Device and method for measuring internal temperature of autoclave

Abstract

The invention discloses a device and method for measuring the internal temperature of an autoclave, and relates to the technical field of high-temperature and high-pressure experiment earth science, and the device 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 invention, the temperature measurement upgrading design of the rapid quenching and cold sealing type high-pressure kettle is planned, the internal temperature of the rapid quenching and cold sealing type high-pressure kettle and the temperature gradient existing at different heights of the sample bin can be accurately measured after improvement, and positive significance is provided for experimental research.

Description

Technical Field

[0001] This invention relates to the field of high-temperature and high-pressure experimental geoscience technology, and in particular to an apparatus and method for measuring the internal temperature of a high-pressure reactor. Background Technology

[0002] The Earth's deep interior is the driving force behind the entire Earth system's operation and plays a crucial role in geological changes and disasters. Currently, drilling and high-temperature, high-pressure (HTHP) experiments are the main research methods. Drilling allows for direct observation and sampling of the Earth's deep interior; however, due to its difficulty and high cost, the depth of drilling has always been very limited. In contrast, HTHP experiments can achieve much higher temperature and pressure conditions, thus occupying an important position in HTHP research within the field of Earth sciences.

[0003] High-temperature and high-pressure experimental technology has developed rapidly, and various experimental devices such as autoclaves and diamond pressure chambers have been developed. Currently, the most widely used is the rapid quenching and cold-sealing autoclave. Temperature and pressure are the two most important indicators in high-temperature and high-pressure experiments, therefore obtaining accurate temperature and pressure information in the rapid quenching and cold-sealing autoclave is particularly important.

[0004] Rapid quenching and cold-sealing autoclaves, as widely used high-temperature and high-pressure equipment, play a crucial role in deep Earth simulation experiments. Accurate temperature measurement is a critical step in high-temperature and high-pressure experiments, directly affecting the quality of experimental data. Currently, temperature measurement in rapid quenching and cold-sealing autoclaves primarily employs an external K-type thermocouple.

[0005] Existing temperature control and monitoring methods have the following limitations:

[0006] First, although external thermocouples are easy to implement, the measured temperature can only indicate the external temperature of the autoclave and cannot represent the actual internal temperature of the autoclave.

[0007] Second, external thermocouples can only obtain one temperature, ignoring the temperature gradient differences caused by the different heights of the sample chamber itself. Summary of the Invention

[0008] Previous researchers used external thermocouples to measure the temperature of a rapid quenching and cold-sealing autoclave, and took this as the internal temperature of the autoclave. However, this method ignores the temperature difference between the inside and outside, which significantly affects the experimental results. Therefore, the purpose of this invention is to provide a device for measuring the internal temperature of an autoclave, which can accurately measure the internal temperature of a rapid quenching and cold-sealing autoclave, as well as the temperature gradient existing at different heights of the sample chamber, which is of positive significance for experimental research. To achieve the above objective, this invention provides the following technical solution:

[0009] The present invention provides a device for measuring the internal temperature of an autoclave, the device comprising: an air compressor, a water pump, a water tank, a pressure relief valve, a main valve, a capillary tube, and K-type thermocouple I, K-type thermocouple II, and K-type thermocouple III;

[0010] in,

[0011] The air compressor is connected to the water pump via a pipe, and a valve is installed on the pipe.

[0012] The water pump is connected to the water tank via a pipe;

[0013] The water pump is also connected to the pressure relief valve and the main valve via a tee.

[0014] The other end of the main valve is connected to a capillary water pipe;

[0015] Both type K thermocouple I and type K thermocouple II are installed inside the autoclave cavity;

[0016] The K-type thermocouple III is installed inside the high-pressure autoclave.

[0017] As a preferred embodiment, the outer diameter of the capillary tube is determined by the hole opened on the conical plug, and distilled water is used as the medium to enter the high-pressure reactor cavity through the capillary tube for pressurization.

[0018] As a preferred embodiment, the K-type thermocouple I, K-type thermocouple II, and K-type thermocouple III are all of the same type and are all made of nickel-chromium-nickel-aluminum material.

[0019] As a preferred embodiment, the diameter of the K-type thermocouple I is such that it can just pass through the hole opened on the conical plug, and the length ensures that its temperature measuring point is located at the top of the autoclave cavity, with an accuracy of Class II ±0.75%.

[0020] As a preferred embodiment, the diameter of the K-type thermocouple II is determined so that it can just pass through the hole opened on the conical plug, and the length ensures that the height difference between its temperature measuring point and the temperature measuring point of the K-type thermocouple I is not less than the sample height, with an accuracy of Class II ±0.75%.

[0021] As a preferred embodiment, the diameter of the K-type thermocouple III is determined by its ability to be inserted into a hole on the outer wall of the autoclave, and its accuracy is Class II ±0.75%.

[0022] As a preferred embodiment, the sample height is 2-4 cm.

[0023] As a preferred embodiment, the autoclave includes: an autoclave body, a nut, a conical plug, and an autoclave cavity; wherein, the conical plug has three holes arranged in a triangle, which are respectively used for passing through a K-type thermocouple I, a K-type thermocouple II, and a capillary tube.

[0024] In a preferred embodiment, the K-type thermocouple I, K-type thermocouple II, and K-type thermocouple III are all connected to a temperature display panel for real-time display of the measured temperature on the temperature display panel.

[0025] The present invention also provides a method for measuring the internal temperature of an autoclave, the method comprising the following steps:

[0026] Step S1: Temperature monitoring during the heating process:

[0027] Step S11: Assemble the device as described above;

[0028] Step S12: Start the air compressor of the above device, open the valve and the pressure relief valve, close the main valve, and discharge the air from the water pump;

[0029] Step S13: Close the pressure relief valve, open the main valve, and input distilled water into the autoclave body through the capillary tube 8 to pressurize the autoclave cavity;

[0030] Step S14: Insert the upper part of the autoclave body into the annular electric furnace and heat the autoclave cavity through the annular electric furnace;

[0031] Step S2, Temperature monitoring during the experiment:

[0032] Step S21: After the heating process is completed, close the main valve. At this time, the temperature displayed by K-type thermocouple I and K-type thermocouple II is the temperature inside the pressure vessel cavity, and the temperature displayed by K-type thermocouple III is the temperature outside the pressure vessel cavity.

[0033] Step S22: Periodically read and record the temperatures of the three K-type thermocouples until the experiment ends;

[0034] Step S3: Record and export temperature data.

[0035] The technical effects and advantages of this invention are as follows:

[0036] This invention proposes an upgraded design for temperature measurement in a rapid quenching and cold-sealing autoclave. The improved design can accurately measure the internal temperature of the rapid quenching and cold-sealing autoclave, as well as the temperature gradient at different heights of the sample chamber, which is of positive significance for experimental research.

[0037] Other features and advantages of the invention will be set forth in the following description, and will be apparent in part from the description, or may be learned by practicing the invention. The objects and other advantages of the invention may be realized and obtained by means of the structures pointed out in the description and the drawings. Attached Figure Description

[0038] Figure 1 This is a schematic diagram of an overall device for measuring the internal temperature of a high-pressure reactor according to the present invention.

[0039] Figure 2 This is a schematic diagram of the front and bottom surfaces of a device for measuring the internal temperature of a high-pressure reactor according to the present invention.

[0040] Figure 3 This is a temperature trend graph measured before calibration of the three K-type thermocouples of this invention;

[0041] Figure 4 This is a temperature trend graph obtained after calibration of the three K-type thermocouples of the present invention;

[0042] Reference numerals: 1. Air compressor; 2. Valve; 3. Water pump; 4. Water tank; 5. Tee; 6. Pressure relief valve; 7. Main valve; 8. Capillary tube; 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. Annular electric furnace. Detailed Implementation

[0043] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0044] To address the shortcomings of existing technologies, this invention discloses a device for measuring the internal temperature of a high-pressure reactor. Figure 1 This is a schematic diagram of an overall device for measuring the internal temperature of a high-pressure reactor according to the present invention, as shown below. 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 tube 8, a type K thermocouple I 9, a type K thermocouple II 10, and a type K thermocouple III 11; wherein,

[0045] The air compressor 1 is connected to the water pump 3 via a pipe, and a valve 2 is installed on the pipe;

[0046] The water pump 3 is connected to the water tank 4 via a pipe;

[0047] The water pump 3 is also connected to the pressure relief valve 6 and the main valve 7 via a tee.

[0048] The other end of the main valve 7 is connected to a capillary tube 8, which passes through the conical plug 14 of the autoclave.

[0049] Both the K-type thermocouple I9 and the K-type thermocouple II10 are installed inside the autoclave cavity 15;

[0050] The K-type thermocouple III11 is installed inside the pressure vessel body 12;

[0051] Furthermore, the capillary tube 8 is connected to the main pipeline, and its outer diameter is designed to just pass through the hole opened on the conical plug 14. Distilled water is used as the medium to enter the high-pressure reactor cavity 15 through the capillary tube 8 for pressurization.

[0052] Furthermore, the K-type thermocouples I9, II10, and III11 are all of the same type, made of nickel-chromium-nickel-aluminum material. The diameter of K-type thermocouple I9 is ​​designed to allow it to pass precisely through the hole in the conical plug 14, and its length ensures that its measuring point is located at the top of the autoclave cavity 15. Its accuracy is within its own accuracy range, i.e., accuracy class II ± 0.75%. The diameter of K-type thermocouple II10 is also designed to allow it to pass precisely through the hole in the conical plug 14, and its length ensures that the height difference between its measuring point and the measuring point of K-type thermocouple I9 is ​​not less than the sample height, where the sample height is 2–4 cm. Its accuracy is within its own accuracy range, i.e., accuracy class II ± 0.75%. The diameter of K-type thermocouple III11 is sufficient to insert it into the hole on the outer wall of the autoclave body 12, and its accuracy is within its own accuracy range, i.e., accuracy class II ± 0.75%. Its length is not subject to special requirements.

[0053] Figure 2 This is a schematic diagram of the front and bottom surfaces of a device for measuring the internal temperature of a high-pressure reactor according to the present invention, as shown below. Figure 2As shown, the autoclave includes: an autoclave body 12, a nut 13, a conical plug 14, and a high-temperature vessel cavity 15. In addition to the original conical plug 14 having only one hole, two more holes are added, forming a triangular distribution. These three holes are used to pass through a K-type thermocouple I 9, a K-type thermocouple II 10, and a capillary tube 8, respectively. The portions of these holes that contact the bottom of the conical plug 14 are welded to ensure a seal. The two K-type thermocouples are connected to a temperature display panel, allowing for real-time display of the measured temperature. The conical plug 14 is placed inside the nut 13. Both the nut 13 and the lower part of the autoclave body 12 have threads. During tightening, the conical plug 14 contacts and presses against the lower opening of the autoclave body 12, achieving a sealing effect. A simple test can be performed on the accuracy of type K thermocouple I9 and type K thermocouple II10. Simply hold the temperature measuring area of ​​each thermocouple by hand and wait for it to stabilize. If both thermocouples show a temperature of 38.1℃, then the accuracy of the two thermocouples can be considered reliable.

[0054] Based on the above-described apparatus, the present invention also discloses a method for measuring the internal temperature of a high-pressure reactor, the method comprising the following steps:

[0055] Step S1: Temperature monitoring during the heating process:

[0056] Step S11: Place two K-type thermocouples I9 and II10 of different lengths into the pressure vessel body 12 and tighten the nut 13 so that the conical plug 14 contacts and seals the bottom of the pressure vessel body 12. Place a K-type thermocouple III11 of different specifications on the outside and fill the water tank 4 with distilled water.

[0057] Step S12: Start the air compressor 1, open valve 2 and pressure relief valve 6, close the main valve 7, and discharge the air from the water pump 3.

[0058] Step S13: Close the pressure relief valve 6, open the main valve 7, and input distilled water into the autoclave body 12 through the capillary tube 8 to pressurize the autoclave cavity 15 to an appropriate value. For example, when the target pressure is set to 200MPa, the appropriate value is about 100MPa.

[0059] Step S14: Insert the upper part of the autoclave body 12 into the annular electric furnace 16 to heat the autoclave cavity 15. The tops of the three K-type thermocouples serve as temperature measuring points. Connecting all three K-type thermocouples to the temperature display panel allows for real-time display of the measured temperature. During heating, the internal and external temperatures of the autoclave cavity 15 can be monitored using the three K-type thermocouples. The internal temperature of the autoclave cavity 15 can be adjusted to the target temperature by adjusting the temperature of the annular electric furnace 16.

[0060] Step S2, Temperature monitoring during the experiment:

[0061] Step S21: After the heating process is completed, close the main valve 7. At this time, the temperature displayed by K-type thermocouple I9 and K-type thermocouple II10 is the temperature inside the autoclave cavity 15, and the temperature displayed by K-type thermocouple III11 is the temperature outside the autoclave cavity 15.

[0062] Step S22: Periodically read and record the temperatures of the three K-type thermocouples until the experiment ends.

[0063] That is, record data once the temperature of the three thermocouples is relatively stable. After that, the temperature will fluctuate within a small range, and then data can be recorded every half hour.

[0064] Step S3: Record and export temperature data:

[0065] The temperature display panel can record the temperature data of the three thermocouples in real time and generate temperature change curves. After the experiment, the temperature data can be exported using a USB flash drive for further analysis. This device has the following main advantages: First, the K-type thermocouples in the autoclave can reflect the true temperature inside the autoclave. Second, the two K-type thermocouples at different heights can reflect the temperature gradient caused by the height of the sample chamber itself.

[0066] Example:

[0067] Before temperature calibration, the temperature data obtained after operating according to the above technical solution is shown in Table 1 below.

[0068] Table 1 Temperature Records Before Correction

[0069]

[0070] The temperature records obtained after changing the temperature zone of the annular electric furnace 16 by replacing it are shown in Table 2 below.

[0071] Table 2 Temperature Record Table After Correction

[0072]

[0073] In Tables 1 and 2, the furnace temperature is the temperature of the annular electric furnace 16, the autoclave temperature is the temperature measured by K-type thermocouple III 11, the upper temperature is the temperature measured by K-type thermocouple II 10, the lower temperature is the temperature measured by K-type thermocouple I 9, and the pressure is the internal pressure of the high-pressure autoclave cavity 15.

[0074] Figure 3 This is a temperature trend graph obtained before calibration of the three K-type thermocouples of this invention. Figure 4 The temperature trend graph obtained after calibration of the three K-type thermocouples of this invention is shown in Tables 1 and 2. Figure 3 and Figure 4It is evident that, after correction, the temperature difference between the upper and lower parts is significantly reduced compared to before correction. When the pressure vessel temperature is 800℃, the internal temperature gradient of the pressure vessel cavity 15 after correction can be maintained at around 5℃, demonstrating a significant temperature correction effect.

[0075] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should 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 includes: an air compressor (1), a water pump (3), a water tank (4), a pressure relief valve (6), a main valve (7), a capillary 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 pipe, and a valve (2) is installed on the pipe; The water pump (3) is connected to the water tank (4) via a pipe; The water pump (3) is also connected to the pressure relief valve (6) and the main valve (7) via a tee. The other end of the main valve (7) is connected to a capillary tube (8); Both the K-type thermocouple I (9) and the K-type thermocouple II (10) are installed inside the high-pressure reactor cavity (15); The K-type thermocouple III (11) is installed inside the autoclave body (12).

2. The device for measuring the internal temperature of a high-pressure reactor according to claim 1, characterized in that, The outer diameter of the capillary tube (8) is determined by the hole opened on the conical plug (14), and distilled water is used as the medium to enter the high pressure vessel cavity (15) through the capillary tube (8) for pressurization.

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

4. The device for measuring the internal temperature of a high-pressure reactor 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 measuring 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 a high-pressure reactor 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, with an accuracy of Class II ±0.75%.

6. The device for measuring the internal temperature of a high-pressure reactor according to claim 3, characterized in that, The diameter of the K-type thermocouple III (11) is determined by the hole that can be inserted into the outer wall of the autoclave body (12), and the accuracy is Class II ±0.75%.

7. The device for measuring the internal temperature of a high-pressure reactor according to claim 5, characterized in that, The height of the sample is 2-4 cm.

8. The device for measuring the internal temperature of a high-pressure reactor according to claim 1, characterized in that, The autoclave includes: autoclave body (12), nut (13), conical plug (14), and autoclave cavity (15); wherein, the conical plug (14) has three holes arranged in a triangle, which are used to pass through K-type thermocouple I (9), K-type thermocouple II (10) and capillary tube (8), respectively.

9. The device for measuring the internal temperature of a high-pressure reactor 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 the temperature display panel and are used to display the measured temperature on the temperature display panel in real time.

10. A method for measuring the internal temperature of an autoclave, based on the apparatus according to any one of claims 1-9, characterized in that, The method includes the following steps: Step S1: Temperature monitoring during the heating process: Step S11: Assemble the device according to any one of claims 1-9; Step S12: Start the air compressor (1) of the above device, open the valve (2) and the pressure relief valve (6), close the main valve (7), and discharge the air in the water pump (3); Step S13: Close the pressure relief valve (6), open the main valve (7), and input distilled water into the autoclave body (12) through the capillary tube 8 to pressurize the autoclave cavity (15); Step S14: Insert the upper part of the autoclave body (12) into the annular electric furnace (16) and heat the autoclave cavity (15) through the annular electric furnace (16); Step S2, Temperature monitoring during the experiment: Step S21: After the heating process is completed, close the main valve (7). At this time, the temperature displayed by K-type thermocouple I (9) and K-type thermocouple II (10) is the temperature inside the high pressure vessel cavity (15), and the temperature displayed by K-type thermocouple III (11) is the temperature outside the high pressure vessel cavity (15). Step S22: Periodically read and record the temperatures of the three K-type thermocouples until the experiment ends; Step S3: Record and export temperature data.

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