CN220772682U - Constant state process adsorption device - Google Patents

Constant state process adsorption device Download PDF

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Publication number
CN220772682U
CN220772682U CN202321838237.8U CN202321838237U CN220772682U CN 220772682 U CN220772682 U CN 220772682U CN 202321838237 U CN202321838237 U CN 202321838237U CN 220772682 U CN220772682 U CN 220772682U
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sealing
module
adsorption
bin
temperature control
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赵尚清
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Jiangcheng Scientific Instrument Shanghai Co ltd
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Jiangcheng Scientific Instrument Shanghai Co ltd
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Abstract

The utility model relates to a constant-state process adsorption device in the technical field of analytical instruments, which comprises an adsorption module, an adsorption medium temperature control assembly, a sealing module, a temperature control module and a sealing module, wherein the adsorption module is connected with the sealing module; the sealing module is connected with the adsorption module, and the temperature control module is arranged in the sealing module or the adsorption module; the sealing module comprises a first sealing bin and/or a second sealing bin; the first sealing bin is arranged in the second sealing bin or connected with the second sealing bin; when the temperature control module is arranged in the adsorption module, the temperature control module and the sealing module are provided with communication ports, and the adsorption medium temperature control assembly is arranged in the second sealing bin or below the first sealing bin. According to the utility model, the sealing module is combined with the internal temperature control module, so that the external environment where the sample tube is positioned is basically unchanged when the first free space is tested, the accuracy and stability of the test of the first free space are ensured, and a foundation is laid for accurate calculation of the effective free space.

Description

Constant state process adsorption device
Technical Field
The utility model relates to the technical field of analytical instruments, in particular to a constant-state process adsorption device.
Background
With the rapid development of material science such as nano materials, energy storage materials, catalytic materials and the like, physical adsorption technology is widely applied to analysis of specific surface area, pore size distribution, adsorption performance, separation effect and the like of solid materials, and nitrogen, argon and the like are common analysis gases. In order to control the adsorption process to be carried out step by step, the sample needs to be maintained at the phase inversion temperature of the corresponding analysis gas, for example, when nitrogen is the analysis gas, the sample needs to be soaked in liquid nitrogen, when argon is the analysis gas, the sample needs to be soaked in liquid argon, the pressure is continuously increased or reduced in the whole analysis process, after the adsorption equilibrium state is reached, the adsorption quantity of the sample at constant temperature and different partial pressures is calculated according to a gas equation, and an isotherm is obtained. And then, analyzing the isotherm by adopting different analysis models to obtain the information of the specific surface area, the pore size distribution, the pore volume and the like of the sample. Of course, in addition to the above analysis gases, studies on adsorption performance of various vapors have been receiving increasing attention, particularly VOC studies, such as water vapor adsorption, benzene vapor adsorption, etc., and such adsorption analysis tends to focus on adsorption amounts at different analysis temperatures.
Physical adsorption, unlike chemisorption, is a nonselective weak adsorption, requiring a longer time for equilibrium to be reached at each partial pressure, whereas isotherms often require data acquisition at multiple partial pressures. The more data are collected, the more accurate the subsequent analysis results are, and the longer the time consumption is. In addition, a large amount of manual operation exists in the operation, so that the time consumption is low, and the operation has a plurality of problems. Often, the sample tube is required to be mounted by a user by screwing the sample tube by hand or by means of a tool such as a wrench or a screwdriver, so that the tightness of the sealed sample tube is extremely difficult to control, the sample tube orifice is easily crushed by over tightening, and air leakage is easily caused by over loosening. Once the gas leaks, the whole analysis process is partly spent, so the need for automated operation is well appreciated.
After the sample tube is connected to the host, firstly testing the sample tube loaded with the sample at normal temperature to obtain a volume which is a first free space; the volume measured at the test temperature (usually low temperature) is the second free space, and the sample tube is partially immersed under the low-temperature liquid (such as liquid nitrogen and liquid argon) and partially above the low-temperature liquid, and can be a non-low-temperature liquid. When the adsorption amount of the sample is calculated, the effective free space of the sample tube needs to be known, and the effective free space is calculated through the first free space and the second free space. Because the analysis process is longer, and the low-temperature liquid in the low-temperature storage device can be gradually volatilized, the liquid level is continuously lowered, so that the second free space is continuously changed, and further, the change of the effective free space is also caused, and thus, a lot of uncertainties are brought to the calculation of the adsorption quantity. In addition, when the first free space and the second free space are tested, the upper ends of the instrument host and the sample tube are at room temperature, but the room temperature also changes along with the day and night, the four seasons change, the instrument placement position and other factors continuously change, and the instrument placement position is interwoven with the low-temperature liquid level change, so that the first free space and the second free space also change at any time, and the repeatability and the accuracy of the test are affected.
For the problem of the influence of the liquid level change on the second free space, the existing main technologies include a porous material method, a liquid level constant method and the like, which have attracted attention, but the measurement of the first free space often assumes that the temperature of the first free space is approximately equal to the temperature of a system, and the actual situation often has larger difference. In addition, the environment of the sample tube is constantly changed in the whole analysis process, such as temperature, humidity, pressure and the like, and even if the liquid level is constant, the change of the environment can influence the test result: the change of the external pressure can lead to the change of saturated vapor pressure; the increase of the humidity can cause ice particles in the low-temperature liquid to influence the purity of the low-temperature liquid, so that the saturated vapor pressure is increased; too much humidity can cause a large amount of ice to form on the sample tube or the dewar bottle mouth, so that safety accidents are easy to occur, a vacuum system, the dewar bottle and the sample tube are damaged, and a second free space is changed; the change in temperature at which the sample tube is subjected to each test also affects the first free space, etc. That is, the whole analysis process includes the installation of the sample tube, the testing of the first free space and the second free space, and the like, and the change of external factors affects the testing result. In order to obtain high accuracy and high reproducibility results, it is necessary to control the same test steps throughout the analysis process, keeping the state constant.
Disclosure of Invention
In order to solve the technical problems that in the prior art, the first free space measurement data is inaccurate and the second free space is not constant and changes due to the change of external factors, so that the subsequent measurement result is influenced, the utility model discloses a constant state process adsorption device, and the technical scheme of the utility model is realized in the following way:
the constant-state process adsorption device comprises an adsorption module, an adsorption medium temperature control assembly, a sealing module, a temperature control module and a sealing module, wherein the adsorption module is connected with the sealing module;
the sealing module is connected with the adsorption module, and the temperature control module is arranged in the sealing module or the adsorption module;
the sealing module comprises a first sealing bin and/or a second sealing bin;
the first sealing bin is arranged in the second sealing bin or is connected with the second sealing bin;
when the temperature control module is arranged in the adsorption module, the temperature control module and the sealing module are provided with a communication port.
The adsorption medium temperature control component is arranged in the second sealed bin or below the first sealed bin.
Preferably, the sealing module comprises a power generator, an auxiliary structure and a test head;
The power device is connected with the auxiliary structure or the test head;
a cavity is formed in the test head, and a connector is arranged at one end of the test head;
a sealing element is assembled in the cavity;
the auxiliary structure comprises an adjusting block;
the adjusting block is provided with a protruding structure corresponding to the sealing piece;
the raised structure is inserted into the cavity.
Preferably, the automatic grabbing module is further included; the automatic grabbing module comprises a fixed arm, a movable arm and a grabbing head; the movable arm is movably arranged on the fixed arm, and the grabbing head is arranged at the end part of the movable arm.
Preferably, the second seal cartridge is provided with a vent passage.
Preferably, a dehumidifying device and/or a humidity sensor are/is arranged in the second sealed bin.
Preferably, the adsorption medium temperature control assembly comprises a circulating Dewar, a first sealing ring of a circulating device, a first sealing cover, a second sealing ring of the circulating device and a second sealing cover;
the bottom of the circulating Dewar is provided with an inlet and an outlet; the circulation Du Wading part is provided with a first annular groove; the upper surface of the first sealing cover is provided with a second annular groove; the first sealing ring of the circulating device is arranged in the first annular groove, and the second sealing ring of the circulating device is arranged in the second annular groove.
Preferably, a power push rod is mounted on the upper surface of the circulating Dewar, and the power push rod is connected with the first sealing cover.
Preferably, the second seal cartridge further comprises an automatic seal door; the automatic sealing door comprises a sliding frame, a sealing window, a power sliding rod, a sealing window and a thruster;
the sealing window is fixed on the inner side of the sliding frame through the thruster, and the sliding frame is slidably arranged on the power sliding rod; the sealing window is embedded with a sealing strip.
Preferably, the temperature control module is arranged in the first sealed bin;
the first sealed bin comprises a sliding rail, a first bin body and a second bin body;
the first bin body and the second bin body are slidably connected with the sliding rail.
Preferably, an exhaust valve is arranged on the exhaust channel; a first pressure sensor is arranged in the second sealing bin;
the adsorption module comprises a standard pipe, a first pressure sensor, an air inlet pipe, an air inlet valve, an exhaust pipe, an exhaust valve, a connecting pipe and a connecting valve;
the standard tube is connected with the first pressure sensor, one end of the air inlet tube, one end of the air exhaust tube and one end of the connecting tube, the other end of the connecting tube is connected with the sealing module, the air inlet valve is arranged on the air inlet tube, the air exhaust valve is arranged on the air exhaust tube, and the connecting valve is arranged on the connecting tube.
According to the utility model, the sealing bin is combined with the automatic temperature control module, so that the outside temperature of the sample tube is kept unchanged when the first free space is measured, the measurement value of the first free space is more accurate, and the accuracy of the adsorption test result is indirectly improved. Meanwhile, the utility model combines the patent with the patent number ZL202222684016.1, an automatic sealing door capable of automatically opening, closing and sealing, a control system of the existing adsorption instrument host, and any commercially available mechanical arm, so that the automatic sealing of the sample tube or the unloading of the sample tube can be realized, and the external environment where the sample tube is positioned in the adsorption process is kept constant, such as temperature, humidity and pressure, the automatic sealing effect of the sample tube each time and the like are stable, thereby ensuring the accuracy and repeatability of the test result.
Drawings
In order to more clearly illustrate the embodiments of the present utility model or the technical solutions of the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only one embodiment of the present utility model, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an embodiment of a constant state process adsorption apparatus:
FIG. 2 is a schematic view of a first seal cartridge embodiment;
FIG. 3 is a schematic structural view of an embodiment of a seal module;
FIG. 4 is a structural exploded view of an embodiment of a seal module;
FIG. 5 is a schematic diagram of an embodiment of an auxiliary structure;
FIG. 6 is a cross-sectional view of an embodiment of a test head;
FIG. 7 is a schematic diagram of an embodiment of a conditioning block;
FIG. 8 is a schematic diagram of an embodiment of an adsorption media temperature control assembly;
FIG. 9 is a structural cross-sectional view of an embodiment of an adsorption media temperature control assembly;
FIG. 10 is a schematic diagram of another embodiment of an adsorption media temperature control assembly;
FIG. 11 is a cross-sectional view of another embodiment of an adsorption media temperature control assembly;
FIG. 12 is a schematic diagram of another embodiment of a constant state process adsorption device;
FIG. 13 is a schematic view of an embodiment of a self-sealing door (right power slide bar not shown, thrusters for the remaining three corners not shown);
FIG. 14 is a schematic block diagram of an embodiment of a self-sealing door for performing self-sealing;
FIG. 15 is a schematic diagram of another embodiment of a constant state process adsorption device;
FIG. 16 is a schematic view of another embodiment of a constant process adsorption device for testing a first free space (automatic gripping device not shown);
FIG. 17 is a schematic diagram of another embodiment of a constant process adsorption device for testing a first free space (automatic gripping device not shown);
FIG. 18 is a schematic diagram of another embodiment of a constant state process adsorption device;
FIG. 19 is a schematic view of another embodiment of a constant process adsorption device for testing a first free space (automatic gripping device not shown);
FIG. 20 is a schematic diagram of another embodiment of a constant process adsorption device for testing a second free space (automatic gripping device not shown);
FIG. 21 is a schematic diagram of another embodiment of a constant state process adsorption device;
FIG. 22 is a schematic diagram of another embodiment of a constant process adsorption device for testing a first free space (automatic gripping device not shown);
FIG. 23 is a cross-sectional view of another embodiment of a constant process adsorption device (automatic gripping device not shown) for testing a first free space;
FIG. 24 is a schematic view of another embodiment of a constant process adsorption device for testing a first free space (automatic gripping device not shown);
FIG. 25 is a cross-sectional view of another embodiment of a constant process adsorption device (automatic gripping device not shown) for testing a first free space;
Fig. 26 is a schematic structural view of an XY axis movement module embodiment.
In the above drawings, each reference numeral indicates:
1. a power device;
2. an auxiliary structure;
3. a test head;
3-1, cavity;
3-2, a connector;
3-3, chamfering
4. An adjusting block;
4-1, bump structure
5. Sample tube
6. Sealing ring
7. A bolt;
8. a standard tube;
9. an air inlet pipe;
10. an air inlet valve;
11. an exhaust pipe;
12. an air extraction valve;
13. a connecting pipe;
14. connecting a valve;
15. sealing the bin;
15-1, a first bin; 15-2, a second bin; 15-3, sliding rails;
16. a second sealed bin;
17. a fixed arm;
18. a moving arm;
19. a grabbing head;
20. an air circulation device;
21. a heating device;
22. a dehumidification module;
23. an exhaust pipe;
24. an exhaust valve;
25. a fluid circulation device;
26. circulating Dewar;
26-1, a water outlet; 26-2, a water inlet;
27. a first sealing ring of the circulating device;
28. a first sealing cover;
29. a second sealing ring of the circulating device;
30. a second sealing cover;
31. a sliding frame;
32. sealing the window;
33. a power slide bar;
34. sealing the window;
35. a thruster;
36. a sealing strip;
37. a power push rod;
38. A temperature control medium storage device;
39. an elevator;
40. an X-axis moving module;
41. a Y-axis moving module;
42. a motor;
43. a slide bar;
44. a fixed rod;
p1, a first pressure sensor;
p2, a second pressure sensor;
t1, a temperature sensor;
h, a humidity sensor;
Detailed Description
The technical solutions of the present utility model will be clearly and completely described below with reference to the embodiments of the present utility model and the accompanying drawings, and it is obvious that the described embodiments are only some embodiments of the present utility model, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the utility model without making any inventive effort, are intended to be within the scope of the utility model.
Examples
In a specific embodiment 1, as shown in fig. 1, a constant process adsorption device includes an adsorption module, a sealing module, a first sealing cabin 15, an automatic grabbing module, and a temperature control module; the first sealed cabin 15 is installed below the adsorption module and connected with the sealing module, and the temperature control module is installed in the first sealed cabin 15. The automatic gripping module is arranged outside the first sealed cabin 15. The automatic grabbing module comprises a fixed arm 17, a movable arm 18 and a grabbing head 19; the movable arm 18 is movably provided on the fixed arm 17, and the gripper 19 is provided at an end of the movable arm 18. The automatic grabbing module is used for grabbing the sample tube 5, then the sample tube 5 is placed in the sealing module, the power device 1 completes extrusion or pressure release of the sealing ring 6 through the up-and-down acting force, and the sample tube 5 is installed or detached. In this embodiment, the automatic grabbing module is a multi-axis robot with functions of grabbing and rotating the sample tube purchased in the market (in addition, the utility model does not propose a new automatic grabbing module, but any robot capable of realizing the same or similar functions in the market can be used as the automatic grabbing module for selection).
The adsorption module comprises a standard pipe 8, a first pressure sensor P1, an air inlet pipe 9, an air inlet valve 10, an air exhaust pipe 11, an air exhaust valve 12, a connecting pipe 13 and a connecting valve 14; the standard pipe 8 is connected with the first pressure sensor P1, one end of the air inlet pipe 9, one end of the air exhaust pipe 11 and one end of the connecting pipe 13, the other end of the connecting pipe 13 is connected with the sealing module, the air inlet valve 10 is arranged on the air inlet pipe 9, the air exhaust valve 12 is arranged on the air exhaust pipe 11, and the connecting valve 14 is arranged on the connecting pipe 13. The air inlet pipe 9 is connected with an external air source, and the air exhaust pipe 11 is connected with an external vacuumizing system. Adsorption modules are common prior art in the art.
As shown in fig. 2, the first sealed cabin 15 comprises a first cabin body 15-1/a second cabin body 15-2 and a sliding rail 15-3; the first bin body 15-1 and the second bin body 15-2 are slidably arranged on the lower side of the sliding rail 15-3; the first and second housings 15-1 and 15-2 are closed and then the internal cavity is sealed.
The first sealing cabin 15 is used for sealing the sample tube 5 when testing the first free space, so as to prevent the sample tube from being influenced by external environment changes, thereby causing larger errors of testing results, especially temperature changes. The temperature control module is used for maintaining the temperature in the first sealed cabin 15 constant. The temperature control module includes an air circulation device 20, a temperature sensor T1, and a heating device 21. The air circulation device 20 in this embodiment is a fan, and the heating device 21 is an air heating rod.
In this embodiment, the first bin 15-1 and the second bin 15-2 slide along the sliding rail 15-3, and the power may be an air cylinder, an electric cylinder, or a sliding table with a motor, so as to control the opening and closing of the first bin 15-1 and the second bin 15-2. In this embodiment, because of the existence of the first seal cabin 15 and the temperature control module, the ambient temperature around the sample tube 5 is unchanged in the whole process of testing the first free space, so that the accuracy and stability of the test of the first free space are ensured, and a foundation is laid for accurate calculation of the effective free space. After the first free space test is finished, the first bin body 15-1 and the second bin body 15-2 are separated, and temperature control is stopped.
As shown in fig. 3-7, the sealing module includes a power machine 1, an auxiliary structure 2, and a test head 3; the test head 3 is arranged inside the auxiliary structure 2; the power device 1 is connected with the auxiliary structure 2; the test head 3 is internally provided with a cavity 3-1, and one end of the test head 3 is provided with a connector 3-2; a sealing ring 6 is assembled in the cavity 3-1; the auxiliary structure 2 comprises an adjusting block 4; the adjusting block 4 is provided with a protruding structure 4-1 corresponding to the sealing ring 6; the protruding structure 4-1 is inserted into the cavity 3-1. The cavity 3-1 is provided with an inwardly converging chamfer 3-3. The adjusting block 4 forms a groove in the auxiliary structure 2; the test head 3 is positioned in the groove; the sealing ring 6 is fixed by the bulge structure 4-1 and the shrinkage chamfer 3-3; the auxiliary structure 2 is internally provided with a through hole for the sample tube 5 to pass through. The auxiliary structure 2 is connected with the power unit 1 by bolts 7.
In this embodiment, the power unit 1 is any power unit on the market that performs up-and-down motion.
The sample tube 5 is arranged in the through hole of the auxiliary structure 2, and the sealing module is connected with the adsorption module through the connector 3-2.
The sample tube 5 is installed into the sealing device through the automatic grabbing module, the tube orifice of the sample tube 5 penetrates through the annular bulge, and after the sealing ring 6 is sleeved in, the tube orifice enters the cavity 3-1 of the test head 3, and when the sample tube 5 is installed, or a user presses a starting button of the power device 1 positioned on the instrument host, or the sample tube 5 moves to a fixed coordinate position, the power device 1 pulls the auxiliary structure 2 to move.
When the auxiliary structure 2 moves upwards, the fixed test head 3 is connected to the fluid module by the connector 3-2 and thus does not move. At this time, the bulge structure 4-1 extrudes the sealing ring 6, the sealing ring 6 moves upwards, the sealing ring 6 is extruded to deform due to the existence of the shrinkage chamfer 3-3, the sealing ring 6 is tightly attached to the sample tube 5, the bulge structure 4-1 and the shrinkage chamfer 3-3, and at this time, the sealing ring 6 uniformly shrinks to extrude the sample tube 5, so that the sealing of the sample tube 5 is realized.
When the sample tube 5 needs to be dismantled, the power device 1 pulls the auxiliary structure 2 to move downwards for a small distance, at this time, the extrusion force born by the sealing ring 6 disappears along with the downward movement of the bulge structure 4-1, the original shape is restored, the binding force between the sample tube 5 and the sealing ring 6 becomes smaller, and thus, the release of the test station to the sample tube 5 is realized.
The sealing device can realize the automatic sealing and dismantling of the sample tube 5, meanwhile, in the process of automatically sealing the sample tube 5, the protruding structure 4-1 corresponds to the size and position of the sealing ring 6, and is combined with the automatic traction auxiliary structure 2 of the power machine 1, so that the degree of extrusion of the sample tube 5 and the sealing ring 6 is ensured to be identical at any time, the degree of extrusion of the sample tube 5 or sealing material is completely identical no matter how a user changes, the problem that the tightening degree of the sample tube 5 is difficult to control is solved, and the problem that the opening of the sample tube 5 is broken or air leakage is easy to occur is avoided; and the operation is easy and convenient, and the increasing demand of society for automation can be satisfied.
The adjusting block 4 is detachably mounted to the bottom of the auxiliary structure 2 by threads or screws.
Since the seal ring 6 is easily deformed or damaged by being squeezed during use, the seal ring 6 needs to be replaced. However, the sealing ring 6 is fixed in the cavity 3-1 inside the test head 3, and the auxiliary structure 2 needs to be completely removed to replace the sealing ring 6, which is very inconvenient and difficult to repair and maintain.
In this embodiment, the adjusting block 4 is detachably arranged, when the sealing ring 6 needs to be replaced, the power device 1 firstly controls the auxiliary structure 2 to downwards, releases the sealing ring 6, then takes out the sample tube 5, screws the adjusting block 4 to detach the sample tube, and then can take out the sealing ring 6 from the cavity 3-1 of the test head 3 without detaching the whole auxiliary structure 2.
In this embodiment, the adsorption medium temperature control assembly is combined with the fluid circulation device 25 to complete the measurement of the second free space volume.
As shown in fig. 8-9, the adsorption medium temperature control assembly comprises a circulating dewar 26, a circulating device first sealing ring 27, a first sealing cover 28, a circulating device second sealing ring 29 and a second sealing cover 30; the bottom of the circulating Dewar 26 is provided with a water inlet 26-2 and a water outlet 26-1; the fluid circulation device 25 is connected with the water inlet 26-2 and the water outlet 26-1, and a first annular groove is formed in the top of the circulation Dewar 26; the upper surface of the first sealing cover 28 is provided with a second annular groove; the first sealing ring 27 of the circulating device is arranged in the first annular groove, and the second sealing ring 29 of the circulating device is arranged in the second annular groove. A fluid circulation device 25 is arranged below the first seal cartridge 15.
In this embodiment, a through hole for connecting the water inlet pipe and the water outlet pipe of the fluid circulation device 25 is provided at the bottom of the first sealed chamber 15.
As shown in fig. 10 to 11, the test flow is as follows:
first, the automatic grasping module connects the nozzle of the sample tube 5 with the sealing device in a state where the first and second housing bodies 15-1 and 15-2 are opened.
The sealing device realizes automatic sealing through the action of the power machine 1.
And connecting the adsorption medium temperature control component and the sample tube 5. And then connects the fluid circulation device 25 with the circulation dewar 26.
The first and second housings 15-1 and 15-2 are closed.
At this time, the fluid circulation device 25 is not started, no liquid exists in the circulation dewar 26, the temperature in the cabin body is controlled by the temperature control module, and the first free space is tested when the temperature reaches the target temperature.
After the first free space is measured, the fluid circulation device 25 is started, the inside of the circulation dewar 26 is filled with liquid, the repeated circulation of the fluid is completed through the water inlet 26-2 and the water outlet 26-1, and after the temperature of the fluid is stabilized to the required test temperature and the pressure is stabilized, the test of the second free space is started.
After the first free space and the second free space are measured, the effective free space can be calculated, and then the adsorption test can be performed to obtain an adsorption curve.
Testing of the first free space, the second free space, the effective free space, and the adsorption curve is a common shared technique in the art.
To prevent excessive liquid inside the circulation dewar 26 from escaping from the circulation dewar 26, the present embodiment deliberately provides for sealing the opening above the circulation dewar 26 by means of a circulation means first seal ring 27 and a circulation means second seal ring 29. Thus, circulating water can only enter from the water inlet 26-2 and be discharged from the water outlet 26-1, and the adsorption process is stable.
In this embodiment, the fluid circulation device 25 is a circulation water bath of a common technology, and the automatic gripping device is a multi-axis robot with a gripper or a tri-axis cantilever Liang Mozu, etc. which are common in the market.
In a preferred embodiment, as shown in fig. 10 and 11, a power push rod 37 is mounted on the upper surface of the circulating dewar 26, and the power push rod 37 is connected to the first sealing cover 28. Under the action of the power push rod 37, the first sealing cover 28 is in sealing contact with and separated from the circulating dewar 26, so that automation is better realized. In addition, when testing the first free space, the power push rod 37 pushes the first sealing cover 28 to move upwards, so that the space inside the circulating dewar 26 is communicated with the space inside the first sealing bin 15 during testing, and the condition that the temperature inside the circulating dewar 26 is different from the temperature inside the first sealing bin 15 and the testing result is influenced is prevented.
Examples
In a preferred embodiment 2, as shown in fig. 12, a constant process adsorption apparatus includes an adsorption module, a sealing module, a second sealing bin 16, an automatic grabbing module, and a temperature control module; the second sealed cabin 16 is installed below the adsorption module and connected with the sealed module, and the temperature control module is installed in the second sealed cabin 16. The automatic grabbing module is arranged outside the second sealing bin 16 and comprises a fixed arm 17, a movable arm 18 and a grabbing head 19; the movable arm 18 is movably provided on the fixed arm 17, and the gripper 19 is provided at an end of the movable arm 18. The automatic grabbing module is used for grabbing the sample tube 5, and installing and detaching the sample tube 5.
A second pressure sensor P2, a dehumidification module 22, a humidity sensor H, an adsorption medium temperature control assembly and an automatic sealing door are arranged in the second sealing bin 16; the surface of the second sealing bin 16 is provided with an exhaust pipe 23; the exhaust pipe 23 is provided with an exhaust valve 24. The dehumidification module 22 in this embodiment is a semiconductor peltier refrigeration principle, and is a common dehumidification device in the market.
As shown in fig. 13 and 14, the self-sealing door includes a sliding frame 31, a sealing window 32, a power sliding rod 33 (which may be a cylinder, an electric cylinder, or the like, a common technique), a sealing window 34, and a thruster 35; the sealing window 32 is fixed on the inner side of the sliding frame 31 through a thruster 35 (which can be a common technology such as a cylinder, an electric cylinder and the like), and the sliding frame 31 is slidably arranged on the power sliding rod 33; the sealing window 34 is embedded with a sealing strip 36.
The power slide bar 33 pulls the sliding frame 31 to the upper edge of the sealing window 34, the thruster 35 pushes the sealing window 32 to move towards the sealing window 34, and the sealing window 32 presses the sealing strip 36, so that the sealing of the automatic sealing door is completed; when the sealing door is opened, the thruster 35 moves in the opposite direction of the sealing window 32, the pressure on the sealing strip 36 is released, and then the power slide rod 33 pulls the sliding frame 31 to the lower edge of the sealing window 34, so that the opening operation is completed.
The second sealing bin 16 is used for sealing the sample tube 5 when testing the first free space and the second free space, preventing the sample tube from being influenced by external environment change to cause larger error of the test result, and the temperature control module is used for maintaining the temperature in the second sealing bin 16 constant. The temperature control module includes an air circulation device 20, a temperature sensor T1, and a heating device 21. The air circulation device 20 in this embodiment is a fan, and the heating device 21 is an air heating rod.
Because of the existence of the second sealing bin 16 and the temperature control module, the ambient temperature around the sample tube 5 is unchanged in the whole process of testing the first free space and the second free space, so that the accuracy and stability of the test of the first free space and the second free space are ensured, and a foundation is laid for the accurate calculation of the effective free space.
In this embodiment, the automatic grabbing module is a multi-axis robot with functions of grabbing and rotating the sample tube purchased in the market (in addition, the utility model does not propose a new automatic grabbing module, but any robot capable of realizing the same or similar functions in the market can be used as a selection of the automatic grabbing module), and the embodiment can realize full automation of the adsorption process.
In this embodiment, the adsorption module includes a standard pipe 8, a first pressure sensor P1, an air inlet pipe 9, an air inlet valve 10, an air exhaust pipe 11, an air exhaust valve 12, a connection pipe 13 and a connection valve 14; the standard pipe 8 is connected with the first pressure sensor P1, one end of the air inlet pipe 9, one end of the air exhaust pipe 11 and one end of the connecting pipe 13, the other end of the connecting pipe 13 is connected with the sealing module, the air inlet valve 10 is arranged on the air inlet pipe 9, the air exhaust valve 12 is arranged on the air exhaust pipe 11, and the connecting valve 14 is arranged on the connecting pipe 13. The air inlet pipe 9 is connected with an external air source, and the air exhaust pipe 11 is connected with an external vacuumizing system. Adsorption modules are common prior art in the art.
As shown in fig. 3-7, the sealing module includes a power machine 1, an auxiliary structure 2, and a test head 3; the test head 3 is arranged inside the auxiliary structure 2; the power device 1 is connected with the auxiliary structure 2; the test head 3 is internally provided with a cavity 3-1, and one end of the test head 3 is provided with a connector 3-2; a sealing ring 6 is assembled in the cavity 3-1; the auxiliary structure 2 comprises an adjusting block 4; the adjusting block 4 is provided with a protruding structure 4-1 corresponding to the sealing ring 6; the protruding structure 4-1 is inserted into the cavity 3-1. The cavity 3-1 is provided with an inwardly converging chamfer 3-3. The adjusting block 4 forms a groove in the auxiliary structure 2; the test head 3 is positioned in the groove; the sealing ring 6 is fixed by the bulge structure 4-1 and the shrinkage chamfer 3-3; the auxiliary structure 2 is internally provided with a through hole for the sample tube 5 to pass through. The auxiliary structure 2 is connected with the power unit 1 by bolts 7.
In this embodiment, the power unit 1 is any power unit on the market that performs up-and-down motion.
The sample tube 5 is arranged in the through hole of the auxiliary structure 2, and the sealing module is connected with the adsorption module through the connector 3-2.
The sample tube 5 is installed into the sealing device through the automatic grabbing module, the tube orifice of the sample tube 5 penetrates through the annular bulge, and after the sealing ring 6 is sleeved in, the tube orifice enters the cavity 3-1 of the test head 3, and when the sample tube 5 is installed, or a user presses a starting button of the power device 1 positioned on the instrument host, or the sample tube 5 moves to a fixed coordinate position, the power device 1 pulls the auxiliary structure 2 to move.
When the auxiliary structure 2 moves upwards, the fixed test head 3 is connected to the fluid module by the connector 3-2 and thus does not move. At this time, the bulge structure 4-1 extrudes the sealing ring 6, the sealing ring 6 moves upwards, the sealing ring 6 is extruded to deform due to the existence of the shrinkage chamfer 3-3, the sealing ring 6 is tightly attached to the sample tube 5, the bulge structure 4-1 and the shrinkage chamfer 3-3, and at this time, the sealing ring 6 uniformly shrinks to extrude the sample tube 5, so that the sealing of the sample tube 5 is realized.
When the sample tube 5 needs to be dismantled, the power device 1 pulls the auxiliary structure 2 to move downwards for a small distance, at this time, the extrusion force born by the sealing ring 6 disappears along with the downward movement of the bulge structure 4-1, the original shape is restored, the binding force between the sample tube 5 and the sealing ring 6 becomes smaller, and thus, the release of the test station to the sample tube 5 is realized.
The sealing device can realize the automatic sealing and dismantling of the sample tube 5, meanwhile, in the process of automatically sealing the sample tube 5, the protruding structure 4-1 corresponds to the size and position of the sealing ring 6, and is combined with the automatic traction auxiliary structure 2 of the power machine 1, so that the degree of extrusion of the sample tube 5 and the sealing ring 6 is ensured to be identical at any time, the degree of extrusion of the sample tube 5 or sealing material is completely identical no matter how a user changes, the problem that the tightening degree of the sample tube 5 is difficult to control is solved, and the problem that the opening of the sample tube 5 is broken or air leakage is easy to occur is avoided; and the operation is easy and convenient, and the increasing demand of society for automation can be satisfied.
The adjusting block 4 is detachably mounted to the bottom of the auxiliary structure 2 by threads or screws.
Since the seal ring 6 is easily deformed or damaged by being squeezed during use, the seal ring 6 needs to be replaced. However, the sealing ring 6 is fixed in the cavity 3-1 inside the test head 3, and the auxiliary structure 2 needs to be completely removed to replace the sealing ring 6, which is very inconvenient and difficult to repair and maintain.
In this embodiment, the adjusting block 4 is detachably arranged, when the sealing ring 6 needs to be replaced, the power device 1 firstly controls the auxiliary structure 2 to downwards, releases the sealing ring 6, then takes out the sample tube 5, screws the adjusting block 4 to detach the sample tube, and then can take out the sealing ring 6 from the cavity 3-1 of the test head 3 without detaching the whole auxiliary structure 2.
In this embodiment, the adsorption medium temperature control component is an elevator 39 and a temperature control medium storage device 38.
This example was used to complete the adsorption curve determination.
In this embodiment, the temperature control medium reservoir 38 is a dewar filled with liquid nitrogen.
The test flow is as follows:
opening the automatic sealing door, and connecting the pipe orifice of the sample pipe 5 with the sealing device by the automatic grabbing module.
The sealing device realizes automatic sealing through the action of the power machine 1.
Because the temperature-controlled medium storage device 38 contains the low-temperature liquid nitrogen, after the automatic sealing door is closed, the low-temperature liquid nitrogen volatilizes, so that the pressure in the second sealing bin 16 is increased, when the pressure detected by the second pressure sensor P2 is higher than the set pressure, for example, the atmospheric pressure, at the moment, the exhaust valve 24 is opened, the gas in the second sealing bin 16 is slowly discharged along the exhaust pipe 23, the internal pressure is reduced, and the atmospheric pressure is maintained; during the removal of the volatilized nitrogen gas, the water vapor in the second sealed compartment 16 is also removed, thereby reducing the humidity.
When the humidity sensor H detects that the humidity of the second sealed cabin 16 is too high, for example, the external humidity is too high, and during the process of opening the automatic sealing door, a large amount of water vapor flows into the second sealed cabin 16, the dehumidification module 22 can be started to help reduce the humidity in the second sealed cabin 16, so that the water vapor is prevented from freezing in the temperature-control medium storage device 38 or on the surface of the sample tube.
The temperature in the second sealed compartment 16 is controlled by the temperature control module and the first free space is tested when it reaches the target temperature.
After the first free space is measured, the temperature control medium storage device 38 is lifted by the elevator 39, the bottom of the sample tube 5 with the sample is soaked in the temperature control medium, and after the pressure of the sample tube 5 is stable, the second free space is tested. The temperature and pressure in the second seal cartridge 16 at this time is then recorded. Since the temperature control medium is often low temperature medium liquid nitrogen, the volatilization of the liquid nitrogen can cause the temperature reduction and the pressure increase in the second sealed cabin 16, but the temperature and the pressure in the second sealed cabin 16 are constant by controlling the temperature through the temperature control module and venting the exhaust pipe 23. The second sealed cabin 16 is sealed, so that the pressure can be controlled to be slightly higher than the atmospheric pressure, moisture in the atmosphere is prevented from entering, and the exhaust pipe 23 can remove the moisture existing in the second sealed cabin 16, so that the humidity is effectively controlled, and the icing is prevented; if the ambient humidity is too high, the dehumidification module 22 may be activated all the way, such as semiconductor peltier dehumidification, which is a well-established technique disclosed, further ensuring that the humidity is as low as possible. After the first free space and the second free space are measured, the effective free space can be calculated, and then the adsorption test can be performed to obtain an adsorption curve.
Testing of the first free space, the second free space, the effective free space and the adsorption curve is a common shared technique in the art.
In this embodiment, the automatic gripping device is a multi-axis robot with a gripper, a tri-axis cantilever Liang Mozu, etc. which are commonly used in the market; the power slide bar, the thruster and the power device are common electric cylinders or air cylinders.
Examples
In a specific embodiment 3, as shown in fig. 15, a constant process adsorption device includes an adsorption module, a sealing module, a first sealing cabin 15, a second sealing cabin 16, an automatic grabbing module, and a temperature control module; the first sealing bin 15 is arranged below the adsorption module and is connected with the sealing module; the first sealed cabin 15 comprises a sliding rail 15-3, a first cabin body 15-1 and a second cabin body 15-2; the first bin body 15-1 and the second bin body 15-2 are slidably arranged on the lower side of the sliding rail 15-3; the first bin body 15-1 and the second bin body 15-2 are closed, then the inner cavity is sealed, and the temperature control module is arranged in the first sealed bin 15. The automatic grabbing module is arranged outside the second sealing bin 16 and comprises a fixed arm 17, a movable arm 18 and a grabbing head 19; the movable arm 18 is movably provided on the fixed arm 17, and the gripper 19 is provided at an end of the movable arm 18. The function of the automatic grabbing module is to achieve the installation and the disassembly of the sample tube 5. The second sealed cabin 16 wraps the first sealed cabin 15; a second pressure sensor P2, a dehumidification module 22, a humidity sensor H, an adsorption medium temperature control assembly and an automatic sealing door are arranged in the second sealing bin 16; the adsorption medium temperature control assembly comprises a temperature control medium storage device 38 and an elevator 39, and is arranged below the first sealed cabin 15.
The surface of the second sealing bin 16 is provided with an exhaust pipe 23; the exhaust pipe 23 is provided with an exhaust valve 24.
As shown in fig. 13 and 14, the self-sealing door includes a sliding frame 31, a sealing window 32, a power slide bar 33, a sealing window 34, and a thruster 35; the sealing window 32 is fixed on the inner side of the sliding frame 31 through a thruster 35, and the sliding frame 31 is slidably arranged on the power sliding rod 33; the sealing window 34 is embedded with a sealing strip 36. The dehumidification module 22 in this embodiment is a semiconductor peltier.
The power slide bar 33 pulls the sliding frame 31 to the upper edge of the sealing window 34, the thruster 35 pushes the sealing window 32 to move towards the sealing window 34, and the sealing window 32 presses the sealing strip 36, so that the sealing of the automatic sealing door is completed; when the sealing door is opened, the thruster 35 moves in the opposite direction of the sealing window 32, the pressure on the sealing strip 36 is released, and then the power slide rod 33 pulls the sliding frame 31 to the lower edge of the sealing window 34, so that the opening operation is completed.
The first sealing cabin 15 is used for sealing the sample tube 5 when testing the first free space, preventing the sample tube from being influenced by external environment change, so that a larger error occurs in the test result, and the temperature control module is used for maintaining the temperature in the first sealing cabin 15 to be a set temperature and is not influenced by the environment. The temperature control module includes an air circulation device 20, a temperature sensor T1, and a heating device 21. The air circulation device 20 in this embodiment is a fan, and the heating device 21 is an air heating rod.
In this embodiment, the first bin 15-1 and the second bin 15-2 slide along the sliding rail 15-3, and the power may be an air cylinder, an electric cylinder, or a sliding table with a motor. In this embodiment, because of the existence of the first seal cabin 15 and the temperature control module, the ambient temperature around the sample tube 5 is unchanged in the whole process of testing the first free space, so that the accuracy and stability of the test of the first free space are ensured, and a foundation is laid for accurate calculation of the effective free space. After the first free space test is completed. The test state is as shown in figure 16,
the first bin body 15-1 and the second bin body 15-2 are separated, and temperature control is stopped.
The second free space is tested after the pressure of the sample tube 5 has stabilized by raising the temperature control medium storage means 38 (e.g. a dewar filled with liquid nitrogen) by means of the elevator 39 and immersing the bottom of the sample tube 5 with the sample in the temperature control medium. The temperature and pressure in the second seal cartridge 16 at this time is then recorded. Since the temperature control medium is often low temperature medium liquid nitrogen, the volatilization of the liquid nitrogen can cause the temperature reduction and the pressure increase in the second sealed cabin 16, but the temperature and the pressure in the second sealed cabin 16 are constant by controlling the temperature through the temperature control module and venting the exhaust pipe 23. The second sealed cabin 16 is sealed, so that the pressure can be controlled to be slightly higher than the atmospheric pressure, moisture in the atmosphere is prevented from entering, and the exhaust pipe 23 can remove the moisture existing in the second sealed cabin 16, so that the humidity is effectively controlled, and the icing is prevented; if the ambient humidity is too high, the dehumidification module 22 may be activated all the way, such as semiconductor peltier dehumidification, which is a well-established technique disclosed, further ensuring that the humidity is as low as possible. After the effective free space is calculated, while maintaining a constant state in the second sealed compartment 16, an adsorption test can be performed. The test state is shown in fig. 17.
In this embodiment, the automatic grabbing module is a multi-axis robot with functions of grabbing and rotating the sample tube purchased in the market (in addition, the utility model does not propose a new automatic grabbing module, but any robot capable of realizing the same or similar functions in the market can be used as a selection of the automatic grabbing module), and the embodiment can realize full automation of the adsorption process.
In this embodiment, the adsorption module includes a standard pipe 8, a first pressure sensor P1, an air inlet pipe 9, an air inlet valve 10, an air exhaust pipe 11, an air exhaust valve 12, a connection pipe 13 and a connection valve 14; the standard pipe 8 is connected with the first pressure sensor P1, one end of the air inlet pipe 9, one end of the air exhaust pipe 11 and one end of the connecting pipe 13, the other end of the connecting pipe 13 is connected with the sealing module, the air inlet valve 10 is arranged on the air inlet pipe 9, the air exhaust valve 12 is arranged on the air exhaust pipe 11, and the connecting valve 14 is arranged on the connecting pipe 13. The air inlet pipe 9 is connected with an external air source, and the air exhaust pipe 11 is connected with an external vacuumizing system. Adsorption modules are common prior art in the art.
As shown in fig. 3-7, the sealing module includes a power machine 1, an auxiliary structure 2, and a test head 3; the test head 3 is arranged inside the auxiliary structure 2; the power device 1 is connected with the auxiliary structure 2; the test head 3 is internally provided with a cavity 3-1, and one end of the test head 3 is provided with a connector 3-2; a sealing ring 6 is assembled in the cavity 3-1; the auxiliary structure 2 comprises an adjusting block 4; the adjusting block 4 is provided with a protruding structure 4-1 corresponding to the sealing ring 6; the protruding structure 4-1 is inserted into the cavity 3-1. The cavity 3-1 is provided with an inwardly converging chamfer 3-3. The adjusting block 4 forms a groove in the auxiliary structure 2; the test head 3 is positioned in the groove; the sealing ring 6 is fixed by the bulge structure 4-1 and the shrinkage chamfer 3-3; the auxiliary structure 2 is internally provided with a through hole for the sample tube 5 to pass through. The auxiliary structure 2 is connected with the power unit 1 by bolts 7.
In this embodiment, the power unit 1 is any power unit on the market that performs up-and-down motion.
The sample tube 5 is arranged in the through hole of the auxiliary structure 2, and the sealing module is connected with the adsorption module through the connector 3-2.
The sample tube 5 is installed into the sealing device through the automatic grabbing module, the tube orifice of the sample tube 5 penetrates through the annular bulge, and after the sealing ring 6 is sleeved in, the tube orifice enters the cavity 3-1 of the test head 3, and when the sample tube 5 is installed, or a user presses a starting button of the power device 1 positioned on the instrument host, or the sample tube 5 moves to a fixed coordinate position, the power device 1 pulls the auxiliary structure 2 to move.
When the auxiliary structure 2 moves upwards, the fixed test head 3 is connected to the fluid module by the connector 3-2 and thus does not move. At this time, the bulge structure 4-1 extrudes the sealing ring 6, the sealing ring 6 moves upwards, the sealing ring 6 is extruded to deform due to the existence of the shrinkage chamfer 3-3, the sealing ring 6 is tightly attached to the sample tube 5, the bulge structure 4-1 and the shrinkage chamfer 3-3, and at this time, the sealing ring 6 uniformly shrinks to extrude the sample tube 5, so that the sealing of the sample tube 5 is realized.
When the sample tube 5 needs to be dismantled, the power device 1 pulls the auxiliary structure 2 to move downwards for a small distance, at this time, the extrusion force born by the sealing ring 6 disappears along with the downward movement of the bulge structure 4-1, the original shape is restored, the binding force between the sample tube 5 and the sealing ring 6 becomes smaller, and thus, the release of the test station to the sample tube 5 is realized.
The sealing device can realize the automatic sealing and dismantling of the sample tube 5, meanwhile, in the process of automatically sealing the sample tube 5, the protruding structure 4-1 corresponds to the size and position of the sealing ring 6, and is combined with the automatic traction auxiliary structure 2 of the power machine 1, so that the degree of extrusion of the sample tube 5 and the sealing ring 6 is ensured to be identical at any time, the degree of extrusion of the sample tube 5 or sealing material is completely identical no matter how a user changes, the problem that the tightening degree of the sample tube 5 is difficult to control is solved, and the problem that the opening of the sample tube 5 is broken or air leakage is easy to occur is avoided; and the operation is easy and convenient, and the increasing demand of society for automation can be satisfied.
The adjusting block 4 is detachably mounted to the bottom of the auxiliary structure 2 by threads or screws.
Since the seal ring 6 is easily deformed or damaged by being squeezed during use, the seal ring 6 needs to be replaced. However, the sealing ring 6 is fixed in the cavity 3-1 inside the test head 3, and the auxiliary structure 2 needs to be completely removed to replace the sealing ring 6, which is very inconvenient and difficult to repair and maintain.
In this embodiment, the adjusting block 4 is detachably arranged, when the sealing ring 6 needs to be replaced, the power device 1 firstly controls the auxiliary structure 2 to downwards, releases the sealing ring 6, then takes out the sample tube 5, screws the adjusting block 4 to detach the sample tube, and then can take out the sealing ring 6 from the cavity 3-1 of the test head 3 without detaching the whole auxiliary structure 2.
When the humidity sensor H detects that the humidity of the second sealed compartment 16 is too high, the dehumidification module 22 is activated to assist in reducing the humidity, preventing icing, and maintaining the second free space constant.
When the temperature sensor T1 detects that the temperature of the adsorption environment changes, the temperature control module installed in the first seal cabin 15 is started to adjust the temperature, so that the temperature is kept constant.
When the second pressure sensor P2 detects that the pressure of the adsorption environment rises, the exhaust valve 24 is opened, the gas in the second sealed cabin 16 is slowly discharged along the exhaust pipe 23, the internal pressure is reduced, the pressure is kept constant, and the saturated vapor pressure of the nitrogen is kept constant, and the high reproducibility and the high precision of the test result are facilitated.
Examples
In a specific embodiment 4, as shown in fig. 18, a constant process adsorption device includes an adsorption module, a sealing module, a first sealing cabin 15, a second sealing cabin 16, an automatic grabbing module, and a temperature control module; the second sealing bin 16 is arranged below the adsorption module and is connected with the sealing module; the first sealing bin 15 is arranged below the second sealing bin 16; the first sealed cabin 15 comprises a sliding rail 15-3, a first cabin body 15-1 and a second cabin body 15-2; the first bin body 15-1 and the second bin body 15-2 are slidably arranged on the lower side of the sliding rail 15-3; the first bin body 15-1 and the second bin body 15-2 are sealed, and the temperature control module is arranged in the second sealed bin 16. The automatic grabbing module is arranged outside the second sealing bin 16 and comprises a fixed arm 17, a movable arm 18 and a grabbing head 19; the movable arm 18 is movably provided on the fixed arm 17, and the gripper 19 is provided at an end of the movable arm 18. The function of the automatic grabbing module is to achieve the installation and the disassembly of the sample tube 5. A second pressure sensor P2, a dehumidification module 22, a humidity sensor H and an adsorption medium temperature control component are arranged in the second sealing bin 16; the adsorption medium temperature control assembly comprises a temperature control medium storage device 38 and an elevator 39, and is arranged below the first sealed cabin 15.
The surface of the second sealing bin 16 is provided with an exhaust pipe 23; the exhaust pipe 23 is provided with an exhaust valve 24.
The dehumidification module 22 in this embodiment is a semiconductor peltier.
The first sealing bin 15 is used for sealing the sample tube 5 when testing the first free space, preventing the sample tube from being influenced by external environment changes, so that a larger error occurs in the test result, and the temperature control module is used for maintaining the temperature in the first sealing bin 15 and the second sealing bin 16 to be a set temperature and is not influenced by the environment. The temperature control module includes an air circulation device 20, a temperature sensor T1, and a heating device 21. The air circulation device 20 in this embodiment is a fan, and the heating device 21 is an air heating rod.
In this embodiment, the first bin 15-1 and the second bin 15-2 slide along the sliding rail 15-3, and the power may be an air cylinder, an electric cylinder, or a sliding table with a motor. In this embodiment, because of the existence of the first seal cabin 15 and the temperature control module, the ambient temperature around the sample tube 5 is unchanged in the whole process of testing the first free space, so that the accuracy and stability of the test of the first free space are ensured, and a foundation is laid for accurate calculation of the effective free space. The test state is shown in fig. 19.
After the first free space test is finished, the first bin body 15-1 and the second bin body 15-2 are separated, and temperature control is stopped.
The temperature control medium storage device 38 (for example, a dewar bottle filled with liquid nitrogen) is lifted by the elevator 39, the bottom of the sample tube 5 with the sample is soaked in the temperature control medium, after the pressure of the sample tube 5 is stable, the second free space is tested, at this time, the temperature control medium storage device 38 is connected with the bottom of the second sealing bin 16 in a sealing way, and therefore the constant environment is ensured when the second free space is tested. The temperature and pressure in the second seal cartridge 16 at this time is then recorded. Since the temperature control medium is often low temperature medium liquid nitrogen, the volatilization of the liquid nitrogen can cause the temperature reduction and the pressure increase in the second sealed cabin 16, but the temperature and the pressure in the second sealed cabin 16 are constant by controlling the temperature through the temperature control module and venting the exhaust pipe 23. The second sealed cabin 16 is sealed, the pressure can be controlled to be slightly higher than the atmospheric pressure, so that moisture in the atmosphere is prevented from entering, and the exhaust pipe 23 can remove the moisture existing in the second sealed cabin 16, so that the humidity is effectively controlled, and the icing is prevented; if the ambient humidity is too high, the dehumidification module 22 may be activated all the way, such as semiconductor peltier dehumidification, which is a well-established technique disclosed, further ensuring that the humidity is as low as possible. After the effective free space is calculated, while maintaining a constant state in the second sealed compartment 16, an adsorption test can be performed. The test state is shown in fig. 20.
In this embodiment, the automatic grabbing module is a multi-axis robot with functions of grabbing and rotating the sample tube purchased in the market (in addition, the utility model does not propose a new automatic grabbing module, but any robot capable of realizing the same or similar functions in the market can be used as a selection of the automatic grabbing module), and the embodiment can realize full automation of the adsorption process.
In this embodiment, the adsorption module includes a standard pipe 8, a first pressure sensor P1, an air inlet pipe 9, an air inlet valve 10, an air exhaust pipe 11, an air exhaust valve 12, a connection pipe 13 and a connection valve 14; the standard pipe 8 is connected with the first pressure sensor P1, one end of the air inlet pipe 9, one end of the air exhaust pipe 11 and one end of the connecting pipe 13, the other end of the connecting pipe 13 is connected with the sealing module, the air inlet valve 10 is arranged on the air inlet pipe 9, the air exhaust valve 12 is arranged on the air exhaust pipe 11, and the connecting valve 14 is arranged on the connecting pipe 13. The air inlet pipe 9 is connected with an external air source, and the air exhaust pipe 11 is connected with an external vacuumizing system. Adsorption modules are common prior art in the art.
As shown in fig. 3-7, the sealing module includes a power machine 1, an auxiliary structure 2, and a test head 3; the test head 3 is arranged inside the auxiliary structure 2; the power device 1 is connected with the auxiliary structure 2; the test head 3 is internally provided with a cavity 3-1, and one end of the test head 3 is provided with a connector 3-2; a sealing ring 6 is assembled in the cavity 3-1; the auxiliary structure 2 comprises an adjusting block 4; the adjusting block 4 is provided with a protruding structure 4-1 corresponding to the sealing ring 6; the protruding structure 4-1 is inserted into the cavity 3-1. The cavity 3-1 is provided with an inwardly converging chamfer 3-3. The adjusting block 4 forms a groove in the auxiliary structure 2; the test head 3 is positioned in the groove; the sealing ring 6 is fixed by the bulge structure 4-1 and the shrinkage chamfer 3-3; the auxiliary structure 2 is internally provided with a through hole for the sample tube 5 to pass through. The auxiliary structure 2 is connected with the power unit 1 by bolts 7.
In this embodiment, the power unit 1 is any power unit on the market that performs up-and-down motion.
The sample tube 5 is arranged in the through hole of the auxiliary structure 2, and the sealing module is connected with the adsorption module through the connector 3-2.
The sample tube 5 is installed into the sealing device through the automatic grabbing module, the tube orifice of the sample tube 5 penetrates through the annular bulge, and after the sealing ring 6 is sleeved in, the tube orifice enters the cavity 3-1 of the test head 3, and when the sample tube 5 is installed, or a user presses a starting button of the power device 1 positioned on the instrument host, or the sample tube 5 moves to a fixed coordinate position, the power device 1 pulls the auxiliary structure 2 to move.
When the auxiliary structure 2 moves upwards, the fixed test head 3 is connected to the fluid module by the connector 3-2 and thus does not move. At this time, the bulge structure 4-1 extrudes the sealing ring 6, the sealing ring 6 moves upwards, the sealing ring 6 is extruded to deform due to the existence of the shrinkage chamfer 3-3, the sealing ring 6 is tightly attached to the sample tube 5, the bulge structure 4-1 and the shrinkage chamfer 3-3, and at this time, the sealing ring 6 uniformly shrinks to extrude the sample tube 5, so that the sealing of the sample tube 5 is realized.
When the sample tube 5 needs to be dismantled, the power device 1 pulls the auxiliary structure 2 to move downwards for a small distance, at this time, the extrusion force born by the sealing ring 6 disappears along with the downward movement of the bulge structure 4-1, the original shape is restored, the binding force between the sample tube 5 and the sealing ring 6 becomes smaller, and thus, the release of the test station to the sample tube 5 is realized.
The sealing device can realize the automatic sealing and dismantling of the sample tube 5, meanwhile, in the process of automatically sealing the sample tube 5, the protruding structure 4-1 corresponds to the size and position of the sealing ring 6, and is combined with the automatic traction auxiliary structure 2 of the power machine 1, so that the degree of extrusion of the sample tube 5 and the sealing ring 6 is ensured to be identical at any time, the degree of extrusion of the sample tube 5 or sealing material is completely identical no matter how a user changes, the problem that the tightening degree of the sample tube 5 is difficult to control is solved, and the problem that the opening of the sample tube 5 is broken or air leakage is easy to occur is avoided; and the operation is easy and convenient, and the increasing demand of society for automation can be satisfied.
The adjusting block 4 is detachably mounted to the bottom of the auxiliary structure 2 by threads or screws.
Since the seal ring 6 is easily deformed or damaged by being squeezed during use, the seal ring 6 needs to be replaced. However, the sealing ring 6 is fixed in the cavity 3-1 inside the test head 3, and the auxiliary structure 2 needs to be completely removed to replace the sealing ring 6, which is very inconvenient and difficult to repair and maintain.
In this embodiment, the adjusting block 4 is detachably arranged, when the sealing ring 6 needs to be replaced, the power device 1 firstly controls the auxiliary structure 2 to downwards, releases the sealing ring 6, then takes out the sample tube 5, screws the adjusting block 4 to detach the sample tube, and then can take out the sealing ring 6 from the cavity 3-1 of the test head 3 without detaching the whole auxiliary structure 2.
When the humidity sensor H detects that the humidity of the second sealed compartment 16 is too high, the dehumidification module 22 is activated to assist in reducing the humidity, preventing icing, and affecting the constancy of the second free space.
When the temperature sensor T1 detects that the temperature of the adsorption environment changes, the temperature control module is started to adjust the temperature, so that the temperature is kept constant.
When the second pressure sensor P2 detects that the pressure of the adsorption environment rises, the exhaust valve 24 is opened, the gas in the second sealed cabin 16 is slowly discharged along the exhaust pipe 23, the internal pressure is reduced, the pressure is kept constant, and the saturated vapor pressure of the nitrogen is kept constant, and the high reproducibility and the high precision of the test result are facilitated.
Examples
In a specific embodiment 5, as shown in fig. 20, a constant process adsorption apparatus includes an adsorption module, a sealing module, a first sealing chamber 15, a second sealing chamber 16, an automatic grabbing module, a temperature control module, an XY axis moving module, and an adsorption medium temperature control assembly; the second sealed cabin 16 is installed below the adsorption module and is connected with the adsorption module, and a communication port capable of being opened and closed is arranged between the second sealed cabin 16 and the adsorption module.
In this embodiment, the adsorption module includes a standard pipe 8, a first pressure sensor P1, an air inlet pipe 9, an air inlet valve 10, an air exhaust pipe 11, an air exhaust valve 12, a connection pipe 13 and a connection valve 14; the standard pipe 8 is connected with the first pressure sensor P1, one end of the air inlet pipe 9, one end of the air exhaust pipe 11 and one end of the connecting pipe 13, the other end of the connecting pipe 13 is connected with the sealing module, the air inlet valve 10 is arranged on the air inlet pipe 9, the air exhaust valve 12 is arranged on the air exhaust pipe 11, and the connecting valve 14 is arranged on the connecting pipe 13. The air inlet pipe 9 is connected with an external air source, and the air exhaust pipe 11 is connected with an external vacuumizing system. Adsorption modules are common prior art in the art.
As shown in fig. 3-7, the sealing module includes a power machine 1, an auxiliary structure 2, and a test head 3; the test head 3 is arranged inside the auxiliary structure 2; the power device 1 is connected with the auxiliary structure 2; the test head 3 is internally provided with a cavity 3-1, and one end of the test head 3 is provided with a connector 3-2; a sealing ring 6 is assembled in the cavity 3-1; the auxiliary structure 2 comprises an adjusting block 4; the adjusting block 4 is provided with a protruding structure 4-1 corresponding to the sealing ring 6; the protruding structure 4-1 is inserted into the cavity 3-1. The cavity 3-1 is provided with an inwardly converging chamfer 3-3. The adjusting block 4 forms a groove in the auxiliary structure 2; the test head 3 is positioned in the groove; the sealing ring 6 is fixed by the bulge structure 4-1 and the shrinkage chamfer 3-3; the auxiliary structure 2 is internally provided with a through hole for the sample tube 5 to pass through. The auxiliary structure 2 is connected with the power unit 1 by bolts 7.
In this embodiment, the power unit 1 is any power unit on the market that performs up-and-down motion.
The sample tube 5 is arranged in the through hole of the auxiliary structure 2, and the sealing module is connected with the adsorption module through the connector 3-2.
The sample tube 5 is installed into the sealing device through the automatic grabbing module, the tube orifice of the sample tube 5 penetrates through the annular bulge, and after the sealing ring 6 is sleeved in, the tube orifice enters the cavity 3-1 of the test head 3, and when the sample tube 5 is installed, or a user presses a starting button of the power device 1 positioned on the instrument host, or the sample tube 5 moves to a fixed coordinate position, the power device 1 pulls the auxiliary structure 2 to move.
When the auxiliary structure 2 moves upwards, the fixed test head 3 is connected to the fluid module by the connector 3-2 and thus does not move. At this time, the bulge structure 4-1 extrudes the sealing ring 6, the sealing ring 6 moves upwards, the sealing ring 6 is extruded to deform due to the existence of the shrinkage chamfer 3-3, the sealing ring 6 is tightly attached to the sample tube 5, the bulge structure 4-1 and the shrinkage chamfer 3-3, and at this time, the sealing ring 6 uniformly shrinks to extrude the sample tube 5, so that the sealing of the sample tube 5 is realized.
When the sample tube 5 needs to be dismantled, the power device 1 pulls the auxiliary structure 2 to move downwards for a small distance, at this time, the extrusion force born by the sealing ring 6 disappears along with the downward movement of the bulge structure 4-1, the original shape is restored, the binding force between the sample tube 5 and the sealing ring 6 becomes smaller, and thus, the release of the test station to the sample tube 5 is realized.
The sealing device can realize the automatic sealing and dismantling of the sample tube 5, meanwhile, in the process of automatically sealing the sample tube 5, the protruding structure 4-1 corresponds to the size and position of the sealing ring 6, and is combined with the automatic traction auxiliary structure 2 of the power machine 1, so that the degree of extrusion of the sample tube 5 and the sealing ring 6 is ensured to be identical at any time, the degree of extrusion of the sample tube 5 or sealing material is completely identical no matter how a user changes, the problem that the tightening degree of the sample tube 5 is difficult to control is solved, and the problem that the opening of the sample tube 5 is broken or air leakage is easy to occur is avoided; and the operation is easy and convenient, and the increasing demand of society for automation can be satisfied.
The adjusting block 4 is detachably mounted to the bottom of the auxiliary structure 2 by threads or screws.
Since the seal ring 6 is easily deformed or damaged by being squeezed during use, the seal ring 6 needs to be replaced. However, the sealing ring 6 is fixed in the cavity 3-1 inside the test head 3, and the auxiliary structure 2 needs to be completely removed to replace the sealing ring 6, which is very inconvenient and difficult to repair and maintain.
In this embodiment, the adjusting block 4 is detachably arranged, when the sealing ring 6 needs to be replaced, the power device 1 firstly controls the auxiliary structure 2 to downwards, releases the sealing ring 6, then takes out the sample tube 5, screws the adjusting block 4 to detach the sample tube, and then can take out the sealing ring 6 from the cavity 3-1 of the test head 3 without detaching the whole auxiliary structure 2.
The temperature control module is arranged in the adsorption module. The automatic grabbing module is arranged outside the second sealing bin 16 and comprises a fixed arm 17, a movable arm 18 and a grabbing head 19; the movable arm 18 is movably provided on the fixed arm 17, and the gripper 19 is provided at an end of the movable arm 18. The function of the automatic grabbing module is to achieve the installation and the disassembly of the sample tube 5. A second pressure sensor P2, a dehumidification module 22 and a humidity sensor H are mounted in the second seal cartridge 16. The surface of the second sealing bin 16 is provided with an exhaust pipe 23; the exhaust pipe 23 is provided with an exhaust valve 24. The dehumidification module 22 in this embodiment is a semiconductor peltier.
The adsorption media temperature control assembly includes a temperature control media reservoir 38 (e.g., a dewar filled with liquid nitrogen).
The XY axis moving module includes an X axis moving module 40 (the X axis moving module 40 is provided with an independent power module, which may be an air cylinder, an electric lever, etc., and is controlled to move left and right, not shown in fig. 26), a Y axis moving module 41 (the Y axis moving module 41 is provided with an independent power module, which may be an air cylinder, an electric lever, etc., and is controlled to move up and down, not shown in fig. 26), a motor 42, a slide rod 43, and a fixing rod 44, the first seal cartridge 15 is slidably mounted on the X axis moving module 40, the X axis moving module 40 is slidably mounted on the Y axis moving module 41, the bottom of the Y axis moving module 41 is fixed on the fixing rod 44, the temperature control medium storing device 38 is connected to the slide rod 43 through the fixing rod 44, and the fixing rod 44 is slidable up and down along the slide rod 43. The motor 42 is provided at the upper end of the slide rod 43 to power the up-and-down movement of the XY-axis moving module as a whole and the up-and-down movement of the fixed rod 44.
The bottom of the second sealing bin 16 is provided with an opening, the shape of the opening is matched with the shape of the top of the first sealing bin 15 and the top of the temperature control medium storage device 38, and a sealing rubber ring is arranged at the opening. The second seal cartridge 16 may be in sealing connection with the first seal cartridge 15 or the temperature control medium reservoir 38. For example, the first seal chamber 15 moves under the opening under the action of the X-axis moving module 40, and then moves upwards by the action of the Y-axis moving module or the pushing force provided by the fixing rod 44, and the top of the first seal chamber 15 presses the rubber ring to seal the first seal chamber 15 and the second seal chamber 16; when the first sealing bin 15 moves to one side of the X-axis moving module 40, the motor 42 controls the fixing rod 44 connected with the temperature control medium storage device 38 to move upwards, and the top of the temperature control medium storage device 38 presses the rubber ring, so that the temperature control medium storage device 38 and the second sealing bin 16 are sealed.
The bottom of the first sealed cabin 15 is provided with an inner groove and a rubber ring which are completely identical with those of the bottom structure of the second sealed cabin 16, when the first sealed cabin 15 moves to the position right above the temperature control medium storage device 38 under the action of the X-axis moving module 40, then the first sealed cabin 15 moves downwards under the action of the X-axis moving module 40, the rubber ring is extruded by the bottom of the first sealed cabin 15 and the top of the temperature control medium storage device 38, and simple isolation sealing of the first sealed cabin 15 and the temperature control medium storage device 38 is realized. In this way, the temperature control medium storage device 38 can be guaranteed to form positive pressure in the temperature control medium storage device 38 due to volatilization of low-temperature liquid nitrogen, and water vapor in the air is prevented from freezing in the temperature control medium storage device 38.
The first sealing bin 15 is used for sealing the second sealing bin 16 when testing the first free space, preventing the sample tube 5 from being influenced by external environment change to cause larger error of the test result, or sealing the temperature control medium storage device 38, and preventing low-temperature liquid nitrogen from freezing in the temperature control medium storage device 38 due to the fact that the temperature is lower than the room temperature.
The temperature control module is used for maintaining the temperature in the second sealed cabin 16 to be a set temperature and is not influenced by the environment, so that the environment of the sample tube is ensured to be constant when the first free space is tested.
The temperature control module includes an air circulation device 20, a temperature sensor T1, and a heating device 21. The air circulation device 20 in this embodiment is a fan, and the heating device 21 is an air heating rod.
In this embodiment, when testing the first free space, first the fixing rod 44 is downward along the sliding rod 43, the temperature control medium storage device 38 sealed by the first sealing bin 15 is separated from the second sealing bin 16, and the automatic gripping module grips the sample tube 5 and fixes it to the sealing module. The fixing lever 44 is upwardly along the sliding lever 43, and the first sealing chamber 15 and the temperature control medium reservoir 38 are simultaneously raised until the first sealing chamber 15 simultaneously seals the second sealing chamber 16 and the temperature control medium reservoir. A first free space test is then performed. At this time, the communication port between the second sealed cabin 16 and the adsorption module is opened, when the temperature sensor T1 detects that the temperature changes, the temperature control module adjusts the temperature, maintains the temperature to a set temperature, and the temperature remains constant, so that the ambient temperature around the sample tube 5 is unchanged in the whole process of testing the first free space, thereby ensuring the accuracy and stability of the test of the first free space and laying a foundation for accurate calculation of the effective free space. The test procedure is shown in fig. 21 and 22.
After the first free space test is completed, the fixed rod 44 moves downward along the sliding rod 43, the first seal cartridge 15 and the temperature control medium storage device 38 move downward, and the communication port is closed.
The first sealing bin 15 moves to one side along the X-axis moving module 40, then moves downwards along the Y-axis moving module 41 until the upper edge of the first sealing bin 15 is not higher than the upper edge of the temperature control medium storage device 38, then the fixing rod 44 moves upwards along the sliding rod 43, the temperature control medium storage device 38 moves upwards, the top of the temperature control medium storage device 38 presses the rubber ring at the bottom opening of the second sealing bin 16, sealing is achieved, at the moment, in the temperature control medium immersed in the bottom of the sample tube 5 filled with the sample, after the pressure of the sample tube 5 is stable, the second free space is tested, and the environment is constant when the second free space is tested because the temperature control medium storage device 38 is in sealing connection with the bottom of the second sealing bin 16. The temperature and pressure in the second seal cartridge 16 at this time is then recorded. Because the temperature control medium is often low-temperature medium liquid nitrogen, the pressure in the second sealed cabin 16 is increased due to volatilization of the liquid nitrogen, and the pressure in the second sealed cabin 16 is constant due to leakage of air through the air exhaust pipe 23. Meanwhile, the volatilization absorbs heat, so that the temperature in the second sealed bin can be reduced, and the second sealed bin can be subjected to temperature compensation by rapidly opening the communication port, so that the constant temperature is maintained. The second sealed cabin 16 is sealed, the pressure can be controlled to be slightly higher than the atmospheric pressure, so that moisture in the atmosphere is prevented from entering, and the exhaust pipe 23 can remove the moisture existing in the second sealed cabin 16, so that the humidity is effectively controlled, and the icing is prevented; if the ambient humidity is too high, the dehumidification module 22 may be activated all the way, such as semiconductor peltier dehumidification, which is a well-established technique disclosed, further ensuring that the humidity is as low as possible. After the effective free space is calculated, while maintaining a constant state in the second sealed compartment 16, an adsorption test can be performed. The test conditions are shown in fig. 23 and 24.
In this embodiment, the automatic grabbing module is a multi-axis robot with functions of grabbing and rotating the sample tube purchased in the market (in addition, the utility model does not propose a new automatic grabbing module, but any robot capable of realizing the same or similar functions in the market can be used as a selection of the automatic grabbing module), and the embodiment can realize full automation of the adsorption process.
When the humidity sensor H detects that the humidity of the second sealed compartment 16 is too high, the dehumidification module 22 is activated to assist in reducing the humidity, preventing icing, and affecting the constancy of the second free space.
When the second pressure sensor P2 detects that the pressure of the adsorption environment rises, the exhaust valve 24 is opened, the gas in the second sealed cabin 16 is slowly discharged along the exhaust pipe 23, the internal pressure is reduced, the pressure is kept constant, and the saturated vapor pressure of the nitrogen is kept constant, and the high reproducibility and the high precision of the test result are facilitated.

Claims (10)

1. The constant-state process adsorption device comprises an adsorption module, an adsorption medium temperature control assembly and a sealing module, wherein the adsorption module is connected with the sealing module; the sealing module is connected with the adsorption module, and the temperature control module is arranged in the sealing module or the adsorption module; the sealing module comprises a first sealing bin and/or a second sealing bin; the first sealing bin is arranged in the second sealing bin or is connected with the second sealing bin; when the temperature control module is arranged in the adsorption module, a communication port is formed between the temperature control module and the sealing module; the adsorption medium temperature control component is arranged in the second sealed bin or below the first sealed bin.
2. The steady state process adsorption device of claim 1, wherein the sealing module comprises a power plant, an auxiliary structure, and a test head; the power device is connected with the auxiliary structure or the test head; a cavity is formed in the test head, and a connector is arranged at one end of the test head; a sealing element is assembled in the cavity; the auxiliary structure comprises an adjusting block; the adjusting block is provided with a protruding structure corresponding to the sealing piece; the raised structure is inserted into the cavity.
3. The steady state process adsorption device of claim 2, further comprising an automatic grasping module; the automatic grabbing module comprises a fixed arm, a movable arm and a grabbing head; the movable arm is movably arranged on the fixed arm, and the grabbing head is arranged at the end part of the movable arm.
4. The steady state process adsorption device of claim 1, wherein the second sealed compartment is provided with a vent channel.
5. The steady state process adsorption device of claim 4, wherein a dehumidification device and/or a humidity sensor is arranged within the second sealed compartment.
6. The steady state process adsorption device of claim 1, wherein the adsorption medium temperature control assembly comprises a circulating dewar, a circulating device first seal ring, a first seal cover, a circulating device second seal ring, and a second seal cover; the bottom of the circulating Dewar is provided with an inlet and an outlet; the circulation Du Wading part is provided with a first annular groove; the upper surface of the first sealing cover is provided with a second annular groove; the first sealing ring of the circulating device is arranged in the first annular groove, and the second sealing ring of the circulating device is arranged in the second annular groove.
7. The steady state process adsorption device of claim 6, wherein a power pushrod is mounted on the upper surface of the cyclic dewar, the power pushrod being connected to the first sealing cap.
8. The steady state process adsorption device of claim 1, wherein the second sealed housing further comprises an automatic sealing door; the automatic sealing door comprises a sliding frame, a sealing window, a power sliding rod, a sealing window and a thruster; the sealing window is fixed on the inner side of the sliding frame through the thruster, and the sliding frame is slidably arranged on the power sliding rod; the sealing window is embedded with a sealing strip.
9. The steady state process adsorption device of claim 1, wherein the first sealed cartridge comprises a sliding rail, a first cartridge body, and a second cartridge body; the first bin body and the second bin body are slidably connected with the sliding rail.
10. The steady state process adsorption device of claim 4, wherein an exhaust valve is provided on the exhaust passage; and a first pressure sensor is arranged in the second sealing bin.
CN202321838237.8U 2023-07-13 2023-07-13 Constant state process adsorption device Active CN220772682U (en)

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Application Number Priority Date Filing Date Title
CN202321838237.8U CN220772682U (en) 2023-07-13 2023-07-13 Constant state process adsorption device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321838237.8U CN220772682U (en) 2023-07-13 2023-07-13 Constant state process adsorption device

Publications (1)

Publication Number Publication Date
CN220772682U true CN220772682U (en) 2024-04-12

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Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
CN (1) CN220772682U (en)

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