Device for measuring internal temperature of autoclave

By installing three K-type thermocouples and capillary pipes in the autoclave, the problem that the prior art cannot accurately measure the internal temperature of the autoclave and ignore the temperature gradient is solved, and the accurate measurement of the internal temperature of the autoclave and the accurate recording of the temperature gradient are achieved, and the quality of the experimental data is improved.

CN222912914UActive Publication Date: 2025-05-27CHINA UNIV OF GEOSCIENCES (WUHAN)
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Patent Information

Application Number
CN202422042425.0
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-08-21
Publication Date
2025-05-27
Estimated Expiration
2034-08-21

AI Technical Summary

Technical Problem

When measuring the temperature of a fast quenching cold seal autoclave, the prior art cannot accurately reflect the actual temperature inside the autoclave, and ignores the temperature gradient differences caused by different heights of the sample chamber.

Method used

A device including three K-type thermocouples is designed, which is placed in the autoclave cavity and the kettle body respectively. The distilled water is pressurized into the autoclave cavity through a capillary pipe to achieve accurate measurement of the internal temperature of the autoclave, and the temperature gradient of the sample chamber is measured by thermocouples of different heights.

Benefits of technology

The accurate measurement of the internal temperature of the fast quenching cold seal autoclave is achieved, which can effectively reflect the real temperature inside the autoclave and accurately record the temperature gradient of the sample chamber at different heights, improving the quality of the experimental data.

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Abstract

The utility model discloses a device for measuring the internal temperature of an autoclave, which relates to the technical field of high-temperature and high-pressure experiment earth science and comprises an air compressor, a water pump, a water tank, a pressure release valve, a main valve, a capillary water pipe, a K-type thermocouple I, a K-type thermocouple II and a K-type thermocouple III. Wherein the air compressor is connected with the water pump through a pipeline, and a valve is arranged on the pipeline; the water pump is connected with the water tank through a pipeline; the water pump is further connected with a pressure release valve and a main valve through a tee joint; the other end of the main valve is connected with a capillary water pipe; the K-type thermocouple I and the K-type thermocouple II are both arranged in the autoclave cavity; and the K-type thermocouple III is arranged in the autoclave body. According to the utility model, the temperature measurement upgrading design of the rapid quenching and cold sealing type autoclave is planned, the internal temperature of the rapid quenching and cold sealing type autoclave and the temperature gradient of the sample bin at different heights can be accurately measured after improvement, and the device has positive significance for experimental research.
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Description

Technical Field

[0001] The utility model relates to the technical field of high-temperature and high-pressure experimental geoscience, and particularly relates to a device for measuring the temperature inside an autoclave. Background Art

[0002] The deep earth is the driving force for the operation of the entire earth system and also plays a very crucial role in surface evolution and geological disasters. Currently, drilling and high-temperature and high-pressure experiments are the main research methods. Drilling can directly observe and sample the deep earth. However, due to the high difficulty and cost, the drilling depth has always been very limited. In contrast, high-temperature and high-pressure experiments can achieve higher temperature and pressure conditions, so high-temperature and high-pressure experimental research in the field of earth science occupies an important position.

[0003] The technology of high-temperature and high-pressure experiments has developed rapidly, and various experimental devices such as autoclaves and diamond anvil cells have been developed. Currently, the rapidly quenched cold-sealed autoclave is widely used. Temperature and pressure are the two most important indicators in high-temperature and high-pressure experiments. Therefore, it is particularly important to obtain accurate temperature and pressure information in the rapidly quenched cold-sealed autoclave.

[0004] As a widely used high-temperature and high-pressure device, the rapidly quenched cold-sealed autoclave plays a key role in deep-earth simulation experiments. Precise temperature measurement is a key step in high-temperature and high-pressure experiments and will directly affect the quality of experimental data. Currently, in the temperature measurement of the rapidly quenched cold-sealed autoclave, a K-type thermocouple is mainly used externally for temperature measurement.

[0005] The existing temperature control and monitoring have the following limitations:

[0006] First, although the external thermocouple is easy to implement, the measured temperature can only indicate the external temperature of the autoclave and cannot represent the actual temperature inside the autoclave.

[0007] Second, the external thermocouple can only obtain one temperature and ignores the temperature gradient difference caused by the different heights of the sample chamber itself. Summary of the Utility Model

[0008] Predecessors used an external thermocouple to measure the temperature of the rapidly quenched cold-sealed autoclave and regarded it as the internal temperature of the rapidly quenched cold-sealed autoclave. However, this method ignores the difference between the internal and external temperatures and has a greater impact on the experimental results. Therefore, the purpose of the utility model is to provide a device for measuring the internal temperature of the autoclave, which can accurately measure the internal temperature of the rapidly quenched cold-sealed autoclave and the temperature gradient existing at different heights of the sample chamber, and has positive significance for experimental research. To achieve the above purpose, the utility model provides the following technical solutions:

[0009] The present utility model provides a device for measuring the internal temperature of an autoclave. The device includes: an air compressor, a water pump, a water tank, a pressure relief valve, a main valve, a capillary water pipe, a Type K thermocouple I, a Type K thermocouple II, and a Type K thermocouple III; wherein,

[0010] The air compressor is connected to the water pump through a pipeline, and a valve is provided on this pipeline;

[0011] The water pump is connected to the water tank through a pipeline;

[0012] The water pump is also connected to the pressure relief valve and the main valve through a tee joint;

[0013] The other end of the main valve is connected to a capillary water pipe;

[0014] Both the Type K thermocouple I and the Type K thermocouple II are arranged inside the autoclave cavity;

[0015] The Type K thermocouple III is arranged inside the autoclave body.

[0016] As a preferred embodiment, the outer diameter of the capillary water pipe is based on being able to pass through the hole positions opened on the conical plug, and distilled water is used as the medium to enter the autoclave cavity through the capillary water pipe for pressure increase.

[0017] As a preferred embodiment, the Type K thermocouple I, the Type K thermocouple II, and the Type K thermocouple III are all the same type of thermocouple, and are all made of nickel-chromium - nickel-aluminum material.

[0018] As a preferred embodiment, the diameter of the Type K thermocouple I is based on being able to just pass through the hole positions opened on the conical plug, and the length ensures that its temperature measurement point is located at the top of the autoclave cavity, with an accuracy of Class II ±0.75%.

[0019] As a preferred embodiment, the diameter of the Type K thermocouple II is based on being able to just pass through the hole positions opened on the conical plug, and the length ensures that the height difference between its temperature measurement point and the temperature measurement point of the Type K thermocouple I is not less than the maximum sample height, with an accuracy of Class II ±0.75%.

[0020] As a preferred embodiment, the diameter of the Type K thermocouple III is based on being able to be inserted into the hole on the outer wall of the autoclave body, with an accuracy of Class II ±0.75%.

[0021] As a preferred embodiment, the sample height is 2 - 4 cm.

[0022] As a preferred embodiment, the autoclave includes: an autoclave body, a nut, a conical plug, and an autoclave cavity; wherein, three hole positions are opened on the conical plug, distributed in a triangular shape, and are respectively used for passing through the Type K thermocouple I, the Type K thermocouple II, and the capillary water pipe.

[0023] As a preferred embodiment, the Type K thermocouple I, Type K thermocouple II, and Type K thermocouple III are all connected to the temperature display panel for real-time display of the measured temperature on the temperature display panel.

[0024] Technical effects and advantages of the present utility model:

[0025] The present utility model intends to upgrade the temperature measurement design of the rapid quenching and cold-sealing autoclave. After improvement, it can accurately measure the internal temperature of the rapid quenching and cold-sealing autoclave and the temperature gradient existing at different heights in the sample chamber, which has positive significance for experimental research.

[0026] Other features and advantages of the present utility model will be described in the subsequent description, and part of them will be obvious from the description or understood by implementing the present utility model. The objectives and other advantages of the present utility model can be achieved and obtained through the structures pointed out in the description, claims, and drawings. Description of the Drawings

[0027] Figure 1 It is an overall schematic diagram of a device for measuring the internal temperature of an autoclave according to the present utility model;

[0028] Figure 2 It is a front view and bottom view schematic diagram of a device for measuring the internal temperature of an autoclave according to the present utility model;

[0029] Figure 3 It is a temperature trend diagram measured before calibration of three Type K thermocouples according to the present utility model;

[0030] Figure 4 It is a temperature trend diagram measured after calibration of three Type K thermocouples according to the present utility model;

[0031] Reference numerals: 1, air compressor; 2, valve; 3, water pump; 4, water tank; 5, tee; 6, pressure relief valve; 7, main valve; 8, capillary water pipe; 9, Type K thermocouple I; 10, Type K thermocouple II; 11, Type K thermocouple III; 12, autoclave body; 13, nut; 14, conical plug; 15, autoclave cavity; 16, ring-shaped electric furnace. Detailed Embodiments

[0032] Next, the technical solutions in the embodiments of the present utility model will be clearly and completely described in conjunction with the drawings in the embodiments of the present utility model. Obviously, the described embodiments are only part of the embodiments of the present utility model, rather than all the embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present utility model.

[0033] To solve the deficiencies of the prior art, the present utility model discloses a device for measuring the internal temperature of an autoclave. Figure 1 The overall schematic diagram of a device for measuring the internal temperature of an autoclave according to the present utility model is shown in Figure 1 As shown, the device includes: an air compressor 1, a water pump 3, a water tank 4, a pressure relief valve 6, a main valve 7, a capillary water pipe 8, a K-type thermocouple I 9, a K-type thermocouple II 10, and a K-type thermocouple III 11; among them,

[0034] The air compressor 1 is connected to the water pump 3 through a pipeline, and a valve 2 is provided on this pipeline;

[0035] The water pump 3 is connected to the water tank 4 through a pipeline;

[0036] The water pump 3 is also connected to the pressure relief valve 6 and the main valve 7 through a tee;

[0037] The other end of the main valve 7 is connected to a capillary water pipe 8, and the capillary water pipe 8 passes through the conical plug 14 of the autoclave;

[0038] The K-type thermocouple I 9 and the K-type thermocouple II 10 are both arranged inside the autoclave cavity 15;

[0039] The K-type thermocouple III 11 is arranged inside the autoclave body 12;

[0040] Furthermore, the capillary water pipe 8 is connected to the main pipeline, and its outer diameter is such that it can just pass through the hole provided on the conical plug 14, and distilled water is used as the medium to enter the autoclave cavity 15 through the capillary water pipe 8 for pressurization;

[0041] Furthermore, the K-type thermocouple I 9, the K-type thermocouple II 10, and the K-type thermocouple III 11 are all of the same type of thermocouple, and are all made of nickel-chromium - nickel-aluminum material. Among them, the diameter of the K-type thermocouple I 9 is such that it can just pass through the hole provided on the conical plug 14, and the length ensures that its temperature measurement point is located at the top of the autoclave cavity 15, and the accuracy is within its own accuracy range, that is, the accuracy is Class II ±0.75%; the diameter of the K-type thermocouple II 10 is also such that it can just pass through the hole provided on the conical plug 14, and the length ensures that the height difference between its temperature measurement point and the temperature measurement point of the K-type thermocouple I 9 is not less than the sample height, where the sample height is 2 - 4 cm, and the accuracy is within its own accuracy range, that is, the accuracy is Class II ±0.75%; the diameter of the K-type thermocouple III 11 is such that it can be inserted into the hole on the outer wall of the autoclave body 12, and the accuracy is within its own accuracy range, that is, the accuracy is Class II ±0.75%, and its length has no special requirements.

[0042] Figure 2 The front and bottom schematic diagrams of a device for measuring the internal temperature of an autoclave according to the present utility model are shown inFigure 2 As shown in the figure, the autoclave includes: an autoclave body 12, a nut 13, a conical plug 14, and a high-temperature autoclave cavity 15. Among them, on the basis of only one hole being opened on the original conical plug 14, two more holes are opened, and the three holes are distributed in a triangle, which are respectively used to pass through the K-type thermocouple I 9, the K-type thermocouple II 10, and the capillary water pipe 8, and the parts in contact with the bottom of the conical plug 14 are welded to ensure sealing. The two K-type thermocouples are connected to the temperature display panel, and the measured temperature can be displayed in real time. Place the conical plug 14 inside the nut 13. Both the nut 13 and the lower part of the autoclave body 12 have threads. During the tightening process, the conical plug 14 contacts and presses against the lower opening of the autoclave body 12 to achieve a sealing effect. Conduct a simple test on the accuracy of the K-type thermocouple I 9 and the K-type thermocouple II 10, that is, pinch the temperature measurement areas of the two thermocouples by hand and wait for them to stabilize. If both thermocouples display 38.1 °C, it can be considered that the accuracy of the two thermocouples is reliable.

[0043] Based on the above device, the present utility model also discloses a method for measuring the internal temperature of an autoclave, and the method includes the following steps:

[0044] Step S1, temperature monitoring during the heating process:

[0045] Step S11, put the K-type thermocouple I 9 and the K-type thermocouple II 10 with different lengths into the autoclave body 12 and tighten the nut 13 to make the conical plug 14 contact and seal with the bottom of the autoclave body 12. Place an external K-type thermocouple III 11 with a different specification, and fill the water tank 4 with distilled water.

[0046] Step S12, start the air compressor 1, open the valve 2 and the pressure relief valve 6, close the main valve 7, and discharge the air in the water pump 3.

[0047] Step S13, close the pressure relief valve 6, open the main valve 7, input distilled water into the autoclave body 12 through the capillary water pipe 8, and pressurize the autoclave cavity 15 to an appropriate value. For example, when the target pressure is set to 200 MPa, the appropriate value is about 100 MPa.

[0048] Step S14, insert the upper part of the autoclave body 12 into the ring-shaped electric furnace 16, and heat the autoclave cavity 15 through the ring-shaped electric furnace 16. The tops of the three K-type thermocouples are the temperature measurement points. Connect the three K-type thermocouples to the temperature display panel, and the measured temperature can be displayed in real time on the temperature display panel. During the heating process, the internal and external temperatures of the autoclave cavity 15 can be monitored through the three K-type thermocouples, and the internal temperature of the autoclave cavity 15 can be adjusted to the target temperature by adjusting the temperature of the ring-shaped electric furnace 16.

[0049] Step S2, temperature monitoring during the experiment:

[0050] Step S21: After the temperature increase process ends, close the main valve 7. At this time, the temperatures shown by the K-type thermocouple I 9 and the K-type thermocouple II 10 are the temperatures inside the autoclave cavity 15, and the temperature shown by the K-type thermocouple III 11 is the temperature outside the autoclave cavity 15.

[0051] Step S22: Regularly read the temperatures of the three K-type thermocouples and record them until the experiment ends.

[0052] That is, record the data once when the temperatures of the three thermocouples are relatively stable. After that, the temperature will fluctuate up and down within a small range, and then the data can be recorded once every half hour.

[0053] Step S3: Record and export the temperature data:

[0054] The temperature display panel can record the temperature data of the three thermocouples in real time and has functions such as generating a temperature change curve. After the experiment ends, the temperature data can be exported using a USB flash drive for further analysis. The main advantages of this device are as follows: First, the K-type thermocouple in the autoclave can reflect the real temperature inside the autoclave. Second, the two K-type thermocouples at different heights can reflect the temperature gradient generated due to the height of the sample chamber itself.

[0055] Example:

[0056] Before temperature correction, after operating according to the above technical solution, the obtained temperature data is shown in Table 1 below.

[0057] Table 1 Temperature Record Table before Correction

[0058]

[0059] After replacing the ring-shaped electric furnace 16 and changing the temperature zone of the ring-shaped electric furnace 16, the obtained temperature record is shown in Table 2 below.

[0060] Table 2 Temperature Record Table after Correction

[0061]

[0062] In Table 1 and Table 2, the furnace temperature is the temperature of the ring-shaped electric furnace 16, the autoclave temperature is the temperature measured by the K-type thermocouple III 11, the upper temperature is the temperature measured by the K-type thermocouple II 10, the lower temperature is the temperature measured by the K-type thermocouple I 9, and the pressure is the internal pressure of the autoclave cavity 15.

[0063] Figure 3 This is the temperature trend chart measured by the three K-type thermocouples of the present invention before correction, Figure 4 This is the temperature trend chart measured by the three K-type thermocouples of the present invention after correction. By comparing Table 1, Table 2, and Figure 3 and Figure 4It can be clearly seen that, compared with before calibration, the difference between the upper temperature and the lower temperature is significantly reduced. When the autoclave temperature is 800 °C, the internal temperature gradient of the autoclave cavity 15 after calibration can be ensured to be about 5 °C, and the temperature calibration effect is obvious.

[0064] Finally, it should be noted that the above are only the preferred embodiments of the present invention and are not used to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A device for measuring the internal temperature of an autoclave, characterized in that The device comprises: an air compressor (1), a water pump (3), a water tank (4), a pressure relief valve (6), a main valve (7), a capillary water tube (8), a K-type thermocouple I (9), a K-type thermocouple II (10) and a K-type thermocouple III (11); wherein: The air compressor (1) is connected to the water pump (3) via a pipeline, and a valve (2) is provided on the pipeline; The water pump (3) is connected to the water tank (4) via a pipeline; The water pump (3) is also connected to the pressure relief valve (6) and the main valve (7) via a three-way connection; The other end of the main valve (7) is connected to a capillary water tube (8); The K-type thermocouple I (9) and the K-type thermocouple II (10) are both arranged in the autoclave cavity (15); The K-type thermocouple III (11) is arranged in the autoclave body (12).

2. The device for measuring the internal temperature of an autoclave according to claim 1, characterized in that: The outer diameter of the capillary water tube (8) is determined to be able to pass through the hole opened on the conical plug (14), and distilled water is used as a medium to enter the autoclave cavity (15) through the capillary water tube (8) for pressurization.

3. A device for measuring the internal temperature of an autoclave according to claim 1 or 2, characterized in that: The K-type thermocouple I (9), K-type thermocouple II (10) and K-type thermocouple III (11) are all thermocouples of the same type and are all made of nickel-chromium-nickel-aluminum material.

4. The device for measuring the internal temperature of an autoclave according to claim 3, characterized in that: The diameter of the K-type thermocouple I (9) is such that it can just pass through the hole opened on the conical plug (14), and the length ensures that its temperature measurement point is located at the top of the autoclave cavity (15), with an accuracy of Class II ±0.75%.

5. The device for measuring the internal temperature of an autoclave according to claim 3, characterized in that: The diameter of the K-type thermocouple II (10) is such that it can just pass through the hole opened on the conical plug (14), and the length ensures that the height difference between its temperature measuring point and the temperature measuring point of the K-type thermocouple I (9) is not less than the sample height, and the accuracy is level II ±0.75%.

6. The device for measuring the internal temperature of an autoclave according to claim 3, characterized in that: The diameter of the K-type thermocouple III (11) is such that it can be inserted into the hole on the outer wall of the autoclave body (12), and the accuracy is grade II ±0.75%.

7. The device for measuring the internal temperature of an autoclave according to claim 5, characterized in that: The sample height is 2 to 4 cm.

8. The device for measuring the internal temperature of an autoclave according to claim 1, characterized in that: The autoclave comprises: an autoclave body (12), a nut (13), a conical plug (14), and an autoclave cavity (15); wherein the conical plug (14) is provided with three holes distributed in a triangular shape, which are used to pass a K-type thermocouple I (9), a K-type thermocouple II (10), and a capillary water tube (8), respectively.

9. The device for measuring the internal temperature of an autoclave according to claim 1, characterized in that: The K-type thermocouple I (9), K-type thermocouple II (10) and K-type thermocouple III (11) are all connected to a temperature display panel and are used to display the measured temperature in real time on the temperature display panel.