closing of the control valve B and the control valve A on the outer sides of the air pipe A and the air pipe B are matched, so that the two groups of vacuum barrels are alternately controlled to be vacuumized, and when one group of vacuum barrels is used for the cryopreservation of biological samples, the other group is in standby state, and the alternating cooperation of the two groups of vacuum barrels improves the cryopreservation efficiency of the biological samples and reduces the waiting time.
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Description

Technical Field

[0001] This invention relates to the field of slurry nitrogen preparation technology, specifically a continuous slurry nitrogen preparation machine. Background Technology

[0002] Liquid nitrogen, with a temperature of -196℃, is widely used for the freezing and preservation of biological samples such as eggs, embryos, umbilical cord blood, and cells. Biological sample freezing is divided into programmed freezing and vitrification freezing. Vitrification freezing uses a high concentration of cryoprotectant to treat the sample. A small volume of sample is quickly placed into liquid nitrogen, and its cooling rate is higher than the vitrification temperature, thus forming a glass-like state without ice crystals. This does not cause intracellular ice damage to cells and improves the survival rate of the sample.

[0003] The key to vitrification freezing is a high concentration of protective agent and a fast cooling rate. Since high-concentration protective agents have solvent toxicity, the concentration cannot be increased indefinitely. The cooling rate can be increased by changing the temperature difference, which can be achieved by lowering the liquid nitrogen temperature. By appropriately reducing the vapor pressure on the surface of liquid nitrogen, slurry liquid nitrogen can be produced, with a temperature of around -210°C. The generally accepted method for producing slurry liquid nitrogen is to place liquid nitrogen in a sealed container, evacuate it, and when the vacuum reaches a certain level and the temperature reaches -210°C, the vacuum is released, the container lid is opened, and the liquid nitrogen is obtained. However, in the existing process of preparing slurry liquid nitrogen, vacuuming is required every time, and the liquid nitrogen quickly returns to room temperature, resulting in low efficiency and long time consumption. Therefore, a continuous slurry nitrogen preparation machine is needed. Summary of the Invention

[0004] The purpose of this invention is to provide a continuous slurry nitrogen preparation machine to solve the problems mentioned in the background art, such as the long cycle of existing slurry nitrogen preparation machines, which cannot meet the requirements for continuous biological sample preservation.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a workbench is included, a Stirling refrigerator is provided on one side of the top of the workbench, a vacuum pumping mechanism is provided in the middle of the top of the workbench, a vacuum insulation barrel mechanism is provided on the other side of the top of the workbench, and a gas pipe conduit mechanism connected to the vacuum pumping mechanism is provided at the bottom of the vacuum insulation barrel mechanism.

[0006] Preferably, the vacuuming mechanism includes a condensation chamber located at the top center of the workbench, an exhaust pipe at the top of the condensation chamber, condensation plates evenly distributed on the four sides of the top of the inner wall of the condensation chamber, a vacuum pump connected to the exhaust pipe at one end of the back of the condensation chamber, and a cold-end heat exchanger extending into the condensation chamber at the output end of the Stirling refrigerator. By providing the vacuuming mechanism, the vacuuming function inside the vacuum insulation barrel mechanism is realized.

[0007] Preferably, the vacuum insulation barrel mechanism includes two sets of vacuum barrels disposed at both ends of one side of the workbench. A support assembly is provided at the bottom inside the vacuum barrel. An inner insulation barrel is fitted inside the vacuum barrel, with its bottom fitting against the top of the support assembly. Overflow holes are evenly distributed on the top of the outer wall of the inner insulation barrel. A thermocouple is disposed on the top of the outer side of the vacuum barrel, with its detection end extending into the vacuum barrel and into the inner insulation barrel through the overflow holes. An opening is provided at the center of the top of the inner insulation barrel. A hanging groove is provided near the opening on the top of the inner insulation barrel. Hanging slots communicating with the opening are evenly distributed inside the hanging groove. A sealing groove is provided on the top of the inner insulation barrel outside the hanging groove. A lid is provided on the top of the vacuum barrel, with a sealing ring adapted to the sealing groove on the inner side of the bottom of the lid. By using two sets of vacuum barrels, the function of alternately and cyclically preparing slurry liquid nitrogen is achieved, improving the efficiency of biological sample freezing.

[0008] Preferably, the support assembly includes an airflow duct disposed in the middle of the bottom of the vacuum barrel. The top of the airflow duct extends into the interior of the vacuum barrel and is provided with a support plate. Support frames are uniformly arranged on the outer side of the support plate, and support legs connected to the bottom of the support frames are provided at the bottom of the support frames. Airflow holes are uniformly arranged on the outer side of the top of the airflow duct located inside the vacuum barrel, and sealing rings that fit against the vacuum barrel are uniformly arranged on the outer side of the airflow duct. By providing the support assembly, the inner insulation barrel is supported, and the gas inside the vacuum barrel and nitrogen molecules overflowing through the overflow holes can be discharged through the airflow duct.

[0009] Preferably, the endotracheal conduit mechanism includes a suction pipe A and a suction pipe B symmetrically arranged at both ends of the bottom of the workbench and interconnected with two sets of airflow conduits. Control valves B and A are respectively arranged on the outer sides of suction pipes A and B. Inlet pipes A and B are symmetrically arranged on the outer sides of suction pipes A and B that are close to each other. Control valve C is arranged on the outer side of inlet pipe A, and control valve D is arranged on the outer side of inlet pipe B. The ends of suction pipes A and B away from the airflow conduits extend into the interior of the condensation chamber. By setting the endotracheal conduit mechanism, the gas inside the vacuum tank can be transported, and the vacuuming and repressurization inside the vacuum tank can be controlled.

[0010] Preferably, the diameter of the top of the inner insulation bucket is larger than the diameter of its bottom, and the outer side of the top of the inner insulation bucket is in close contact with the inner wall of the vacuum bucket. The inner side of the bottom of the bucket lid is in close contact with the top of the inner insulation bucket, and a sealing structure is provided between the edge of the bottom of the bucket lid and the edge of the top of the vacuum bucket. By the outer top of the inner insulation bucket being in close contact with the inside of the vacuum bucket, a sealing structure is formed between the top of the inner insulation bucket and the vacuum bucket.

[0011] Compared with the prior art, the present invention provides a continuous slurry nitrogen preparation machine, which has the following beneficial effects:

[0012] 1. This invention features two sets of vacuum chambers connected to a vacuum pumping mechanism via endotracheal tubes. By controlling the opening and closing of control valves B and A on the outer sides of the suction pipes A and B, the vacuum pumping of the two sets of vacuum chambers is alternately controlled. Thus, when one set of vacuum chambers is used for cryopreservation of biological samples, the other set is in standby mode. This alternating operation of the two sets of vacuum chambers improves the freezing efficiency of biological sample preservation and reduces waiting time.

[0013] 2. This invention utilizes a condensation chamber to collect nitrogen molecules that overflow from the vacuum chamber extracted by the vacuum mechanism. The cold end of the Stirling refrigerator is located inside the condensation chamber, thereby capturing and cooling the nitrogen molecules. This reduces the instability inside the condensation chamber, allowing the nitrogen molecules to condense on the surface of the condensation plate and the cold end heat exchanger, thus improving the vacuum efficiency. Attached Figure Description

[0014] Figure 1 This is a schematic diagram of the main structure of the present invention. Figure 1 ;

[0015] Figure 2 This is a schematic diagram of the main structure of the present invention. Figure 2 ;

[0016] Figure 3 This is an enlarged cross-sectional view of the vacuum mechanism in this invention;

[0017] Figure 4 This is an enlarged cross-sectional view of the structure of the vacuum insulation barrel mechanism in this invention;

[0018] Figure 5 This is an enlarged cross-sectional view of the structure of the inner insulation barrel in this invention;

[0019] Figure 6 For the present invention Figure 5 Enlarged schematic diagram of the structure at point A;

[0020] Figure 7 This is an enlarged cross-sectional view of the structure at the bucket lid in this invention;

[0021] Figure 8 This is an enlarged cross-sectional view of the structure at the support component in this invention;

[0022] Figure 9 This is an enlarged cross-sectional view of the endotracheal tube mechanism in this invention.

[0023] In the diagram: 1. Workbench; 2. Stirling refrigerator; 3. Vacuum pump; 4. Exhaust pipe; 5. Bucket lid; 6. Thermocouple; 7. Vacuum bucket; 8. Evacuation pipe A; 9. Condensation chamber; 10. Evacuation pipe B; 11. Control valve A; 12. Cold end heat exchanger; 13. Condensation plate; 14. Overflow hole; 15. Airflow duct; 16. Inner insulation bucket; 17. Support frame; 18. Hanging groove; 19. Suspension groove; 20. Sealing groove; 21. Sealing ring; 22. Support plate; 23. Airflow hole; 24. Sealing ring; 25. Control valve B; 26. Control valve C; 27. Inlet pipe A; 28. Inlet pipe B; 29. ​​Control valve D. Detailed Implementation

[0024] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0025] Example 1:

[0026] Please see Figure 1-9 The present invention provides a technical solution: a continuous slurry nitrogen preparation machine, including a workbench 1, a Stirling refrigerator 2 is provided on one side of the top of the workbench 1, a vacuum pumping mechanism is provided in the middle of the top of the workbench 1, a vacuum insulation barrel mechanism is provided on the other side of the top of the workbench 1, and a gas pipe conduit mechanism connected to the vacuum pumping mechanism is provided at the bottom of the vacuum insulation barrel mechanism.

[0027] As a preferred embodiment, the vacuuming mechanism includes a condensation chamber 9 located at the top center of the workbench 1. An exhaust pipe 4 is provided on the top of the condensation chamber 9. Condensation plates 13 are evenly distributed on the four sides of the top of the inner wall of the condensation chamber 9. A vacuum pump 3 connected to the output end of the exhaust pipe 4 is provided at one end of the back of the condensation chamber 9. A cold end heat exchanger 12 extending into the condensation chamber 9 is provided at the output end of the Stirling refrigerator 2. By providing the vacuuming mechanism, the vacuuming function inside the vacuum insulation barrel mechanism is realized.

[0028] As a preferred embodiment: the vacuum insulation barrel mechanism includes two sets of vacuum barrels 7 disposed at both ends of one side of the workbench 1. A support assembly is provided at the bottom inside the vacuum barrel 7. An inner insulation barrel 16 is fitted inside the vacuum barrel 7, with the bottom of the inner insulation barrel 16 fitting against the top of the support assembly. Overflow holes 14 are evenly distributed on the top of the outer wall of the inner insulation barrel 16. A thermocouple 6 is disposed on the top of the outer side of the vacuum barrel 7, with the detection end of the thermocouple 6 extending into the interior of the vacuum barrel 7 and penetrating into the interior of the inner insulation barrel 16 through the overflow holes 14. The inner insulated container 16 has a bucket opening at the top center. A hanging groove 19 is provided near the bucket opening at the top of the inner insulated container 16. Hanging slots 18 that communicate with the bucket opening are evenly arranged inside the hanging groove 19. A sealing groove 20 is provided on the outside of the hanging groove 19 at the top of the inner insulated container 16. A lid 5 is provided on the top of the vacuum container 7. A sealing ring 21 that matches the sealing groove 20 is provided on the inner side of the bottom of the lid 5. By setting up two sets of vacuum containers 7, the function of alternately and cyclically preparing slurry liquid nitrogen is realized, which improves the efficiency of biological sample freezing.

[0029] As a preferred embodiment, the support assembly includes an airflow duct 15 disposed at the center of the bottom of the vacuum barrel 7. The top of the airflow duct 15 extends into the interior of the vacuum barrel 7 and is provided with a support plate 22. Support frames 17 are uniformly disposed on the outer side of the support plate 22, and support legs connected to the bottom of the support frame 17 are provided at the bottom. Airflow holes 23 are uniformly disposed on the outer side of the top of the airflow duct 15 located inside the vacuum barrel 7, and sealing rings 24 that fit together with the vacuum barrel 7 are uniformly disposed on the outer side of the airflow duct 15. By providing the support assembly, the inner insulation barrel 16 is supported, and the gas inside the vacuum barrel 7 and the nitrogen molecules overflowing through the overflow hole 14 can be discharged through the airflow duct 15.

[0030] As a preferred embodiment, the endotracheal tube mechanism includes a suction pipe A8 and a suction pipe B10 symmetrically arranged at both ends of the bottom of the workbench 1 and interconnected with two sets of airflow ducts 15. Control valves B25 and A11 are respectively arranged on the outer side of suction pipes A8 and B10. Inlet pipes A27 and B28 are symmetrically arranged on the outer side of suction pipes A8 and B10 that are close to each other. Control valve C26 is arranged on the outer side of inlet pipe A27, and control valve D29 is arranged on the outer side of inlet pipe B28. The ends of suction pipes A8 and B10 away from the airflow ducts 15 extend into the interior of the condensation chamber 9. By setting the endotracheal tube mechanism, the gas inside the vacuum tank 7 is transported, and the vacuuming and repressurization inside the vacuum tank 7 are controlled.

[0031] In a preferred embodiment, the diameter of the top of the inner insulation bucket 16 is larger than the diameter of its bottom, and the outer side of the top of the inner insulation bucket 16 is in close contact with the inner wall of the vacuum bucket 7. The inner side of the bottom of the bucket lid 5 is in close contact with the top of the inner insulation bucket 16, and a sealing structure is provided between the bottom edge of the bucket lid 5 and the top edge of the vacuum bucket 7. By the outer top of the inner insulation bucket 16 being in close contact with the inside of the vacuum bucket 7, a sealing structure is formed between the top of the inner insulation bucket 16 and the vacuum bucket 7.

[0032] like Figure 1-9 As shown, during the preparation of slurry nitrogen, liquid nitrogen is first added to the interiors of the two sets of inner insulated tanks 16, then the tank lids 5 are closed. The Stirling refrigerator 2 and vacuum pump 3 are then turned on. The vacuum pump 3 draws airflow from the interior of the condensation chamber 9, which is then transported through the suction pipes A8 and B10. At this time, control valves A11 and B25 are opened while control valves C26 and D29 are closed simultaneously. This allows the airflow inside the vacuum tank 7 and the overflowing nitrogen molecules to enter the airflow duct 15 through the airflow hole 23 at the top of the airflow duct 15, and further transported to the interior of the condensation chamber 9 through the suction pipes A8 and B10. At this time, the cold end heat exchanger 12 is activated. The heat causes the internal temperature of the condensation chamber 9 to decrease, which in turn causes the air and nitrogen molecules inside the condensation chamber 9 to condense. The condensed air and nitrogen molecules condense on the surface of the cold end heat exchanger 12 and the condensation plate 13, thereby reducing the air content inside the vacuum barrel 7, the evacuation pipe A8, the evacuation pipe B10 and the condensation chamber 9, and thus increasing the vacuum degree. At this time, by evacuating the vacuum, the air inside the inner insulation barrel 16 and the overflowing nitrogen molecules enter the interior of the vacuum barrel 7 through the overflow hole 14, thereby reducing the temperature of the liquid nitrogen inside the inner insulation barrel 16. By reducing the temperature inside the inner insulation barrel 16 and observing it through the thermocouple 6, the preparation of slurry liquid nitrogen is achieved when the temperature drops to -210℃.

[0033] When freezing biological samples, by closing the suction pipe A8 or B10, and then opening control valve C26 or D29, the internal pressure of one set of vacuum chambers 7 is restored. Once the internal pressure of this set of vacuum chambers 7 stabilizes, the lid 5 is opened, and the biological sample to be frozen is placed inside the inner insulated chamber 16. The sample placement rack is positioned and supported by the hanging groove 18 and suspension recess 19. Meanwhile, the other set of vacuum chambers 7 is in standby mode. When the temperature inside this set of vacuum chambers 7 rises, causing the inner insulated chamber to... When the liquid nitrogen inside the warming tank 16 returns to room temperature, the lid 5 of that group of tanks is closed and the lid 5 of the top of another group of vacuum tanks 7 is opened for replacement. At the same time, control valve C26 or control valve D29 is closed and evacuation pipe A8 or evacuation pipe B10 is opened, so that the used vacuum tank 7 is connected to the interior of the condensation chamber 9 again. The air inside the vacuum tank 7 is then extracted again by the vacuum pump 3, thereby realizing the function of alternating and cyclical use, which improves the freezing efficiency of biological samples and optimizes the problem of long waiting time for freezing biological samples.

[0034] Working principle: Two sets of vacuum tanks 7 are connected to the condensation chamber 9 via suction pipes A8 and B10. A vacuum pump 3 evacuates the interior of the condensation chamber 9, causing the airflow inside the vacuum tanks 7, suction pipes A8 and B10 to collect and discharge through the condensation chamber 9. By alternately opening and closing control valves B25, A11, C26, and D29, the evacuation and repressurization of the two sets of vacuum tanks 7 are controlled. An endothermic reaction occurs at the cold end heat exchanger 12 at one end of the Stirling refrigerator 2, allowing air and nitrogen molecules inside the condensation chamber 9 to condense on the surfaces of the cold end heat exchanger 12 and the condensation plate 13, thus improving the vacuum level. The alternating use of the two sets of vacuum tanks 7 reduces the waiting time for freezing biological samples and improves sample manufacturing efficiency.

[0035] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.

Claims

1. A continuous slurry nitrogen preparation machine, comprising a worktable (1), characterized in that: A Stirling refrigerator (2) is provided on one side of the top of the workbench (1), a vacuum pumping mechanism is provided in the middle of the top of the workbench (1), a vacuum insulation barrel mechanism is provided on the other side of the top of the workbench (1), and a gas pipe duct mechanism connected to the vacuum pumping mechanism is provided at the bottom of the vacuum insulation barrel mechanism. The vacuum mechanism includes a condensing chamber (9) located at the top center of the workbench (1), an exhaust pipe (4) located at the top of the condensing chamber (9), condensation plates (13) evenly arranged on the top four sides of the inner wall of the condensing chamber (9), a vacuum pump (3) connected to the output end of the exhaust pipe (4) located at one end of the back of the condensing chamber (9), and a cold end heat exchanger (12) extending into the condensing chamber (9) located at the output end of the Stirling refrigerator (2). The vacuum insulation barrel mechanism includes two sets of vacuum barrels (7) located at both ends of one side of the workbench (1). A support assembly is provided at the bottom of the vacuum barrel (7). An inner insulation barrel (16) is fitted inside the vacuum barrel (7), and the bottom of the inner insulation barrel (16) is in contact with the top of the support assembly. An overflow hole (14) is evenly provided on the top of the outer wall of the inner insulation barrel (16). A thermocouple (6) is provided on the top of the outer side of the vacuum barrel (7). The detection end of the thermocouple (6) extends into the interior of the vacuum barrel (7) and extends into the vacuum barrel (7) through the overflow hole (14). Inside the inner heat-insulating barrel (16), a barrel opening is provided at the middle of the top of the inner heat-insulating barrel (16), a hanging groove (19) is provided at the top of the inner heat-insulating barrel (16) near the barrel opening, and hanging grooves (18) that communicate with the barrel opening are evenly provided inside the hanging groove (19). A sealing groove (20) is provided on the outside of the hanging groove (19) at the top of the inner heat-insulating barrel (16). A barrel cover (5) is provided on the top of the vacuum barrel (7), and a sealing ring (21) that matches the sealing groove (20) is provided on the inner side of the bottom of the barrel cover (5). The support assembly includes an airflow duct (15) disposed in the middle of the bottom of the vacuum barrel (7). The top of the airflow duct (15) extends into the interior of the vacuum barrel (7) and is provided with a support plate (22). Support frames (17) are uniformly disposed on the outer side of the support plate (22), and support legs connected to the bottom of the support frame (17) are provided at the bottom. Airflow holes (23) are uniformly disposed on the outer side of the top of the airflow duct (15) inside the vacuum barrel (7), and sealing rings (24) that fit together with the vacuum barrel (7) are uniformly disposed on the outer side of the airflow duct (15). The tracheal conduit mechanism includes a suction pipe A (8) and a suction pipe B (10) symmetrically arranged at both ends of the bottom of the workbench (1) and connected to two sets of airflow conduits (15). Control valves B (25) and A (11) are respectively arranged on the outside of the suction pipe A (8) and the suction pipe B (10). Inlet pipes A (27) and B (28) are symmetrically arranged on the side of the suction pipes A (8) and the suction pipe B (10) that are close to each other. Control valve C (26) is arranged on the outside of the intake pipe A (27) and control valve D (29) is arranged on the outside of the intake pipe B (28). The end of the suction pipe A (8) and the suction pipe B (10) away from the airflow conduit (15) extends into the interior of the condensation chamber (9).

2. The continuous slurry nitrogen preparation machine according to claim 1, characterized in that: The diameter of the top of the inner heat-insulating barrel (16) is larger than the diameter of its bottom, and the outer side of the top of the inner heat-insulating barrel (16) is in contact with the inner wall of the vacuum barrel (7). The inner side of the bottom of the barrel cover (5) is in contact with the top of the inner heat-insulating barrel (16), and a sealing structure is provided between the edge of the bottom of the barrel cover (5) and the edge of the top of the vacuum barrel (7).

Citation Information

Patent Citations

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    CN114798125A

  • Vacuumizing equipment

    CN217531820U