Tube furnace for realizing in-situ test under high-temperature, low-water and low-oxygen conditions and use method of tube furnace

Abstract

The invention discloses a tubular furnace for realizing an in-situ test under high temperature, low water and low oxygen and a use method thereof. The tubular furnace comprises a sealed operation device, a telescopic sample introduction rod, a tubular furnace device, an air inlet device and a vacuum pump, the sealing operation device comprises a sealing box, and the sealing box is provided with an operation opening, a first air inlet, a second air inlet, a telescopic rod first connector, a first air outlet, a sample inlet and a vacuumizing connector connected with a vacuum pump; the first air inlet and the second air inlet are both connected with the air inlet device; the tubular furnace device comprises a heating furnace body, a glass tube and a crucible; the glass tube is placed in the heating furnace body, and two ends extend out of the heating furnace body; the crucible is fed into the sealing box from the sample inlet and is placed in the glass tube; a first flange is installed at one end of the glass tube, and a second flange is installed at the other end of the glass tube and provided with a second air outlet and a second telescopic rod connector. The equipment is low in cost and simple to operate, and can meet various test reaction requirements.

Description

Technical Field

[0001] The present invention relates to the technical field of tube furnaces, and in particular to a tube furnace for realizing in-situ testing under high temperature, low water and low oxygen conditions and a method for using the tube furnace. Background Art

[0002] Tube furnaces are widely used in various fields such as metallurgy, materials, new energy batteries and catalysis. Currently, the most commonly used tube furnace is a small horizontal tube furnace. However, this type of tube furnace is difficult to carry out high-temperature or vacuum high-altitude experiments. When performing high-temperature sampling under inert conditions, it is easy to introduce air and affect the experimental results. At the same time, after the current tube furnace experiment, the sample will come into contact with oxygen and moisture after being taken out. When the sample is susceptible to the reaction of oxygen and moisture, it will affect the subsequent test results. Summary of the Invention

[0003] The purpose of the present invention is to overcome the above-mentioned deficiencies of the prior art and to provide a tubular furnace for carrying out in-situ testing under high temperature, low water and low oxygen conditions and a method for using the same.

[0004] The present invention is achieved through the following technical solutions: a tubular furnace for carrying out in-situ tests under high temperature, low water and low oxygen conditions, comprising a sealing operating device, a telescopic sampling rod, a tubular furnace device, an air intake device and a vacuum pump; the sealing operating device comprises a sealing box, the sealing box is provided with an operating port, a first air inlet, a second air inlet, a first interface of the telescopic rod, a first air outlet, a vacuum interface and an inlet; the first air inlet and the second air inlet are both connected to the air intake device, and the vacuum pump is connected to the vacuum interface; the tubular furnace device comprises a heating furnace body, a glass tube and a crucible; the glass tube is placed in the heating furnace body, and its two ends extend out of the heating furnace body; the crucible is fed from the inlet to the crucible. into the sealed box and placed in the glass tube; a first flange is installed at one end of the glass tube, and a second flange is installed at the other end thereof, and the second flange is provided with a second air outlet and a second interface of the telescopic rod; the telescopic injection rod is inserted into the first interface of the telescopic rod and the second interface of the telescopic rod and can slide along them to push or hook and pull the crucible to move along the glass tube; the air intake device is connected to the interior of the glass tube after passing through the first flange through the air pipe; the sampling port is installed with a third flange, the sampling port is connected to the air intake device through the air inlet, and the sampling port is connected to the vacuum pump through the air outlet; the second air outlet is connected to the outside world after passing through the first air outlet through the air pipe provided with a first valve.

[0005] The sealed box is also provided with a temporary sample storage box, a sample cooling table, a drying device and a monitoring device for monitoring the temperature, humidity, pressure and oxygen concentration in the sealed box.

[0006] The telescopic injection rod includes a telescopic rod, a connecting head and a toggle rod with a right-angle hook at the front end; the rear end of the toggle rod is rotatably connected to the front end of the telescopic rod through the connecting head; the telescopic injection rod pushes the crucible into the reaction area of the glass tube through the right-angle hook, or the telescopic injection rod hooks the crucible through the right-angle hook and pulls the crucible out of the reaction area of the glass tube; dynamic sealing structures are provided between the second interface of the telescopic rod and the toggle rod, and between the first interface of the telescopic rod and the telescopic rod.

[0007] It also includes a support frame, which is arranged in the sealed box. The glass tube is placed on the upper end of the support frame. The support frame and the tube furnace device form a support structure for fixing the glass tube.

[0008] Two access ports are provided, both located on the front side of the sealed box. Nitrile rubber gloves are attached to the access ports. A sealing ring is provided between the injection port and the third flange, and a vacuum gauge is installed at the injection port. Nitrile gloves are installed at both access ports, allowing for dual-action operation and resistant to high temperatures and corrosion. The sealing rings eliminate the risk of leakage and enhance the seal.

[0009] The length of the glass tube is 1.5-2.0 times the length of the heating furnace body; with one end of the first flange as the front end, the length of the portion of the front end of the glass tube extending out of the heating furnace body is 30-60 cm.

[0010] The support frame is placed at a position where the glass tube exceeds 1 / 2 of the axial length of the heating furnace body.

[0011] The sample cooling table is a cooling table made of corundum material, on which a movable double-layer clay net is placed; the drying device is a container filled with color-changing silica gel.

[0012] The air intake device includes an inert gas cylinder, a valve and a flow meter, which are connected to the interior of the glass tube through an air pipe. A vacuum gauge is also provided on the air pipe.

[0013] A method for using a tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions comprises the following steps:

[0014] S1. Turn on the vacuum pump to evacuate the sealed box, and then introduce inert gas into the sealed box through the first air inlet and / or the second air inlet. Repeat the vacuuming and introducing inert gas operations at least three times; observe the reading of the detection device until a predetermined condition is met; turn off the vacuum pump. After the process is completed, the sealed box is filled with inert gas;

[0015] S2, open the 3rd flange of sampling port, put into the crucible equipped with sample and close the 3rd flange of sampling port, vacuumize the space between the sampling port and the 3rd flange and circulate inert gas replacement for at least three times; Open the flange that sampling port is positioned at the sealed box and take out crucible, crucible is placed in the temporary storage box for sample, and the 3rd flange of sampling port is closed;

[0016] S3. Place the crucible containing the reaction sample into the glass tube through the operation port and install the second flange;

[0017] S4, turning on the heating furnace to heat the reaction area of the glass tube to a predetermined temperature, turning on the gas inlet device to introduce a predetermined flow rate of inert gas into the glass tube;

[0018] S5. Push the telescopic rod inward to drive the toggle rod so that the crucible is located in the middle of the heating furnace body;

[0019] S6. After a single reaction is completed, rotate the telescopic rod and push the toggle rod inward to the outside of the crucible. Rotate the telescopic rod to drive the toggle rod 180°, then push it forward 1-2 cm. Continue to rotate the telescopic rod to drive the toggle rod 180°. Slowly pull the telescopic rod outward. The right-angle hook will contact the inner wall of the crucible. Pull the telescopic rod outward to drive the toggle rod to pull the crucible out. Open the second flange and move the crucible to the sample cooling table through the double-layer clay mesh for cooling.

[0020] S7. If the next experiment is required, repeat steps S3-S6;

[0021] S8. After the experiment is completely completed, turn off the heating furnace, put the samples that are sensitive to air and moisture into containers, and seal them in the containers or use a vacuum pump to store them under the protection of inert gas in a sealed box. Open the sampling port and take out the reacted samples.

[0022] Compared with the prior art, the advantages of the present invention are:

[0023] 1) This device can be used for high-temperature, low-oxygen, and low-moisture environmental reactions of common samples, as well as high-temperature reactions of samples that are sensitive to air and moisture. At the same time, the sealed box is filled with an inert atmosphere and equipped with a vacuum pump. The prepared samples can be stored in a vacuum-sealed container or in a container filled with an inert atmosphere. These samples are protected from contamination by moisture and oxygen in the air, and their subsequent testing is equivalent to the effect of high-temperature in-situ testing.

[0024] 2) In actual use, the flange outside the glass tube is equipped with a vacuum display, which can be combined with a vacuum pump to perform vacuum extraction operations, as well as vacuum high-temperature experiments. At the same time, replacing the gas cylinder can realize experiments under various reaction atmospheres. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1Schematic diagram of the structure of an embodiment of the present invention.

[0026] The meanings of the reference numerals in the figure are: 5. Sealing box; 6. Operation port; 7. First air inlet; 8. Second air inlet; 9. First interface of telescopic rod; 10. First air outlet; 11. Vacuum interface; 12. Vacuum pump; 13. Inlet; 14. Toggle lever; 15. Connector; 16. Telescopic rod; 17. Heating furnace body; 18. Glass tube; 19. Crucible; 20. Support frame; 21. First flange; 22. Vacuum gauge; 23. Second flange; 24. Second air outlet; 25. Second interface of telescopic rod; 26. First valve; 27. Monitoring device; 28. Temporary sample storage box; 29. Sample cooling table; 30. Drying device; 31. Inert gas cylinder. DETAILED DESCRIPTION

[0027] The present invention will be described in further detail below with reference to the accompanying drawings and specific embodiments.

[0028] Example

[0029] See Figure 1 , which is a tubular furnace for performing in-situ tests under high temperature, low water and low oxygen conditions, including a sealing operation device, a telescopic sampling rod, a tubular furnace device, an air intake device and a vacuum pump 12; the sealing operation device includes a sealing box 5, which is provided with an operation port 6, a first air inlet 7, a second air inlet 8, a first interface 9 of the telescopic rod, a first air outlet 10, a vacuum interface 11 and an injection port 13; the first air inlet 7 and the second air inlet 8 are both connected to the air intake device, and the vacuum pump 12 is connected to the vacuum interface 11; the tubular furnace device includes a heating furnace body 17, a glass tube 18 and a crucible 19; the glass tube 18 is placed in the heating furnace body 17, and its two ends extend out of the heating furnace body 17; the crucible 19 is fed into the sealing box 5 from the injection port 13 And placed in the glass tube 18; a first flange 21 is installed at one end of the glass tube 18, and a second flange 23 is installed at the other end thereof, and the second flange 23 is provided with a second air outlet 24 and a second interface 25 of the telescopic rod; the telescopic injection rod is inserted into the first interface 9 of the telescopic rod and the second interface 25 of the telescopic rod and can slide along them to push or hook and pull the crucible 19 to move along the glass tube 18; the air intake device is connected to the interior of the glass tube 18 after passing through the first flange 21 through the air pipe; the sampling port 13 is installed with a third flange, the sampling port 13 is connected to the air intake device through the air inlet, and the sampling port 13 is connected to the vacuum pump 12 through the air outlet; the second air outlet 24 is connected to the outside world after passing through the first air outlet 10 through the air pipe provided with a first valve 26.

[0030] The sealed box 5 is further provided with a temporary sample storage box 28 , a sample cooling table 29 , a drying device 30 and a monitoring device 27 for monitoring the temperature, humidity, pressure and oxygen concentration in the sealed box 5 .

[0031] The telescopic injection rod includes a telescopic rod 16, a connector 15, and a toggle rod 14 with a right-angled hook at the front end. The rear end of the toggle rod 14 is rotatably connected to the front end of the telescopic rod 16 via the connector 15. The telescopic injection rod pushes the crucible 19 into the reaction area of the glass tube 18 via the right-angled hook, or the telescopic injection rod hooks the crucible 19 with the right-angled hook and pulls the crucible 19 out of the reaction area of the glass tube 18. Dynamic sealing structures are provided between the second interface 25 of the telescopic rod and the toggle rod 14, and between the first interface 9 of the telescopic rod and the telescopic rod 16. In this embodiment, when the crucible 19 needs to be pushed into the reaction area, the toggle rod 14 is directly pushed inward to push the crucible 19 toward the reaction area. To remove crucible 19, rotate telescopic rod 16, push lever 14 inward to the outside of crucible 19, then rotate telescopic rod 16 again to rotate lever 14 180°, then push lever 14 forward 1-2 cm. Continue rotating telescopic rod 16 to rotate lever 14 180°, then slowly pull telescopic rod 16 outward. The right-angle hook will contact the inner wall of crucible 19. Pull telescopic rod 16 outward to drive lever 14 to pull crucible 19 out. The dynamic sealing structure can use adhesive or sealing ring.

[0032] The support frame 20 is also included. The support frame 20 is arranged in the sealed box 5. The glass tube 18 is placed on the upper end of the support frame 20. The support frame 20 and the tube furnace device form a support structure for fixing the glass tube 18.

[0033] Two operating ports 6 are provided, both located on the front side of the sealed box 5. Nitrile rubber gloves are attached to the operating ports 6. A sealing ring is provided between the injection port 13 and the third flange, and the injection port 13 is equipped with a vacuum gauge. Nitrile gloves are installed at both operating ports 6, allowing for dual-operation and high-temperature and corrosion resistance. The sealing rings eliminate the risk of leakage and enhance the seal.

[0034] The length of the glass tube 18 is 1.5-2.0 times the length of the heating furnace body 17. With the first flange 21 end as the front end, the rear end of the glass tube 18 extends 30-60 cm from the heating furnace body 17. In this embodiment, approximately half of the length of the glass tube 18 is located outside the heating furnace body 17.

[0035] The support frame 20 is placed at a position where the glass tube 18 exceeds 1 / 2 of the axial length of the heating furnace body 17 .

[0036] The sample cooling table 29 is a cooling table made of corundum, on which a movable double-layer clay net is placed; the drying device 30 is a container filled with color-changing silica gel.

[0037] The air intake device includes an inert gas cylinder 31, a valve and a flow meter. The inert gas cylinder 31, the valve, the flow meter and the interior of the glass tube 18 are connected through an air pipe. A vacuum gauge 22 is also provided on the air pipe.

[0038] A method for using a tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions comprises the following steps:

[0039] S1. Turn on the vacuum pump 12 to evacuate the sealed box 5, and then introduce inert gas into the sealed box 5 through the first air inlet 7 and / or the second air inlet 8. Repeat the vacuuming and introducing inert gas operations at least three times; observe the reading of the detection device until the predetermined condition is met; turn off the vacuum pump 12. After the process is completed, the sealed box 5 is filled with inert gas;

[0040] S2, open the third flange of the sampling port 13, put into the crucible 19 containing the sample and close the third flange of the sampling port 13, and evacuate the space between the sampling port 13 and the third flange and perform an inert gas replacement cycle at least three times; open the flange of the sampling port 13 located in the sealed box 5 and take out the crucible 19, place the crucible 19 in the temporary sample storage box 28, and close the third flange of the sampling port 13;

[0041] S3. Place the crucible 19 containing the reaction sample into the glass tube 18 through the operation port 6 and install the second flange 23;

[0042] S4, turning on the heating furnace 17 to heat the reaction area of the glass tube 18 to a predetermined temperature, turning on the gas inlet device to introduce a predetermined flow of inert gas into the glass tube 18;

[0043] S5, push the telescopic rod 16 inward to drive the toggle rod 14 so that the crucible 19 is located in the middle of the heating furnace body 17;

[0044] S6. After the single reaction is completed, rotate the telescopic rod 16 and push the toggle rod 14 inward to the outside of the crucible 19. Rotate the telescopic rod 16 to drive the toggle rod 14 to rotate 180°, then push it forward 1-2 cm. Continue to rotate the telescopic rod 16 to drive the toggle rod 14 to rotate 180° and pull it back 1-2 cm. Slowly pull the telescopic rod 16 outward. The right-angle hook will contact the inner wall of the crucible 19. Pull the telescopic rod 16 outward to drive the toggle rod 14 to pull the crucible 19 out. Open the second flange 23 and move the crucible 19 to the sample cooling table 29 for cooling.

[0045] S7. If the next experiment is required, repeat steps S3-S6;

[0046] S8. After the experiment is completely completed, the heating furnace body 17 is turned off, and the samples that are sensitive to air and moisture are placed in containers. Under the protection of the inert gas in the sealed box 5, the samples are sealed and stored in the containers or vacuumed and stored by the vacuum pump 12. The sample inlet 13 is opened to take out the reacted samples.

[0047] In this embodiment, the inlet and outlet ports of the sample inlet 13 are valved, allowing for vacuuming and connection to an inert gas cylinder 31. When a sample is placed, repeated vacuuming and ventilation operations are performed to remove air from the sample inlet 13, allowing the sample to be introduced into the sealed chamber 5 under an inert atmosphere. Both sides of the sample inlet 13 are sealed with flanges and gaskets. A movable glass tube 18 is horizontally positioned within the heating furnace 17. The portion of the glass tube 18 extending beyond the heating furnace 17 is provided with a movable support frame 20. The position of the glass tube 18 and support frame 20 can be flexibly adjusted according to experimental needs. The temperature of the portion of the glass tube 18 away from the heating furnace 17 is unaffected by the temperature of the heating furnace 17 and serves as a waiting zone for the reaction. The toggle lever 14 is a thin iron rod, and the telescopic rod 16 is a telescopic iron rod. The monitoring device 27 can be a multifunctional integrated device or a device comprising multiple single-function structures. This is a mature technology, so detailed structural analysis is unnecessary. Commonly used indoor or industrial thermo-hygrometers and positive and negative pressure gauges can be used. The temporary sample storage box 28 is a common plastic box. The drying device 30 is a container such as a beaker, which is filled with color-changing silica gel. The color-changing silica gel can be dried in an oven and reused many times.

[0048] Example 1

[0049] Assemble the tube furnace: Pass the glass tube 18 through the heating furnace body 17. Connect the vacuum gauge 22 and the air inlet pipe via the first flange 21 at the front end. Install the second flange 23 at the end. Place the support frame 20 outside the heating furnace body 17 to ensure the glass tube 18 is level. Connect the telescopic injection rod to the sealed box 5 via the first telescopic rod interface 9. Install a flange with a valve on the injection port 13 and connect it to the inert gas cylinder 31 via the air pipe. Place a monitoring device 27 inside the sealed box 5 to display the humidity, oxygen content, and pressure in real time.

[0050] The high temperature, low oxygen and low water environment in this embodiment refers to the test conditions that the test personnel want to achieve. The temperature, oxygen concentration, humidity and pressure mainly depend on the test requirements. The heating temperature is generally from room temperature to 1000°C, the humidity can be controlled to <10% RH, the oxygen is less than 1% vol, and the pressure atmosphere in the sealed box 5 is -0.1-0.7MPa.

[0051] Preparation of inert environment: Close all valves, start the vacuum pump 12 to evacuate the sealed box 5 to -0.1 MPa, introduce high-purity inert gas through the second air inlet 8 to normal pressure, repeat 3 times to replace the residual air, and confirm that the humidity monitoring value is stable at <10% RH and the oxygen is less than 1% vol.

[0052] Sample pretreatment: Place the weighed sample into crucible 19. Open the switch on the outside of the sealed box 5 at the sampling port 13 and place the crucible 19 inside the sampling port 13. The two valves of the sampling port 13 are connected to the vacuum pump 12 and the inert gas cylinder 31, respectively. Start the vacuum pump 12 to pump the sampling port 13 to -0.1 MPa. Then, introduce high-purity inert gas to atmospheric pressure. Repeat this three times to displace any remaining air. Using the nitrile gloves at the operating port 6, open the sampling port 13 inside the sealed box 5 and place the crucible 19 into the temporary sample storage box 28. Close the sampling port 13. The temporary sample storage box 28 can store more than 10 crucibles 19 at the same time.

[0053] High-temperature sampling experiment: Use the nitrile gloves at the operating port 6 to place the crucible 19 in the temporary sample storage box at the rear end of the glass tube 18. Install the second flange 23, set the heating furnace body 17 to heat from room temperature to 800°C at a rate of 5°C / min, and at the same time turn on the argon flowmeter to maintain a 50mL / min air flow. When the furnace temperature stabilizes, push the telescopic iron rod (telescopic rod 16) to allow the thin iron rod (toggle rod 14) to push the crucible 19 to the center of the heating zone, and maintain the reaction for 60 minutes.

[0054] Sampling and cooling: After the reaction is completed, rotate the telescopic rod 180°, push it forward 1 cm and rotate it 180°, hook the inner wall of the crucible 19, slowly pull it out to the waiting area and cool it for 10 minutes, open the second flange 23, and move the crucible 19 to the sample cooling table 29 through the double-layer clay mesh. After it cools to room temperature, put the reacted sample into an argon-filled sealed bag to avoid contact with air, and take it out through the sampling port 13.

[0055] Example 2

[0056] The difference between Example 2 and Example 1 is:

[0057] In this embodiment, there is no need to ventilate the sealed box 5 , and the tube furnace is directly vacuumed and ventilated to remove the air and moisture in the glass tube 18 . This method can be used to perform high-temperature experiments on samples with low requirements.

[0058] Sample preparation: The weighed sample is placed into the crucible 19 , which is placed at the rear end of the glass tube 18 , and the second flange 23 is installed.

[0059] Prepare an inert environment: Close the first valve 26 of the tubular furnace outlet, connect the vacuum pump 12 to the first air inlet 7, start the vacuum pump 12 to evacuate the sealed box 5 to -0.1 MPa, close the valve, and introduce high-purity inert gas through the first air inlet 7 to normal pressure. Repeat this three times to replace the residual air. After completion, open the first valve 26 of the air outlet.

[0060] High-temperature sample injection experiment: Set the heating furnace 17 to 800°C at a rate of 5°C / min. Simultaneously, turn on the argon flowmeter to maintain a 50 mL / min flow. Once the furnace temperature stabilizes, push the telescopic iron rod (telescopic rod 16) so that the thin iron rod (toggle rod 14) pushes the crucible 19 to the center of the heating zone. Maintain the reaction for 60 minutes. After the reaction is complete, rotate the telescopic rod 180°, advance it 1 cm, then rotate it 180°. Engage the inner wall of the crucible 19 and slowly pull it out to the holding zone. Cool it for 10 minutes. Then, open the second flange 23 and move the crucible 19 through the double-layered clay mesh to the sample cooling table 29. Cool it and remove it.

[0061] This equipment is suitable for tube furnace experiments with sample introduction in specific high-temperature environments, experiments in high-temperature, low-oxygen, and low-water environments, and experiments with samples sensitive to oxygen and moisture in the air. It can avoid contact between samples and contaminated carbon and contaminated oxygen in the air after the reaction, and is suitable for tests with high requirements for experimental conditions. This equipment achieves high-temperature sample introduction and preparation of experimental samples equivalent to in-situ testing at a lower cost.

[0062] The above detailed description is a specific description of a feasible embodiment of the present invention. The embodiment is not intended to limit the patent scope of the present invention. Any equivalent implementation or modification that does not depart from the present invention should be included in the patent scope of this case.

Claims

1. A tubular furnace for conducting in-situ tests under high temperature, low water and low oxygen conditions, characterized by: The invention comprises a sealing operation device, a telescopic injection rod, a tubular furnace device, an air intake device and a vacuum pump; the sealing operation device comprises a sealing box, the sealing box is provided with an operation port, a first air intake port, a second air intake port, a first interface of the telescopic rod, a first air outlet port, a vacuum interface and an injection port; the first air intake port and the second air intake port are both connected to the air intake device, and the vacuum pump is connected to the vacuum interface; the tubular furnace device comprises a heating furnace body, a glass tube and a crucible; the glass tube is placed in the heating furnace body, and its two ends extend out of the heating furnace body; the crucible is fed into the sealing box from the injection port and placed in the glass tube; the glass tube is A first flange is installed at one end, and a second flange is installed at the other end, and the second flange is provided with a second air outlet and a second interface of the telescopic rod; the telescopic injection rod is inserted into the first interface of the telescopic rod and the second interface of the telescopic rod and can slide along them to push or hook and pull the crucible to move along the glass tube; the air intake device is connected to the inside of the glass tube after passing through the first flange through the air pipe; the injection port is provided with a third flange, an air inlet and an air outlet, the injection port is connected to the air intake device through the air inlet, and the injection port is connected to the vacuum pump through the air outlet; the second air outlet is connected to the outside world after passing through the first air outlet through the air pipe provided with a first valve.

2. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: The sealed box is also provided with a temporary sample storage box, a sample cooling table, a drying device and a monitoring device for monitoring the temperature, humidity, pressure and oxygen concentration in the sealed box.

3. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: The telescopic injection rod includes a telescopic rod, a connecting head and a toggle rod with a right-angle hook at the front end; the rear end of the toggle rod is rotatably connected to the front end of the telescopic rod through the connecting head; the telescopic injection rod pushes the crucible into the reaction area of the glass tube through the right-angle hook, or the telescopic injection rod hooks the crucible through the right-angle hook and pulls the crucible out of the reaction area of the glass tube; dynamic sealing structures are provided between the second interface of the telescopic rod and the toggle rod, and between the first interface of the telescopic rod and the telescopic rod.

4. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: It also includes a support frame, which is arranged in the sealed box. The glass tube is placed on the upper end of the support frame. The support frame and the tube furnace device form a support structure for fixing the glass tube.

5. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: There are two operation ports, both arranged on the front side of the sealing box, and gloves made of nitrile rubber are connected to the operation ports; a sealing ring is provided between the sampling port and the third flange, and a vacuum gauge is provided on the sampling port.

6. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: The length of the glass tube is 1.5-2.0 times the length of the heating furnace body; with one end of the first flange as the front end, the length of the portion of the rear end of the glass tube extending out of the heating furnace body is 30-60 cm.

7. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 4, characterized in that: The support frame is placed at a middle position where the glass tube exceeds the heating furnace body.

8. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 2, characterized in that: The sample cooling table is a cooling table made of corundum material, on which a movable double-layer clay net is placed; the drying device is a container filled with color-changing silica gel.

9. The tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: The air intake device includes an inert gas cylinder, a valve and a flow meter, which are connected to the interior of the glass tube through an air pipe. A vacuum gauge is also provided on the air pipe.

10. A method for using the tubular furnace for performing in-situ testing under high temperature, low water and low oxygen conditions according to claim 1, characterized in that: The steps include: S1. Turn on the vacuum pump to evacuate the sealed box, and then introduce inert gas into the sealed box through the first air inlet and / or the second air inlet. Repeat the vacuuming and introducing inert gas operations at least three times; observe the reading of the detection device until a predetermined condition is met; turn off the vacuum pump. After the process is completed, the sealed box is filled with inert gas; S2, open the 3rd flange of sampling port, put into the crucible equipped with sample and close the 3rd flange of sampling port, vacuumize the space between the sampling port and the 3rd flange and circulate inert gas replacement for at least three times; Open the flange that sampling port is positioned at the sealed box and take out crucible, crucible is placed in the temporary storage box for sample, and the 3rd flange of sampling port is closed; S3. Place the crucible containing the reaction sample into the glass tube through the operation port and install the second flange; S4, turning on the heating furnace to heat the reaction area of the glass tube to a predetermined temperature, turning on the gas inlet device to introduce a predetermined flow rate of inert gas into the glass tube; S5. Push the telescopic rod inward to drive the toggle rod so that the crucible is located in the middle of the heating furnace body; S6. After a single reaction is completed, rotate the telescopic rod and push the toggle rod inward to the outside of the crucible. Rotate the telescopic rod to drive the toggle rod 180°, then push it forward 1-2 cm. Continue to rotate the telescopic rod to drive the toggle rod 180°. Slowly pull the telescopic rod outward. The right-angle hook will contact the inner wall of the crucible. Pull the telescopic rod outward to drive the toggle rod to pull the crucible out. Open the second flange and move the crucible to the sample cooling table through the double-layer clay mesh for cooling. S7. If the next experiment is required, repeat steps S3-S6; S8. After the experiment is completely completed, turn off the heating furnace, put the samples that are sensitive to air and moisture into containers, and seal them in the containers or use a vacuum pump to store them under the protection of inert gas in a sealed box. Open the sampling port and take out the reacted samples.

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