A steady-state liquid nitrogen slurry preparation and sample quick-freezing integrated device

Abstract

The utility model provides a steady state liquid nitrogen mud preparation and sample quick freezing integrated device, including bucket body, ball valve, sample rod, acrylic sample sample channel cylinder and quick detach assembly, the below of acrylic sample sample channel cylinder is fixed with the second magnetic seal ring that is opposite with first magnetic seal ring magnetism, quick detach assembly includes rectangular block, L type round bar and U type board, the top of rectangular block is equipped with L type groove, L type round bar horizontal end fixed sleeve has the support ring, the right side fixed sleeve of support ring has the second spring of the outside of L type round bar horizontal end, U type board and L type round bar horizontal end sliding sleeve, the left side fixed sleeve of second spring and U type board, the upper end fixed sleeve of sample rod has the support piece The utility model discloses rational in structure, is convenient for real -time compensation pressure difference, controls vacuum flow rate, makes the pressure in the closed space can steady maintain, and after sample quick freezing, through sample stage on sample rod and liquid nitrogen cup in base clamping groove can fast drop, is convenient for to sample and disassembly preservation.

Description

Technical Field

[0001] This invention relates to an integrated device for the preparation of steady-state liquid nitrogen mud and rapid freezing of samples, belonging to the technical field of integrated devices for the preparation of steady-state liquid nitrogen mud and rapid freezing of samples. Background Technology

[0002] Cryotherapy typically uses liquid nitrogen as a coolant to freeze and fix the solvent. The key is to avoid damaging the sample structure during the freezing process. If the sample is directly immersed in liquid nitrogen, due to the Leidenfrost effect (the phenomenon where a liquid does not wet a hot surface but only forms a vapor layer on it), the liquid nitrogen surrounding the sample will immediately boil, encasing the sample in an adiabatic nitrogen atmosphere. This prevents the sample from cooling down immediately, causing water to crystallize. The expansion during water crystallization damages the sample's microstructure, such as disrupting the network structure formed by gel molecules or causing droplets in emulsions to burst.

[0003] Patent No. CN107991330B discloses an apparatus and method for preparing liquid nitrogen mud frozen samples. The method involves using a sample introduction device to fix the sample and deliver it into a liquid nitrogen mud cooling device. A vacuum pump is used to place the sample introduction device and the liquid nitrogen mud cooling device under vacuum. Liquid nitrogen in the liquid nitrogen mud cooling device, under vacuum, transforms into liquid nitrogen mud. The sample is then inserted into the liquid nitrogen mud to obtain a rapidly frozen liquid nitrogen mud sample. The frozen samples prepared using the apparatus and method of this invention have the advantages of rapid cooling, prevention of ice crystal formation, and preservation of the microstructure. However, during the liquid nitrogen mud preparation process, when liquid nitrogen is evacuated to 850 mbar in a sealed space, it transforms into liquid nitrogen mud. Since the process of liquid nitrogen forming into mud requires continuous vacuuming, and the liquid state is immediately restored upon evacuation, while the vacuum pump continues to run, the liquid nitrogen in the sealed space is constantly circulating. This causes the liquid nitrogen mud to quickly solidify into a solid ice state, making it difficult to maintain a stable liquid nitrogen mud state. Therefore, there is an urgent need for an integrated device for preparing stable liquid nitrogen mud and rapidly freezing samples to solve the aforementioned problems. Utility Model Content

[0004] To address the shortcomings of existing technologies, the purpose of this invention is to provide an integrated device for the preparation of steady-state liquid nitrogen sludge and rapid freezing of samples, thereby solving the problems mentioned in the background art. This invention has a reasonable structure, facilitates real-time compensation of pressure difference, and controls vacuum flow rate, so that the pressure in the sealed space can be maintained stably. Moreover, after the sample is rapidly frozen, it can be quickly detached from the sample stage on the sample rod and the base slot in the liquid nitrogen cup, making it easy to disassemble and store the sample. At the same time, a spring is added to the sample rod to reduce the suction force of negative pressure on the sample rod during experimental operations. After the sample is placed, it can automatically spring back to its original position, allowing for quick installation and disassembly. It is lightweight, easy to operate, and highly practical.

[0005] To achieve the above objectives, this utility model is implemented through the following technical solution: an integrated device for preparing steady-state liquid nitrogen mud and rapidly freezing samples, comprising a barrel, a ball valve, a sample inlet rod, an acrylic sample inlet channel cylinder, and a quick-release assembly. An acrylic plate is installed on the top of the barrel. A vacuum pump is installed on the rear side of the acrylic plate, communicating with the inside of the barrel, and a vacuum flow meter is connected to the upper end of the vacuum pump. A safety pressure relief valve is installed on the left side of the vacuum pump. A first magnetic sealing ring is installed on the upper end of the ball valve. A second magnetic sealing ring with opposite magnetic properties to the first magnetic sealing ring is fixedly connected to the lower part of the acrylic sample inlet channel cylinder. The quick-release assembly comprises a rectangular block, an L-shaped rod, and a U-shaped plate. An L-shaped groove is provided on the top of the rectangular block. A support ring is fixedly sleeved on the horizontal end of the L-shaped rod. A second spring is fixedly sleeved on the right side of the support ring and sleeved on the outside of the horizontal end of the L-shaped rod. The U-shaped plate is slidably sleeved with the horizontal end of the L-shaped rod. The second spring is fixedly connected to the left side of the U-shaped plate. A support plate is fixedly connected to the upper end of the sample inlet rod.

[0006] Furthermore, a second magnetic sheet is fixedly connected to the right side of the horizontal end of the L-shaped rod, and an L-shaped block is fixedly connected to the lower side of the vertical end of the L-shaped rod.

[0007] Furthermore, two first magnetic sheets with opposite magnetic properties to the second magnetic sheet are installed on the annular side of the ball valve, and two quick-release components are provided. The two rectangular blocks are fixed to the left and right sides of the ball valve, and the two U-shaped plates are fixed to the left and right sides of the acrylic sample inlet channel cylinder.

[0008] Furthermore, a first spring is fixedly connected to the lower end of the support plate and sleeved on the outside of the injection rod. The lower end of the first spring is fixedly connected to the ball valve, and a sample rod is fixedly connected to the lower end of the injection rod.

[0009] Furthermore, a liquid nitrogen cup is installed on the bottom surface of the barrel by screws, and a sample holder matching the sample rod is installed on the bottom of the liquid nitrogen cup by screws.

[0010] Furthermore, a liquid nitrogen delivery pipe is inserted and installed on the left side of the barrel, and a venting pipe is connected and installed on the right side of the barrel. A precision venting valve is installed at the right end of the venting pipe, and the input end of the precision venting valve is sealed and connected to the venting pipe.

[0011] The beneficial effects of this utility model: This utility model provides an integrated device for the preparation of steady-state liquid nitrogen mud and rapid freezing of samples. Because this utility model adds an acrylic plate, a safety pressure relief valve, a vacuum flow meter, a sample inlet rod, a first spring, a support plate, a ball valve, a liquid nitrogen delivery pipe, a liquid nitrogen cup, a sample holder, a first magnetic plate, a sample rod, a rectangular block, an L-shaped groove, an L-shaped block, an L-shaped round rod, a U-shaped plate, a support ring, a second spring, and a second magnetic plate, our design improvements and actual use show that this device has a reasonable structure, facilitates the control of vacuum flow rate, enables the pressure in the sealed space to be maintained stably, and facilitates the quick installation and disassembly of the sample inlet rod, making it highly practical. Attached Figure Description

[0012] Other features, objects, and advantages of this invention will become more apparent from the following detailed description of non-limiting embodiments with reference to the accompanying drawings: Figure 1 This is a three-dimensional schematic diagram of the overall structure of the integrated device for preparing steady-state liquid nitrogen mud and quick-freezing samples according to the present invention. Figure 2 This is a three-dimensional schematic diagram of the barrel structure of an integrated device for preparing steady-state liquid nitrogen mud and quick-freezing samples according to the present invention. Figure 3 This is a three-dimensional schematic diagram of the ball valve structure of the integrated device for preparing steady-state liquid nitrogen mud and quick-freezing samples according to the present invention; Figure 4 This is a three-dimensional schematic diagram of the acrylic plate structure of the integrated device for preparing steady-state liquid nitrogen mud and quick-freezing samples according to the present invention. Figure 5 This is a schematic cross-sectional view of the ball valve in the integrated device for preparing steady-state liquid nitrogen mud and quick-freezing samples according to this utility model.

[0013] In the diagram: 1-Barrel body, 2-Precision venting valve, 3-Venting pipe, 4-Acrylic plate, 5-Safety pressure relief valve, 6-Vacuum flow meter, 7-Injection rod, 8-First spring, 9-Support plate, 10-Ball valve, 11-First magnetic sealing ring, 12-Second magnetic sealing ring, 13-Acrylic sample injection channel cylinder, 14-Quick release assembly, 15-Liquid nitrogen delivery pipe, 16-Liquid nitrogen cup, 17-Sample holder, 18-First magnetic plate, 19-Sample rod, 20-Vacuum pump, 1401-Rectangular block, 1402-L-shaped groove, 1403-L-shaped block, 1404-L-shaped round rod, 1405-U-shaped plate, 1406-Supporting ring, 1407-Second spring, 1408-Second magnetic plate. Detailed Implementation

[0014] To make the technical means, creative features, objectives and effects of this utility model easier to understand, the present utility model will be further described below in conjunction with specific embodiments.

[0015] Please see Figures 1-5 This utility model provides a technical solution including a barrel body 1, a ball valve 10, a sample inlet rod 7, an acrylic sample inlet channel cylinder 13, and a quick-release assembly 14. An acrylic plate 4 is installed on the top of the barrel body 1. A vacuum pump 20 is installed on the upper rear side of the acrylic plate 4, communicating with the inside of the barrel body 1. A vacuum flow meter 6 is connected to the upper end of the vacuum pump 20. A safety pressure relief valve 5 is installed on the left side of the vacuum pump 20. A first magnetic sealing ring 11 is installed on the upper end of the ball valve 10. A second magnetic sealing ring 12 with opposite magnetic properties to the first magnetic sealing ring 11 is fixed below the acrylic sample inlet channel cylinder 13. The quick-release assembly 14 includes a rectangular block 1401, an L-shaped rod 1404, and a U-shaped plate 1405. An L-shaped groove 1402 is provided on the upper part of the rectangular block 1401. The L-shaped rod 1404 is horizontal. A support ring 1406 is fixedly sleeved at the end. A second spring 1407 is fixedly sleeved on the right side of the support ring 1406 and sleeved on the outside of the horizontal end of the L-shaped round rod 1404. A U-shaped plate 1405 is slidably sleeved with the horizontal end of the L-shaped round rod 1404. The second spring 1407 is fixedly sleeved on the left side of the U-shaped plate 1405. A support plate 9 is fixedly sleeved at the upper end of the injection rod 7. This design solves the problem in the original device that when liquid nitrogen is evacuated to 850 mbar in a closed space during the liquid nitrogen mud production process, the liquid nitrogen turns into liquid nitrogen mud. However, since the process of liquid nitrogen turning into mud requires continuous evacuation, it immediately returns to the liquid state when the evacuation stops. The vacuum flow meter is running continuously, and the liquid nitrogen in the closed space is constantly circulating. The liquid nitrogen mud quickly turns into solid ice and cannot maintain a stable state of liquid nitrogen mud.

[0016] As the first embodiment of this utility model: a second magnetic sheet 1408 is fixedly connected to the right side of the horizontal end of the L-shaped rod 1404, and an L-shaped block 1403 is fixedly connected to the lower side of the vertical end of the L-shaped rod 1404. The L-shaped block 1403 is set to facilitate engagement with the L-shaped groove 1402. Two first magnetic sheets 18 with opposite magnetic properties to the second magnetic sheet 1408 are installed on the annular side of the acrylic sample inlet channel cylinder 13. Two quick-release components 14 are provided. Two rectangular blocks 1401 are fixedly connected to the left and right sides of the ball valve 10, and two U-shaped plates 1405 are fixedly connected to the left and right sides of the acrylic sample inlet channel cylinder 13. The first magnetic sheets 18 are set to facilitate magnetic attraction with the second magnetic sheets 1408. A first spring 8, sleeved on the outside of the sample inlet rod 7, is fixedly connected to the lower end of the support plate 9. The lower end of the first spring 8 is fixedly connected to the acrylic sample inlet channel cylinder 13. A sample rod 19 is fixedly connected to the lower end of the sample inlet rod 7. The first spring 8 helps to reduce the pressure when injecting and withdrawing the sample rod. A liquid nitrogen cup 16 is installed on the bottom surface of the barrel 1 by screws. A sample holder 17 matching the sample rod 19 is installed on the bottom of the liquid nitrogen cup 16 by screws. The sample holder 17 facilitates sample placement. A liquid nitrogen delivery pipe 15 is inserted and installed on the left side of the barrel 1. A vent pipe 3 is connected and installed on the right side of the barrel 1. A precision vent valve 2 is installed on the right end of the vent pipe 3, and the input end of the precision vent valve 2 is sealed and connected to the vent pipe 3. Liquid nitrogen is introduced into the liquid nitrogen cup 16 through the liquid nitrogen delivery pipe 15 and an external nitrogen supply device.

[0017] As a second embodiment of this utility model: In use, liquid nitrogen is introduced into the liquid nitrogen cup 16 by cooperating with an external nitrogen supply device and the liquid nitrogen supply pipe 15. Then, the vacuum pump 20 is started to evacuate the container 1. When the vacuum negative pressure reaches 850 mbar, the liquid nitrogen is converted into liquid nitrogen slurry. By adjusting the precision venting valve 2, the pressure in the sealed space is maintained and stabilized at -850 mbar, and the vacuum flow rate is kept constant, so that the liquid nitrogen in the sealed vacuum state is converted into liquid nitrogen slurry and maintained in the state of liquid nitrogen slurry. Then, the sample is quickly fixed on the sample stage at the lower end of the sample rod 19. Then, the ball valve 10 is opened, and the sample inlet rod 7 is quickly inserted into the acrylic sample inlet channel cylinder 13, so that the sample is inserted into the clamp holder in the liquid nitrogen cup corresponding to the liquid nitrogen slurry. Quick-freeze for 30-60 seconds, reduce the vacuum to restore the liquid nitrogen to a liquid state, rotate the sample rod 19, and release the entire sample stage clamp onto the sample holder 17 in the liquid nitrogen cup. The sample holder 17 falls off and is stored in the bottom sample clamp. When it is necessary to disassemble the acrylic sample inlet channel cylinder 13, push the two L-shaped rods 1404 so that the two L-shaped rods 1404 respectively drive the two second magnetic pieces 1408 and the two first magnetic pieces 18 to approach each other. At this time, under the action of the U-shaped plate 1405 and the support ring 1406, the two second springs 1407 are squeezed. When the two second magnetic pieces 1408 and the two first magnetic pieces 18 are magnetically attracted, they can temporarily limit the two L-shaped rods 1404. Then the acrylic sample inlet channel cylinder 13 can be removed.

[0018] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. It will be apparent to those skilled in the art that this utility model is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or basic characteristics of this utility model. Therefore, the embodiments should be considered exemplary and non-limiting in all respects. The scope of this utility model is defined by the appended claims rather than the foregoing description, and thus all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this utility model. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0019] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A steady-state liquid nitrogen slurry preparation and sample quick-freezing integrated device, comprising a barrel (1), a ball valve (10), a sample feeding rod (7), an acrylic sample feeding channel cylinder (13) and a quick-release assembly (14), characterized in that: An acrylic plate (4) is installed on the top of the barrel (1). A vacuum pump (20) is installed on the rear side of the acrylic plate (4) and connected to the inside of the barrel (1). A vacuum flow meter (6) is connected to the upper end of the vacuum pump (20). A safety pressure relief valve (5) is installed on the left side of the vacuum pump (20). A first magnetic sealing ring (11) is installed on the upper end of the ball valve (10). A second magnetic sealing ring (12) with opposite magnetism to the first magnetic sealing ring (11) is fixed below the acrylic sample injection channel cylinder (13). The quick-release assembly (14) includes a rectangular block (1401), an L-shaped rod (1404), and a U-shaped plate (1405). An L-shaped groove (1402) is provided above the rectangular block (1401). A support ring (1406) is fixedly sleeved on the horizontal end of the L-shaped rod (1404). A second spring (1407) is fixedly sleeved on the right side of the support ring (1406) and sleeved on the outside of the horizontal end of the L-shaped rod (1404). The U-shaped plate (1405) is slidably sleeved on the horizontal end of the L-shaped rod (1404). The second spring (1407) is fixedly sleeved on the left side of the U-shaped plate (1405). A support piece (9) is fixedly sleeved on the upper end of the injection rod (7).

2. The device according to claim 1, wherein the device is characterized in that: A second magnetic sheet (1408) is fixed to the right side of the horizontal end of the L-shaped rod (1404), and an L-shaped block (1403) is fixed to the lower side of the vertical end of the L-shaped rod (1404).

3. The device according to claim 1, wherein the device is characterized by: The acrylic sample inlet channel cylinder (13) has two first magnetic sheets (18) with opposite magnetic properties to the second magnetic sheet (1408) installed on its annular side. The quick-release assembly (14) has two of them. The two rectangular blocks (1401) are fixed to the left and right sides of the ball valve (10), and the two U-shaped plates (1405) are fixed to the left and right sides of the acrylic sample inlet channel cylinder (13).

4. The device according to claim 1, wherein the device is characterized by: The lower end of the support plate (9) is fixedly connected to a first spring (8) sleeved on the outside of the injection rod (7). The lower end of the first spring (8) is fixedly connected to the acrylic sample injection channel cylinder (13). The lower end of the injection rod (7) is fixedly connected to a sample rod (19).

5. The device according to claim 1, wherein the device is characterized by: The bottom of the barrel (1) is fitted with a liquid nitrogen cup (16) by screws, and the bottom of the liquid nitrogen cup (16) is fitted with a sample holder (17) that matches the sample rod (19) by screws.

6. The apparatus according to claim 1, wherein the apparatus is characterized by: A liquid nitrogen delivery pipe (15) is inserted and installed on the left side of the barrel (1), and a venting pipe (3) is connected and installed on the right side of the barrel (1). A precision venting valve (2) is installed at the right end of the venting pipe (3), and the input end of the precision venting valve (2) is sealed and connected to the venting pipe (3).

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