Ultralow-temperature sample freezing table, freezing platform and pyrolytic analysis cooperative work system

By designing an ultra-low-temperature freezing sample table including sample placement box, refrigeration pipeline, mobile bin door and drive device, the problem of poor effect of existing low-temperature equipment is solved, and effective freezing and thermal analysis of samples in ultra-low-temperature state is achieved, and working efficiency and sealing performance are improved.

CN119738245APending Publication Date: 2025-04-01CHINA PETROLEUM & CHEMICAL CORP +1

Patent Information

Application Number
CN202311281164.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-09-30
Publication Date
2025-04-01

AI Technical Summary

Technical Problem

The existing low-temperature equipment is poor in freezing and pyrolysis analysis, and the structural design is unreasonable, so it cannot be effectively applied to the low-temperature freezing operation of shale samples.

Method used

An ultra-low temperature freezing sample table is designed, including sample placement box, refrigeration pipeline, mobile bin door and drive device. The mobile bin door is opened and closed by chain transmission or belt transmission, and combined with the refrigeration device and drying device, ensuring that the samples are subject to batch freezing and thermal analysis in ultra-low temperature state.

Benefits of technology

Effective freezing and pyrolysis analysis of the samples under ultra-low temperature conditions is achieved, which avoids the loss of light hydrocarbons, improves working efficiency, and has a reasonable structural design and good sealing performance.

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Abstract

The invention relates to the technical field of freezing pyrolysis analysis, and discloses an ultralow-temperature freezing sample table, a freezing platform and a pyrolysis analysis cooperative work system. According to the ultra-low temperature freezing sample table, a sample placing box is provided with an opening; the refrigeration pipeline is fixed in the sample placing box; the movable bin door is connected above the sample placing box; the driving device is connected with the movable bin door and used for driving the movable bin door to open and close the opening. The pyrolysis analysis cooperative work system comprises a pyrolysis instrument and an ultralow-temperature freezing platform, and the ultralow-temperature freezing sample table supplies a sample to the pyrolysis instrument. The ultra-low temperature freezing sample table and the ultra-low temperature freezing platform can be matched with the pyrolysis instrument to perform pyrolysis work. Compared with a traditional pyrolysis experiment, the technical scheme provided by the invention can ensure that a sample to be pyrolyzed and analyzed is kept in an ultralow temperature state, so that the loss of light hydrocarbon is avoided, and the use effect is better. Compared with frozen closed crushed sample pyrolysis, the technical scheme provided by the invention can realize batch analysis of samples in cooperation with a pyrolysis instrument, and the working efficiency is greatly improved.
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Description

Technical Field

[0001] The present invention relates to the field of cryo-pyrolysis analysis technology, and in particular to an ultra-low temperature freezing sample stage, a freezing platform and a pyrolysis analysis collaborative working system; the present technology is mainly applied to the oil content of shale, and batch cryo-pyrolysis analysis is carried out in conjunction with a pyrolyzer, so as to conduct a more accurate oil content evaluation. Background Art

[0002] A search and analysis was conducted in this technical field to obtain the following relatively close prior arts.

[0003] 1. Application No. CN202120318388.5 discloses an electrical low-temperature protection device. After analysis, the device has no door control system, and the door is opened and closed entirely by manual operation; the door is an integrated hard structure, and it is impossible to achieve continuous changes in the opening and closing state; there is no sealing structure between the door and the box body, and changes in external temperature and humidity can easily affect the environment inside the box; dehumidification is performed by the fan on the top, which further affects the overall thermal insulation and sealing performance.

[0004] 2. Application No. CN201610330783.9 discloses a double-head insulation box for low-temperature CTOD testing. In the technical solution, a low-temperature solution is directly poured into the insulation box to achieve refrigeration. If the coolant is not replaced, the temperature of the insulation box will rise to room temperature after a period of time. There is no control system that cooperates with the test machine. Regardless of whether the test machine is working or not, the insulation box as a whole is always in an open state, and it is impossible to ensure whether the environment inside the insulation box is dry.

[0005] 3. Application No. CN202121119381.7 discloses a vacuum system for a vacuum freeze dryer. The vacuum system does not have a door control system. The door is closed by manually pressing the top plate down until the slot is stuck in the connection slot; drying is achieved by the freeze dryer inside the box; the inside of the box is in a strictly sealed state when working, and the vacuum is evacuated by the vacuum pump inside the box; it contains a timing system, which starts timing when working, and the user manually controls the working state according to the timing situation.

[0006] 4. Application No. CN202120764579.4 discloses a multifunctional heating, cooling and heat preservation box. The cooling is realized by the semiconductor chip inside the box; it can be used for both cooling and heating; the heat dissipation during cooling is realized by the fan inside the box. The cooling effect is poor.

[0007] 5. Application No. CN200420017227.9 discloses a small low-temperature biological freezer. After analysis, it is found that the refrigeration method is to directly immerse the sample to be frozen in supercooled liquid nitrogen, which can quickly cool the sample to -210°C, but the volume of the refrigerated sample is very small, only at the millimeter level.

[0008] Analysis of the above-mentioned cryogenic equipment shows that due to poor refrigeration effect and unreasonable structural design, this type of equipment cannot be used for low-temperature freezing operations of shale samples. Summary of the invention

[0009] The present application provides an ultra-low temperature freezing sample table, a freezing platform and a pyrolysis analysis collaborative working system to solve the above-mentioned technical problems in which the prior art has poor effects.

[0010] According to one aspect of the present application, an embodiment provides an ultra-low temperature freezing sample stage, comprising:

[0011] A sample placement box having an opening;

[0012] A refrigeration pipe, fixed in the sample placement box;

[0013] A movable compartment door connected above the sample placement box; and

[0014] A driving device is connected to the movable door and is used to drive the movable door to open and close the opening.

[0015] In one embodiment, the driving device comprises:

[0016] A rotating shaft, rotatably arranged at two ends of the sample placement box;

[0017] A driving wheel coaxially connected to both ends of the rotating shaft; and

[0018] A motor, drivingly connected to the rotating shaft;

[0019] Wherein, synchronously moving driving elements are arranged on both sides of the sample placement box, and the driving elements are sleeved on two driving wheels on the same side; the movable chamber door is connected to the driving elements.

[0020] In one embodiment, the driving device is configured as a chain drive, and the driving element is configured as a driving chain; or

[0021] The driving device is configured as a belt drive, and the driving element is configured as a driving belt; or

[0022] The driving device is configured as a rope transmission, and the driving element is configured as a driving rope.

[0023] In one embodiment, the movable door is configured as a flexible structure; and / or,

[0024] The driving wheel is configured as a gear, and the driving belt is configured as a toothed belt.

[0025] In one embodiment, the driving device comprises:

[0026] A push-pull mechanism, wherein the execution end of the push-pull mechanism is connected to the movable warehouse door.

[0027] In one embodiment, the ultra-low temperature freezing sample stage comprises:

[0028] A warehouse door control system is connected to the driving device.

[0029] According to one aspect of the present application, an embodiment provides an ultra-low temperature freezing platform, comprising: an ultra-low temperature freezing sample stage as described in any one of the above;

[0030] The ultra-low temperature freezing platform further comprises: one or both of a refrigeration device and a drying device; and / or,

[0031] The ultra-low temperature freezing platform also includes: a cold plate;

[0032] Wherein, the refrigeration device is connected to a refrigeration pipeline, and the refrigeration device is used to pass low-temperature cooling liquid into the refrigeration pipeline; the refrigeration device is connected to a control system;

[0033] The drying device is connected to the sample placement box;

[0034] The cold plate is provided with a sample placement hole.

[0035] In one embodiment, the refrigeration device includes a compressor, a condenser, a throttling capillary tube, a stop valve, a temperature control system and an evaporator connected in sequence;

[0036] The drying device comprises a self-pressurizing liquid nitrogen tank; the self-pressurizing liquid nitrogen tank is used to pass dry nitrogen into the sample placement box to prevent moisture from entering the sample placement box when the opening is at least partially opened; and / or the drying device is connected to a dry gas control system; the dry gas control system is connected to the self-pressurizing liquid nitrogen tank and / or the tank valve.

[0037] According to one aspect of the present application, an embodiment provides a pyrolysis analysis collaborative working system, including a pyrolyzer and an ultra-low temperature freezing platform as described above; the ultra-low temperature freezing sample platform supplies samples to the pyrolyzer.

[0038] In one embodiment, the pyrolysis analysis collaborative working system further includes a manipulator; the manipulator is used to take samples from the ultra-low temperature freezing sample table and / or change samples from the pyrolysis instrument.

[0039] The ultra-low temperature freezing sample stage and ultra-low temperature freezing platform of the above-mentioned embodiment of the present application can cooperate with the pyrolysis instrument to perform pyrolysis. Compared with the traditional pyrolysis experiment, the technical solution of the present invention can ensure that the sample to be analyzed by pyrolysis is kept at an ultra-low temperature to avoid the loss of light hydrocarbons, and the use effect is better.

[0040] Compared with the pyrolysis of frozen and sealed crushed samples, the technical solution of the present invention can realize batch analysis of samples in conjunction with a pyrolyzer, greatly improving work efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 The structure diagram of the ultra-low temperature freezing sample stage in one embodiment when the movable chamber door is half open;

[0042] Figure 2 The structure diagram of the ultra-low temperature freezing sample stage in one embodiment when the movable chamber door is fully opened;

[0043] Figure 3 is a schematic diagram of the structure of a cold plate in an embodiment;

[0044] Figure 4 is a schematic structural diagram of a refrigeration device in an embodiment;

[0045] Figure 5 is a schematic diagram of the working process of a pyrolysis analysis collaborative working system in an embodiment;

[0046] Figure 6 The figure is a schematic diagram of the process of manipulator sampling in an embodiment.

[0047] Reference numerals:

[0048] 1-cold plate; 2-sample placement hole; 3-sample placement box; 4-refrigeration pipe; 5-rotating shaft; 6-coolant inlet; 7-coolant outlet; 8-pipe support; 9-gear; 10-toothed belt; 11-movable door; 12-compressor; 13-condenser; 14-throttling capillary; 15-stop valve; 16-temperature control system; 17-evaporator. DETAILED DESCRIPTION

[0049] It should be noted that, in the absence of conflict, the embodiments and features in the embodiments of the present application can be combined with each other. The present application will be described in detail below with reference to the accompanying drawings and in combination with the embodiments.

[0050] In order to enable those skilled in the art to better understand the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only embodiments of a part of the present application, not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in the field without creative work should fall within the scope of protection of the present application.

[0051] It should be noted that the terms "first", "second" etc. in the present application are used to distinguish similar objects, and need not be used to describe a specific order or sequential order. It should be understood that the data used in this way can be interchanged in appropriate circumstances, so that the embodiments of the present application described here. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, the process, method, system, product or equipment comprising a series of steps or units need not be limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or equipment.

[0052] It should be understood that when an element (such as a layer, film, region, or substrate) is described as being "on" another element, the element may be directly on the other element, or there may be an intermediate element. Moreover, in this application, when an element is described as being "connected" to another element, the element may be "directly connected" to the other element, or "connected" to the other element through a third element.

[0053] Embodiment 1

[0054] Please refer to Figure 1-Figure 4 One embodiment provides an ultra-low temperature freezing sample table, including: a sample placement box 3 with an opening, a refrigeration pipe 4 fixed in the sample placement box 3, a movable chamber door 11 connected above the sample placement box 3, and a driving device connected to the movable chamber door 11. The sample can be taken in and out through the opening. The refrigeration pipe 4 is used to cool the sample placement box 3 and provide an ultra-low temperature freezing environment. The driving device is used to drive the movable chamber door 11 to open and close the opening; after the opening is opened, the sample can be taken in and out; after the opening is closed, the sample placement box 3 is in a closed state, and the sample is cryogenically frozen. The sample is generally placed on a cold plate 1. The opening is generally opened at the top of the sample placement box 3 to facilitate the taking in and putting of the sample.

[0055] Regarding the first embodiment of the driving device, the driving device includes: a rotating shaft 5, a driving wheel and a motor. The rotating shaft 5 is rotatably arranged at both ends of the sample placement box 3; the driving wheel is coaxially connected to both ends of the rotating shaft 5; and the motor is connected to the rotating shaft 5. In addition, synchronously moving driving elements are arranged on both sides of the sample placement box 3, and the driving elements are sleeved on two driving wheels on the same side; the mobile warehouse door 11 is connected to the driving element, generally connected to the upper surface of the driving element. The rotating shaft 5 is driven by the motor, and the driving wheel drives the driving element to move; when the driving element moves, the mobile warehouse door 11 is synchronously driven to complete the opening and closing during the movement. The driving elements on both sides of the sample placement box 3 move synchronously, which ensures the stability of the movement of the mobile warehouse door 11.

[0056] In one embodiment, the driving device is configured as a chain drive, and the driving element is configured as a driving chain; or the driving device is configured as a belt drive, and the driving element is configured as a driving belt; or the driving device is configured as a rope drive, and the driving element is configured as a driving rope.

[0057] In the structure of the above-mentioned driving device, preferably, the movable chamber door 11 is set as a flexible structure. It is further preferred that the driving wheel is set as a gear 9, and the driving belt is set as a toothed belt 10. The gear 9 drives the toothed belt 10 to move, and the toothed belt 10 drives the movable chamber door 11 to move. When the movable chamber door 11 moves, the movable chamber door 11 has a flexible structure, and a part or all of the movable chamber door 11 moves to the back of the sample placement box 3. At this time, a part of the opening is opened or all of the openings are opened. Afterwards, the movable chamber door 11 moves in the opposite direction to close the opening.

[0058] Regarding the second embodiment of the driving device, the driving device includes: a push-pull mechanism; the execution end of the push-pull mechanism is connected to the movable door 11. The push-pull mechanism directly pushes the movable door 11 to move to open and close the opening. The push-pull mechanism can be a hydraulic cylinder, a pneumatic cylinder or an electric cylinder. At this time, guiding structures for guiding the movement of the movable door 11 can be set on both sides of the sample placement box 3. After removing the motor from the driving device of the first embodiment, the driving element can realize the function of guiding the movable door 11.

[0059] Regarding the third embodiment of the driving device, the push-pull mechanism of the driving device can also be configured to pull one end of the mobile door 11 to move it; a spring is connected to the other end of the mobile door 11 for resetting the mobile door 11.

[0060] In one embodiment, the ultra-low temperature freezing sample stage includes: a door control system connected to the driving device.

[0061] The ultra-low temperature freezing sample stage of the present invention has a door control system that controls the movement state of the motor. When sampling is required, the motor starts, drives the gear 9 to rotate, and the toothed belt 10 moves and drives the movable door 11 attached to the toothed belt 10 to move, thereby opening the opening. After the movable door 11 moves to an appropriate position, the motor stops working. After the sampling is completed, the motor continues to start reverse rotation, and the movable door 11 moves in the opposite direction until the movable door 11 completely closes the opening.

[0062] The ultra-low temperature freezing sample stage of the present invention can cooperate with the sixth generation HAWK pyrolysis instrument to perform batch freezing pyrolysis, which mainly consists of a cold plate 1 (such as Figure 4) and a sample placement box 3 with heat preservation and / or drying functions. The samples to be analyzed in the pyrolysis experiment are stored in the sample placement box 3, and the samples to be analyzed are kept in an ultra-low temperature environment through a matching refrigeration device to avoid the loss of light hydrocarbons. At the same time, the opening and closing of the sample placement box 3 is controlled by the ultra-low temperature frozen sample batch analysis collaborative platform (ultra-low temperature freezing platform) to cooperate with the pyrolyzer to perform sampling and sample replacement, so as to realize the smooth progress of the batch frozen pyrolysis experiment.

[0063] Embodiment 2

[0064] Please refer to Figure 1-Figure 4 An embodiment provides an ultra-low temperature freezing platform, including an ultra-low temperature freezing sample platform as described in any one of the above embodiments; the ultra-low temperature freezing platform also includes: one or both of a refrigeration device and a drying device; and / or, the ultra-low temperature freezing sample platform also includes: a cold plate 1. The refrigeration device is connected to a refrigeration pipe 4, and the refrigeration device is used to pass a low-temperature coolant into the refrigeration pipe 4; the refrigeration device is connected to a control system. The drying device is connected to the sample placement box 3. A sample placement hole 2 is provided on the cold plate 1.

[0065] The ultra-low temperature freezing sample stage can also be set up as follows.

[0066] In one embodiment, the overall appearance of the ultra-low temperature freezing sample stage is designed as a 280 mm×120 mm cuboid. The overall design meets the strict small volume requirement to cope with the narrow space.

[0067] In one embodiment, in the ultra-low temperature freezing sample table, the cold plate 1 has a total of 4×5 sample placement holes 2. Preferably, the cold plate 1 has a size of 280mm×120mm. The external refrigerant circulation of the 4×5 sample placement holes 2 can maintain a low temperature environment of -40°C to achieve sample freezing. The sample placement box 3 is grooved around to form a box body, and a sealing mechanism that can automatically open and close the opening is set on the top. The freeze-drying storage of the sample can be achieved, and it can work in conjunction with the pyrolysis instrument.

[0068] In one embodiment, the sample placement box 3 is set as a heat preservation drying box, the overall appearance is a rectangular parallelepiped, and it is made of heat preservation material, wherein the heat preservation drying shell can realize the freeze-drying storage of the sample and adapt to the narrow space. The heat preservation drying box is made of high-performance insulation material as a whole, which further prevents heat transfer and isolates the air. Furthermore, gears 9 and toothed belts 10 are provided on both sides of the heat preservation drying box, and the gears 9 rotate under the drive of the motor to drive the toothed belt 10 to move. At the same time, a flexible rolling door is installed on the toothed belt 10, and the flexible rolling door moves with the movement of the toothed belt 10; the flexible rolling door acts as a mobile warehouse door 11, which can realize the opening and closing. Among them, part or all of the flexible rolling door moves to the back of the sample placement box 3 to ensure that the opening is fully opened. The flexible rolling door can be designed as a rolling door, which is a thin layer of heat-insulating and easy-to-roll material to reduce the space occupancy rate. Among them, the motor that controls the opening and closing of the mobile warehouse door 11 has a control accuracy of up to ±1mm.

[0069] In addition, the heat-insulating drying box is externally connected to a drying device (self-pressurizing liquid nitrogen tank) to further cool and dry the environment inside the tooling box (sample placement box 3). Specifically, in one embodiment, the drying device includes a self-pressurizing liquid nitrogen tank; the self-pressurizing liquid nitrogen tank is used to pass dry nitrogen into the sample placement box 3 when the opening is at least partially opened to prevent moisture from entering the sample placement box 3; and / or, the drying device is connected to a dry gas control system; the dry gas control system is connected to the self-pressurizing liquid nitrogen tank and / or the tank valve. The dry gas control system controls the switch state of the valve of the self-pressurizing liquid nitrogen tank. When the door control system is started so that the mobile door 11 is in a non-fully closed state, the valve opens, and dry nitrogen is continuously passed into the plane where the mobile door 11 is located to prevent moisture in the external environment from entering the heat-insulating drying box.

[0070] In one embodiment, a cooling pipe and a pipe bracket 8 are installed inside the heat-insulating drying box. Low-temperature coolant flows in from the coolant inlet 6 and flows out from the coolant outlet 7. The coolant circulates in the heat-insulating drying box along the refrigeration pipe 4 to achieve a low-temperature environment inside the heat-insulating drying box.

[0071] In one embodiment, the refrigeration device comprises a compressor 12, a condenser 13, a throttling capillary 14, a stop valve 15, a temperature control system 16 and an evaporator 17 connected in sequence. The refrigeration device realizes a continuous supply of low-temperature coolant to the refrigeration pipeline 4.

[0072] In one embodiment, the temperature control system 16 includes a temperature sensor. When the temperature exceeds -40 degrees Celsius, the temperature sensor senses the temperature rise and flips a switch to convert the disconnected circuit in the temperature control system 16 into a smooth circuit, and starts the refrigeration device to cool the sample placement box 3 (insulated drying box).

[0073] Compared with an electrically operated low-temperature protection device (application number CN202120318388.5) in the prior art, the ultra-low temperature freezing platform of the present invention is controlled by the door control system to open and close the mobile door 11 so as to cooperate with the pyrolyzer; the mobile door 11 is made of flexible material and can achieve continuous changes from fully closed to fully open; the mobile door 11 fits tightly with the sample placement box 3, and changes in the external environment have little effect on the environment inside the box; it is dried by dry nitrogen and is not connected to the outside, further ensuring the overall sealing performance.

[0074] The ultra-low temperature freezing platform of the present invention is compared with the double-head insulation box for low-temperature CTOD test in the prior art (application number CN201610330783.9). The coolant is injected into the refrigeration pipe 4 for refrigeration through the refrigeration device to maintain the low temperature state of the entire sample placement box 3, and the low temperature state of the sample placement box 3 can be maintained as long as the refrigeration device continues to work. It can cooperate with the pyrolyzer. When the pyrolyzer is working, the door control system controls the flexible rolling door to open, and the low-temperature dry gas is ejected, which can ensure that the interior of the sample placement box 3 is always in a low-temperature dry state, and the mobile door 11 remains closed in the non-working state to further improve the insulation and drying effect.

[0075] Compared with a vacuum system for a vacuum freeze dryer in the prior art (application number CN202121119381.7), the ultra-low temperature freezing platform of the present invention is controlled by the door control system to open and close the movable door 11 so as to cooperate with the pyrolyzer; the drying work is realized by the self-pressurized liquid nitrogen tank; when working, the inside of the sample placement box 3 is sealed and maintains low temperature drying without vacuum; the working state of the entire ultra-low temperature freezing sample platform is uniformly controlled by the control system, and no additional manual intervention is required.

[0076] Compared with a multifunctional heating and cooling insulation box (application number CN202120764579.4) in the prior art, the ultra-low temperature freezing platform of the present invention is realized by an external professional refrigeration device, which can reach a lower temperature; it can only cool but not heat; the heat dissipation during cooling is realized by a professional evaporator 17.

[0077] Compared with the existing small and medium-sized low-temperature biological freezer (application number CN200420017227.9), the ultra-low temperature freezing platform of the present invention adopts a refrigeration method of injecting coolant into the refrigeration pipe 4 (condenser) for refrigeration, which can maintain the low temperature environment inside the entire sample placement box 3; the refrigeration efficiency is average, but the environment inside the entire sample placement box 3 can be maintained at -40°C for a long time.

[0078] Embodiment 3

[0079] Please refer to Figure 1-Figure 5One embodiment provides a pyrolysis analysis collaborative working system, including a pyrolyzer and an ultra-low temperature freezing platform as described in any one of the above embodiment 2; the ultra-low temperature freezing sample station supplies samples to the pyrolyzer. Among them, the freezing sample station works in conjunction with the pyrolyzer, which can effectively avoid the loss of light hydrocarbons in the sample to be analyzed during pyrolysis analysis, and will not affect the batch pyrolysis analysis of the pyrolyzer. Preferably, the ultra-low temperature freezing sample station (ultra-low temperature freezing platform) can cooperate with the sixth-generation HAWK pyrolyzer to perform batch frozen pyrolysis.

[0080] In one embodiment, the pyrolysis analysis collaborative working system further includes a manipulator; the manipulator is used to take samples from the ultra-low temperature freezing sample stage and / or change samples from the pyrolysis instrument. Figure 6 , Figure 6 This reflects the workflow of the manipulator taking samples in cooperation with the mobile door, refrigeration device and drying device.

[0081] In one embodiment, there is provided Figure 5 , Figure 5 This reflects the workflow of the pyrolysis analysis collaborative system for pyrolysis analysis of the sample to be tested.

[0082] In one embodiment, the following takes the testing and research on fresh samples from a certain company's Haiye 1 well as an example to illustrate the working conditions of the pyrolysis analysis collaborative working system of the present invention.

[0083] (1) Obtain fresh shale samples at the Haiye 1 shale oil exploration well site.

[0084] (2) The sample placement box 3 is cooled to below -40°C by a refrigeration device.

[0085] (3) After the samples are frozen in liquid nitrogen, they are all placed in an ultra-low temperature freezing sample table.

[0086] (4) When the pyrolyzer is executing the analysis program, the opening of the ultra-low temperature freezing sample stage is closed, so that the sample to be analyzed is kept in an ultra-low temperature state to avoid the loss of light hydrocarbons.

[0087] (5) When the pyrolyzer executes the sample changing procedure, the opening of the ultra-low temperature freezing sample table is opened, and the robot arm of the pyrolyzer is used to perform sampling and sample changing. After the sampling is completed, the opening of the ultra-low temperature freezing sample table is closed, and the refrigeration device and the drying device cool down and dry the sample placement box 3.

[0088] (6) Compare the batch cryo-pyrolysis results with the single cryo-pyrolysis analysis results to ensure the accuracy of the results.

[0089] The above description is only the preferred embodiment of the present application and is not intended to limit the present application. For those skilled in the art, the present application may have various modifications and variations. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. An ultra-low temperature freezing sample stage, characterized in that: include: A sample placement box having an opening; A refrigeration pipe, fixed in the sample placement box; A movable door is connected above the sample placement box; and A driving device is connected to the movable door and is used to drive the movable door to open and close the opening.

2. The ultra-low temperature freezing sample stage according to claim 1, characterized in that: The driving device comprises: A rotating shaft, rotatably arranged at two ends of the sample placement box; A driving wheel coaxially connected to both ends of the rotating shaft; and A motor, drivingly connected to the rotating shaft; Wherein, synchronously moving driving elements are arranged on both sides of the sample placement box, and the driving elements are sleeved on two driving wheels on the same side; the movable chamber door is connected to the driving elements.

3. The ultra-low temperature freezing sample stage according to claim 2, characterized in that: The driving device is configured as a chain drive, and the driving element is configured as a driving chain; or The driving device is configured as a belt drive, and the driving element is configured as a driving belt; or The driving device is configured as a rope transmission, and the driving element is configured as a driving rope.

4. An ultra-low temperature freezing sample stage according to claim 2 or 3, characterized in that: The movable door is configured as a flexible structure; and / or, The driving wheel is configured as a gear, and the driving belt is configured as a toothed belt.

5. The ultra-low temperature freezing sample stage according to claim 1, characterized in that: The driving device comprises: A push-pull mechanism, wherein the execution end of the push-pull mechanism is connected to the movable warehouse door.

6. The ultra-low temperature freezing sample stage according to claim 1, characterized in that: The ultra-low temperature freezing sample stage comprises: A warehouse door control system is connected to the driving device.

7. An ultra-low temperature freezing platform, characterized in that: include: The ultra-low temperature freezing sample stand according to any one of claims 1 to 6; The ultra-low temperature freezing platform further comprises: one or both of a refrigeration device and a drying device; and / or, The ultra-low temperature freezing platform also includes: a cold plate; Wherein, the refrigeration device is connected to a refrigeration pipeline, and the refrigeration device is used to pass low-temperature cooling liquid into the refrigeration pipeline; the refrigeration device is connected to a control system; The drying device is connected to the sample placement box; The cold plate is provided with a sample placement hole.

8. The ultra-low temperature freezing platform according to claim 7, characterized in that: The refrigeration device comprises a compressor, a condenser, a throttling capillary tube, a stop valve, a temperature control system and an evaporator which are connected in sequence; The drying device comprises a self-pressurizing liquid nitrogen tank; the self-pressurizing liquid nitrogen tank is used to pass dry nitrogen into the sample placement box to prevent moisture from entering the sample placement box when the opening is at least partially opened; and / or the drying device is connected to a dry gas control system; the dry gas control system is connected to the self-pressurizing liquid nitrogen tank and / or the tank valve.

9. A pyrolysis analysis collaborative working system, characterized in that: It comprises a pyrolyzer and an ultra-low temperature freezing platform as described in claim 7 or 8; the ultra-low temperature freezing sample stage supplies samples to the pyrolyzer.

10. A pyrolysis analysis collaborative working system according to claim 9, characterized in that: The pyrolysis analysis collaborative working system also includes a manipulator; the manipulator is used to take samples from the ultra-low temperature freezing sample stage and / or change samples from the pyrolysis instrument.

Citation Information

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