Non-metal high-capacity high-temperature saturated steam pressure balance reaction kettle device and use method thereof

Abstract

The invention discloses a nonmetal high-capacity high-temperature saturated steam pressure balance reaction kettle device and a use method thereof. The device comprises a drying oven, a kettle body, a kettle cover, an inner container, a temperature sensor and a pressure sensor, a hollow base is arranged at the lower end in the drying oven to support the kettle body, the inner container is arranged in the kettle body, a gap is reserved between the inner container and the kettle body to accommodate a heat transfer medium, an opening of the inner container is welded and sealed, and the kettle cover and the kettle body are sealed and detachably connected through bolts and sealing rings. The monitoring end of the temperature sensor extends into the kettle body, one end of the pipeline is communicated with the interior of the kettle body, the other end of the pipeline penetrates through the drying oven to be connected with an external pressure sensor, and the temperature sensor and the pressure sensor are respectively connected with a controller through signal cables. The controller is connected with the control end of the drying oven and a display screen on the drying oven through signal cables. Internal and external pressure balance and explosion prevention of the inner container are achieved through vaporization of the heat transfer medium, the quartz inner container is matched with parent metal elements, the requirement for the large sample loading amount is met, and the application range is wide.

Description

Technical Field

[0001] This invention belongs to the field of reaction vessel technology, and relates to a non-metallic, large-capacity, high-temperature saturated steam pressure balance reaction vessel device and its usage method. Background Technology

[0002] Reactors are commonly used containers in chemical reactions. Existing reactors mostly use metal liners, which are unsuitable for experiments involving metal-sensitive substances. For metalophilic elements such as rhenium (Re) and osmium (Os), or for hydrogen generation simulation experiments where metal liners readily react with metals at high temperatures, the metal liners will directly react with the sample, interfering with material stability. On the other hand, some non-metallic liner materials suffer from insufficient high-temperature resistance and are prone to cracking under high pressure, making them unsuitable for high-temperature and high-pressure conditions. Existing non-metallic liner reactors generally have small sample capacity, with liner volumes mostly below 100 mL, only sufficient for trace samples. For samples such as rock powder that require a certain quantity to ensure experimental representativeness, small-capacity liners cannot provide sufficient reaction space. Furthermore, existing reactors do not apply uniform or constant temperature and pressure to the sample during heating and pressurization, particularly struggling to maintain a constant high saturated vapor pressure. Therefore, there is an urgent need for a reactor device suitable for metallic materials. Summary of the Invention

[0003] This invention provides a non-metallic, large-capacity, high-temperature saturated vapor pressure equilibrium reactor device to solve the problems of unsuitable metal material for metal-sensitive experiments and small sample loading capacity in the prior art.

[0004] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is: a non-metallic large-capacity high-temperature saturated steam pressure balance reactor device, including an oven, a reactor body, a reactor lid, an inner liner, a temperature sensor, and a pressure sensor; The oven has a base at its lower interior, and the vessel body rests on the base. An inner liner seat is located at the lower interior of the vessel body, and the inner liner rests on the inner liner seat. A gap is formed between the outer side of the inner liner and the vessel body to accommodate the heat transfer medium. The inner liner is made of a high-temperature and high-pressure resistant material. The upper opening of the inner liner is sealed by welding. A sealing ring groove is formed at the upper edge of the vessel body, and a sealing ring is installed inside the groove. The vessel lid is detachably connected to the vessel body by bolts and sealed by a sealing ring. The vessel body and lid are made of high-temperature and high-pressure resistant materials, and a temperature sensor is connected to the lid. The temperature sensor's monitoring end extends into the interior of the vessel. The vessel lid is also connected to a pipe, one end of which is connected to the interior of the vessel, and the other end of which is connected to the monitoring end of the pressure sensor through a through-hole on the oven. The temperature sensor and pressure sensor are respectively connected to the controller via signal cables. The controller is connected to the control terminal of the oven and the display screen on the oven via signal cables. The controller is used to receive temperature and pressure data collected by the temperature sensor and pressure sensor, and to adjust the heating mode of the oven according to the data. The display screen is used to display the temperature and pressure data.

[0005] Furthermore, a first mating hole is provided at the opening edge of the vessel body, and a second mating hole is provided at the edge of the vessel lid corresponding to the first mating hole. A bolt is installed in both the first and second mating holes. The vessel lid is also provided with ejector threaded holes, and a screw is connected in each ejector threaded hole. The end of the screw abuts against the upper end of the vessel body.

[0006] Furthermore, the vessel body has a cylindrical structure and is made of high-strength alloy steel.

[0007] Furthermore, the inner liner has a cylindrical structure and is made of quartz material.

[0008] Furthermore, the lid of the vessel is made of high-strength alloy steel.

[0009] Furthermore, the base has a hollow structure.

[0010] Furthermore, the sealing ring is made of graphite material.

[0011] Furthermore, a protective cover is provided around the body of the vessel, and the lower end of the protective cover is fixed to the base.

[0012] Furthermore, the protective cover has a hollow structure.

[0013] This invention also provides a method for using a non-metallic, large-capacity, high-temperature saturated vapor pressure-balanced reactor, comprising the following steps: S1. Place the reactant into the inner liner, then weld and seal the opening of the inner liner. Place the sealed inner liner into the vessel body, and inject the heat transfer medium into the gap between the outer side of the inner liner and the vessel body. Use bolts to achieve a detachable connection between the vessel body and the vessel lid, and seal it with a sealing ring to form a closed cavity. Open the oven door and place the sealed vessel body and vessel lid inside the oven, so that the vessel body is placed on the base. A temperature sensor is connected to the vessel lid, and the detection end of the temperature sensor is connected to the inside of the vessel body. A pipeline is also connected to the vessel lid. One end of the pipeline is connected to the inside of the vessel body, and the other end of the pipeline is connected to the monitoring end of the pressure sensor outside the oven. S2. Close the oven door and start the oven. The oven heats the vessel body, and the heat is transferred to the heat transfer medium inside the vessel body to form saturated steam. The heat is then transferred to the inner liner, so that the reactants in the inner liner react in a high temperature and high saturated steam pressure reaction environment. Temperature and pressure sensors collect temperature and pressure data in real time and upload them to the controller. The controller compares the preset parameters and adjusts the oven heating mode to maintain the pressure balance between the vessel body and the inner liner. S3. After the reaction is complete, close the oven and cool it down. After cooling, open the oven door, remove the temperature sensor from the lid, remove the pipeline from the lid, remove the body and lid from the oven, remove the bolts on the body and lid, rotate the screws to open the lid, open the lid and take out the inner liner, cut open the welded end of the inner liner and take out the reaction product inside the inner liner.

[0014] Compared with the prior art, the beneficial effects of the above-mentioned technical solution of the present invention are as follows: This invention heats the vessel body in an oven and then transfers the heat to the inner liner. The heat transfer medium surrounding the inner liner and the steam generated during heating enable uniform and constant heating of the sample inside the inner liner. A temperature sensor monitors the internal temperature of the vessel body in real time. The temperature inside the vessel body rises to a set high temperature and the saturated steam pressure reaches a set high pressure. Simultaneously, the temperature inside the inner liner rises to a set high temperature and the saturated steam pressure reaches a set high pressure. A pressure sensor monitors the internal pressure of the vessel body in real time. The pressure inside and outside the inner liner is in a state of pressure equilibrium, maintaining a constant pressure and preventing the inner liner from bursting. The sample is subjected to constant temperature and pressure loading in the sealed inner liner, and no leakage occurs during the loading reaction.

[0015] The inner liner of this invention is made of quartz material, which is suitable for metal-sensitive elements, such as metalophilic elements like Re and Os, as well as hydrogen-generating substances that readily react with metals at high temperatures. The chemical stability of quartz material can prevent contamination of the products during high-temperature reactions; the inner liner of the reactor device has a large sample loading capacity. Attached Figure Description

[0016] Figure 1 This is a three-dimensional view of a high-temperature saturated steam pressure equilibrium reactor.

[0017] Figure 2 This is a front view of a high-temperature saturated steam pressure equilibrium reactor.

[0018] Figure 3 This is a front view of a high-temperature saturated steam pressure equilibrium reactor.

[0019] Figure 4 This is a side view of a high-temperature saturated vapor pressure equilibrium reactor.

[0020] Figure 5 for Figure 4 Sectional view along the AA direction.

[0021] The reference numerals in the attached figures are as follows: 1-Oven; 11-Display screen; 12-Door; 21-Bottle body; 211-Inner liner seat; 212-Sealing ring groove; 213-Sealing ring; 22-Bottle cover; 221-Pipeline; 231-Bolt; 232-Screw; 24-Protective cover; 25-Base; 3-Inner liner; 41-Temperature sensor; 42-Pressure sensor; 421-Pipe hole. Detailed Implementation

[0022] The present invention will be further illustrated below with reference to embodiments. These embodiments are for illustrative purposes only and are not intended to limit the invention in any way. It should be understood that the described embodiments are merely some, not all, of the embodiments described in this application. All other embodiments obtained by those skilled in the art based on the embodiments in this application without inventive effort are within the scope of protection of this application. Example

[0023] See Figures 1-5 A non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor device includes an oven, reactor body, inner liner, reactor lid, temperature sensor, and pressure sensor. The oven 1 is connected to the door 12. A base 15 is located at the lower end of the oven 1. The base 25 has a hollow structure. An inner liner seat 211 is located at the lower end of the vessel body 21. The inner liner 3 is placed on the inner liner seat 211. The upper opening of the inner liner 3 is sealed by welding. The inner liner 3 is a cylindrical inner liner made of quartz material. A sealing ring groove 212 is opened at the upper edge of the vessel body 21. A sealing ring 213 made of graphite material is installed in the sealing ring groove 212. The sealing ring 213 achieves a tight seal between the vessel body 21 and the vessel lid 22. The vessel body 21 has eight first mating holes at its opening edge, and the vessel cover 22 has eight second mating holes at its edge corresponding to the first mating holes. The first and second mating holes are connected detachably to the vessel body 21 and the vessel cover 22 by bolts 231. The vessel cover 22 also has two ejector threaded holes, each containing a screw 232. The end of the screw 232 contacts the upper end of the vessel body 21. A perforated protective cover 24 surrounds the vessel body 21. The lower end is fixed to the hollow structure base 15 inside the oven 1. Both the base 15 and the protective cover 24 are hollow structures to ensure that the vessel body 21 is heated evenly. A temperature sensor 41 is connected to the vessel cover 22. The monitoring end of the temperature sensor 41 is connected to the inside of the vessel body 21. A pipe 221 is also connected to the vessel cover 22. One end of the pipe 221 is connected to the inside of the vessel body 21, and the other end of the pipe 221 is connected to the monitoring end of the pressure sensor 42 through the through hole 421 on the oven 1. The temperature sensor 41 and the pressure sensor 42 are respectively connected to the controller through signal cables. The controller is also connected to the control terminal of the oven 1 and the display screen 11 on the oven 1 through signal cables. The controller is used to receive the temperature and pressure data collected by the temperature sensor 41 and the pressure sensor 42, and adjust the heating mode of the oven according to the temperature and pressure data. The display screen 11 on the oven 1 is used to display the temperature and pressure data. The temperature sensor 41 and the pressure sensor 42 can monitor the temperature and pressure data of the reaction in real time and change the heating mode of the oven 1 in real time. Among them, oven 1 can provide a variety of heating modes, such as constant temperature mode, segmented mode, and curve mode.

[0024] See Figures 3-5 The vessel body 21 has an inner liner seat 211 inside, and an inner liner 3 is placed on the inner liner seat 211. The upper opening of the inner liner 3 is sealed by welding. The vessel body 21 and the vessel cover 22 are detachably connected by bolts 231 and screws 232. The vessel body 21 is a cylindrical vessel body 21 made of high-strength alloy steel. The vessel cover 22 is also made of high-strength alloy steel. A temperature sensor 41 is connected to the vessel cover 22. The monitoring end of the temperature sensor 41 extends into the vessel body 21. A pipe 221 is also connected to the vessel cover 22. One end of the pipe 221 extends into the vessel body 21, and the other end of the pipe 221 is connected to the monitoring end of the pressure sensor 42 through the through hole 421 on the oven 1.

[0025] This embodiment also provides a method for using a non-metallic, large-capacity, high-temperature saturated vapor pressure-balanced reactor. This method is applied to the reactor apparatus described in the above embodiment and specifically includes the following steps: S1. Place the reactants into the inner liner 3 and seal the upper opening of the inner liner 3 by welding. Place the sealed inner liner 3 inside the vessel body 21. Inject heat transfer liquid into the gap between the outer wall of the inner liner 3 and the vessel body 21. The vessel lid 22 and the vessel body 21 are sealed together by a sealing ring 213. The vessel lid 22 and the vessel body 21 are detachably connected by bolts 231 to form a sealed cavity. Open the door 12 of the oven 1 and place the sealed vessel body 21 and vessel lid 22 inside the oven 1. The vessel body 21 is placed on the hollow structure base 25 inside the oven 1. The base 25 supports the vessel body 21 without affecting the heat transfer from the oven 1 to the vessel body 21 from below. A temperature sensor 41 is connected to the lid 22. The monitoring end of the temperature sensor 41 is connected to the inside of the vessel body 21. A pipe 221 is also connected to the lid 22. One end of the pipe 221 is connected to the inside of the vessel body 21, and the other end of the pipe 221 is connected to the monitoring end of the pressure sensor 42 through the through hole 421 on the oven 1. S2. Close the door 12 of the oven 1 and start the oven 1. The oven 1 heats the vessel body 21, so that the heat is transferred to the heat transfer medium inside the vessel body 21 and forms saturated steam. Then, the heat is transferred to the inner liner 3, so that the reactants in the inner liner 3 can react in a high temperature and high saturated steam pressure reaction environment. The temperature sensor 41 and the pressure sensor 42 collect temperature and pressure data in real time and upload them to the controller. The controller compares the preset parameters and adjusts the oven heating mode to maintain the pressure balance between the vessel body 21 and the inner liner 3. The temperature and pressure data are displayed in real time on the display screen 11. S3. After the reaction is complete, close the oven 1. After cooling, open the door 12 of the oven 1. Remove the temperature sensor 41 and the pipeline 221 from the lid 22. Remove the body 21 and lid 22 from the oven 1. First, remove the bolt 231 that fixes the body 21 and lid 22. Then, rotate the screw 232 on the edge of the lid 22 so that the end of the screw 232 abuts against the upper surface of the body 21 and generates a pushing force. This will lift the lid 22, which may have adhered to the opening of the body after the high-temperature reaction. Open the lid 22 and take out the inner liner 3. Cut open the welded end of the inner liner 3 and take out the product after the reaction inside the inner liner 3 to obtain the desired product.

[0026] Of course, the above description is not intended to limit the present invention, and the present invention is not limited to the examples given above. Any changes, modifications, additions or substitutions made by those skilled in the art within the scope of the present invention should also fall within the protection scope of the present invention.

Claims

1. A non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor, characterized in that, Includes oven, vessel body, vessel lid, inner liner, temperature sensor, and pressure sensor; The oven has a base at its lower interior, and the vessel body rests on the base. An inner liner seat is located at the lower interior of the vessel body, and the inner liner rests on the inner liner seat. A gap is formed between the outer side of the inner liner and the vessel body to accommodate the heat transfer medium. The inner liner is made of a high-temperature and high-pressure resistant material. The upper opening of the inner liner is sealed by welding. A sealing ring groove is formed at the upper edge of the vessel body, and a sealing ring is installed inside the groove. The vessel lid is detachably connected to the vessel body by bolts and sealed by a sealing ring. The vessel body and lid are made of high-temperature and high-pressure resistant materials, and a temperature sensor is connected to the lid. The temperature sensor's monitoring end extends into the interior of the vessel. The vessel lid is also connected to a pipe, one end of which is connected to the interior of the vessel, and the other end of which is connected to the monitoring end of the pressure sensor through a through-hole on the oven. The temperature sensor and pressure sensor are respectively connected to the controller via signal cables. The controller is connected to the control terminal of the oven and the display screen on the oven via signal cables. The controller is used to receive temperature and pressure data collected by the temperature sensor and pressure sensor, and to adjust the heating mode of the oven according to the data. The display screen is used to display the temperature and pressure data.

2. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, A first mating hole is provided at the opening edge of the vessel body, and a second mating hole is provided at the edge of the vessel lid corresponding to the first mating hole. A bolt is installed in both the first and second mating holes. The vessel lid is also provided with ejector threaded holes, and a screw is connected in each ejector threaded hole. The end of the screw abuts against the upper end of the vessel body.

3. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, The vessel body has a cylindrical structure and is made of high-strength alloy steel.

4. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, The inner liner has a cylindrical structure and is made of quartz material.

5. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, The lid of the vessel is made of high-strength alloy steel.

6. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, The base has a hollow structure.

7. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, The sealing ring is made of graphite material.

8. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 1, characterized in that, A protective cover is arranged around the body of the vessel, and the lower end of the protective cover is fixed to the base.

9. The non-metallic, large-capacity, high-temperature saturated steam pressure balance reactor according to claim 8, characterized in that, The protective cover has a hollow structure.

10. A method of using a non-metallic, large-capacity, high-temperature saturated vapor pressure balance reactor according to any one of claims 1-9, characterized in that, Includes the following steps: S1. Place the reactant into the inner liner, then weld and seal the opening of the inner liner. Place the sealed inner liner into the vessel body, and inject the heat transfer medium into the gap between the outer side of the inner liner and the vessel body. Use bolts to achieve a detachable connection between the vessel body and the vessel lid, and seal it with a sealing ring to form a closed cavity. Open the oven door and place the sealed vessel body and vessel lid inside the oven, so that the vessel body is placed on the base. A temperature sensor is connected to the vessel lid, and the detection end of the temperature sensor is connected to the inside of the vessel body. A pipeline is also connected to the vessel lid. One end of the pipeline is connected to the inside of the vessel body, and the other end of the pipeline is connected to the monitoring end of the pressure sensor outside the oven. S2. Close the oven door and start the oven. The oven heats the vessel body, and the heat is transferred to the heat transfer medium inside the vessel body to form saturated steam. The heat is then transferred to the inner liner, so that the reactants in the inner liner react in a high temperature and high saturated steam pressure reaction environment. Temperature and pressure sensors collect temperature and pressure data in real time and upload them to the controller. The controller compares the preset parameters and adjusts the oven heating mode to maintain the pressure balance between the vessel body and the inner liner. S3. After the reaction is complete, close the oven and cool it down. After cooling, open the oven door, remove the temperature sensor from the lid, remove the pipeline from the lid, remove the body and lid from the oven, remove the bolts on the body and lid, rotate the screws to open the lid, open the lid and take out the inner liner, cut open the welded end of the inner liner and take out the reaction product inside the inner liner.

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