Refractory material multi-component atmosphere erosion resistant reaction device and test method thereof
By designing a reaction device for refractory materials to resist erosion in a multi-component atmosphere, the problem that existing testing methods cannot simulate high-temperature and high-pressure gaseous media has been solved, realizing efficient and accurate testing of the erosion performance of multi-component atmospheres and ensuring that the samples are consistent with actual applications.
Patent Information
- Application Number
- CN202511767565.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-28
- Publication Date
- 2026-02-06
AI Technical Summary
Existing testing methods cannot realistically simulate the dynamic erosion environment of high-temperature and high-pressure gaseous media on refractory materials, and existing devices cannot simultaneously perform lateral comparisons of multi-component atmospheres and on-site molding of refractory materials, resulting in inaccurate test results and low efficiency.
A reaction device for refractory materials to resist erosion by a multi-component atmosphere is designed. The device uses a cylindrical container composed of two to four fan-shaped cylindrical panels, which are spliced together by an Ω-shaped tenon and mortise interlocking structure. The internal partition plate divides the container into multiple reaction chambers. Combined with external pipes, the gas medium and pressure are controlled to simulate actual working conditions. The device can be easily disassembled and assembled, and it is convenient to prepare samples consistent with actual applications.
It enables precise simulation of acidic and reducing atmospheres under high temperature and high pressure, improving testing efficiency and accuracy. It can simultaneously compare the erosion performance under multi-component atmospheres, ensuring the consistency between the sample and actual application.
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Figure CN121476038A_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of refractory performance testing, in particular to a multi-component atmosphere erosion resistance reaction device for refractory and a test method thereof. BACKGROUND
[0002] Hydrogen metallurgy process is a steel smelting technology that uses hydrogen (H2) instead of traditional fossil fuels (such as coke) as a reducing agent and energy carrier. The core goal is to achieve deep decarburization in steel production through "hydrogen instead of carbon" (theoretically reducing CO2 emissions by 80-90%), which is an important measure to achieve the "double carbon target". Currently, the rich hydrogen smelting technology is mainly used, that is, H2, CO and a small amount of methane are used to reduce iron ore. Compared with traditional blast furnace-coking ironmaking, the atmosphere is more complex and contains a certain amount of H2O, which seriously erodes and damages cement-bonded, carbon-containing, and silicon carbide refractories.
[0003] In waste incinerators, coal-to-gas equipment and other high-temperature industrial furnaces, the lining refractories are exposed to a harsh environment of sulfur dioxide, nitrogen oxides and water vapor for a long time. These gases have strong penetration and erosion effects on the lining refractories of the furnace under high temperature and high pressure conditions, significantly shortening their service life.
[0004] Currently, the conventional test methods for the atmosphere erosion resistance of refractories in the industry mainly include liquid immersion and heating furnace combustion simulation. The liquid immersion method involves immersing the refractory sample in an acidic solution for a certain period of time, and then testing the volume density or strength loss rate. However, this test method has a large gap with the actual working conditions. The erosion medium in the actual working conditions is high-temperature gas, which has a large molecular kinetic energy, strong penetration, and a much higher reaction activity with the material surface than liquid acid. In addition, the actual working conditions often involve high system pressure, which further exacerbates the penetration and erosion process of the gas. The existing liquid phase method cannot simulate the dynamic erosion environment of high-temperature and high-pressure gaseous medium, resulting in test results that cannot truly reflect the performance of the refractory in actual use. In the heating furnace combustion simulation test, the existing integral container cannot simultaneously compare multiple-component atmospheres horizontally, and it cannot form a simulated site for the refractory. The refractory samples produced have low consistency with the actual application, making it difficult to accurately and efficiently test the erosion resistance of the refractory in actual working conditions.
[0005] Therefore, we propose a multi-component atmosphere erosion resistance reaction device for refractory and a test method thereof. SUMMARY
[0006] The application aims to provide a refractory material multi-component atmosphere erosion reaction device and a test method thereof, so as to solve the technical problem that the liquid phase method for evaluating the erosion resistance of the refractory material cannot simulate the dynamic erosion environment of the high-temperature and high-pressure gaseous medium, the test result cannot truly reflect the performance of the refractory material in actual use, the existing overall container cannot simultaneously compare the multi-component atmosphere in the transverse direction in the heating furnace combustion simulation test, the refractory material cannot be formed on site, the consistency of the refractory material sample produced with the actual application is low, and the erosion resistance of the refractory material in the actual use condition cannot be accurately and efficiently tested.
[0007] In order to achieve the above-mentioned purpose, the application adopts the following technical scheme: The application provides a refractory material multi-component atmosphere erosion reaction device, which comprises a cylindrical container, the cylindrical container is composed of two to four cylindrical panel segments in the shape of a sector, and two adjacent cylindrical panel segments are connected through a Ω-shaped mortise and tenon engagement structure.
[0008] Preferably, the top of the first baffle is higher than the top of the second baffle, and the part of the first baffle that is higher than the second baffle is bent inward to form a chamfer.
[0009] Preferably, the two first baffles and the two second baffles jointly enclose a sample space for accommodating a refractory material sample.
[0010] Preferably, the cylindrical container is made of heat-resistant steel, the material of the partition plate is quartz or platinum, and the sealing strip is woven from a ceramic fiber rope impregnated with tar or folded and wrapped from a carbon fiber cloth.
[0011] Preferably, the inner surface of the cylindrical container and the inner surface of the end cover are provided with a corrosion-resistant and high-temperature-resistant coating.
[0012] Preferably, the corrosion-resistant and high-temperature-resistant coating is a nano ceramic coating.
[0013] Preferably, the outer wall of the cylindrical panel is provided with a plurality of strip-shaped ribs extending in the circumferential direction thereof, and the strip-shaped ribs on adjacent cylindrical panels are connected through fastening bolts.
[0014] Preferably, the Ω-shaped mortise and tenon joint structure of the cylindrical panel is provided with a sealing groove at the position of the splicing joint.
[0015] Preferably, the external pipe is used for introducing and discharging different reaction media into the reaction chamber and controlling the pressure in the reaction chamber.
[0016] A test method for a refractory material reaction device resistant to multi-component atmosphere erosion, comprising the following steps: S1: splice the cylindrical panels into a cylinder, and install corresponding partition plates and sealing strips to form a multi-cavity structure; S2: evenly smear lubricating grease on the inner wall of the cylindrical panel and the partition plate, then prepare amorphous refractory material or inlay set shaped refractory product samples in the multi-cavity structure by pouring, spraying, ramming or bonding, the thickness of the refractory material is about 50-150mm, a gas flow channel is left near the center of the cylinder, the diameter of the gas flow channel is not less than 40mm, then perform curing, drying and baking; S3: install end covers and external pipes, and fix the strip-shaped ribs by bolts; S4: place the cylindrical container assembled in S3 in a tube furnace, heat to a test temperature, introduce test gas of different combinations of pressure and preheating temperature into each cavity through the external pipes, if necessary, pre-introduce nitrogen or inert gas to replace air before performing the operation; S5: after a period of reaction, introduce nitrogen or inert gas to remove the reaction gas in the cylindrical container, cool the furnace to room temperature, disassemble the cylindrical container, and take out the refractory materials in each cavity, test and compare the reaction depth, apparent porosity, pore size or strength of the refractory materials in each cavity at different depths, and analyze the erosion resistance of the refractory materials in various gas atmospheres.
[0017] Compared with the prior art, the beneficial effects of the present application are: 1、In the present application, the external pipe is used to introduce gas reaction media into the sealed cylindrical container and control the pressure, and the entire device is placed in an external heating furnace, which can accurately simulate the high-temperature, high-pressure acid gas, reducing gas and water vapor atmosphere in the actual industrial environment, overcoming the problem of distorted test results caused by the inconsistency of medium state and pressure conditions in the existing liquid immersion method; 2、In the present application, the container can be easily disassembled and assembled by splicing two to four cylindrical panels through the Ω-shaped mortise and tenon joint structure, which allows the staff to easily prepare or install refractory material samples in the sample space enclosed by the first baffle and the second baffle by pouring, spraying, ramming or bonding, etc., in the disassembled state, so as to directly test the material performance under the forming process consistent with the actual application; 3、The present application, by inserting the partition plate in the clamping groove formed by the first baffle plate adjacent to the two connected cylindrical panels, the internal space of the cylindrical container is flexibly divided into multiple independent reaction chambers, so that in a high temperature and high pressure experiment, a variety of atmosphere, different pressure environment comparison test can be carried out at the same time, greatly improving the test efficiency, and ensuring the consistency of the basic parameters between the test conditions. BRIEF DESCRIPTION OF DRAWINGS
[0018] Figure 1 is the schematic diagram of the overall structure of the present application; Figure 2 is the schematic diagram of the internal structure of the cylindrical container of the present application; Figure 3 is the schematic diagram of the cylindrical panel structure of the present application Figure 2 is the enlarged schematic diagram of the A area in the present application; Figure 4 is the schematic diagram of the cylindrical panel connection structure of the present application; Figure 5 is the enlarged schematic diagram of the B area in the present application; Figure 4 Figure 6 is the schematic diagram of the cylindrical panel structure of the present application Figure 7 is the enlarged schematic diagram of the C area in the present application Figure 6 Figure 8 is the schematic diagram of the rib mounting structure of the present application.
[0019] In the figure: 1, cylindrical container; 2, cylindrical panel; 3, end cover; 4, first baffle plate; 5, clamping groove; 6, second baffle plate; 7, partition plate; 8, external pipe; 9, strip-shaped rib; 10, sealing groove; 11, sealing strip. DETAILED DESCRIPTION
[0020] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all.
[0021] Referring to Figures 1-8 A refractory material reaction device resistant to multi-component atmosphere erosion includes a cylindrical container 1, which is composed of two to four fan-shaped cylindrical panels 2. Adjacent cylindrical panels 2 are connected by an Ω-shaped tenon and mortise interlocking structure. End caps 3 are threadedly installed at both ends of the cylindrical container 1. First baffles 4 are provided along the length direction of the inner walls of the cylindrical panels 2 towards the axis of the cylindrical container 1. The first baffles 4 of two adjacent cylindrical panels 2 are spliced together to form a groove 5. Second baffles 6 are provided at both ends of the cylindrical panels 2 towards the center in the arc direction. A partition plate 7 is inserted into the groove 5, which divides the internal space of the cylindrical container 1 into multiple independent reaction chambers. The end caps 3 are connected to external pipes 8.
[0022] The top height of the first baffle 4 is greater than the top height of the second baffle 6, and the higher part of the first baffle 4 is bent inward to form a chamfer.
[0023] The two first baffles 4 and the two second baffles 6 together form a sample space for accommodating the refractory material sample.
[0024] The cylindrical container 1 is made of heat-resistant steel, the partition plate 7 is made of quartz or platinum, and the sealing strip 11 is made of ceramic fiber rope woven with tar impregnated on the outside or folded and wrapped with carbon fiber cloth.
[0025] The inner surface of the cylindrical container 1 and the inner surface of the end cap 3 are both coated with a corrosion-resistant and high-temperature resistant coating.
[0026] The corrosion-resistant and high-temperature resistant coating is a nano-ceramic coating.
[0027] The outer wall of the cylindrical panel 2 is provided with several strip ribs 9 extending along its circumference, and the strip ribs 9 on adjacent cylindrical panels 2 are connected by fastening bolts.
[0028] A sealing groove 10 is provided at the joint of the Ω-shaped tenon and mortise structure of the cylindrical panel 2; a sealing strip 11 is provided inside the sealing groove 10.
[0029] External fitting 8 is used to introduce and discharge different reaction media into the reaction chamber and to control the pressure inside.
[0030] A test method for a refractory material resistance reaction device to multi-component atmosphere erosion includes the following steps: S1: Assemble the cylindrical panels 2 into a cylinder, and install the corresponding partition plates 7 and sealing strips 11 to form a multi-cavity structure; S2: After uniformly applying grease to the inner wall of the cylindrical panel 2 and the partition plate 7, prepare unshaped refractory materials or embed shaped refractory product samples in the multi-cavity structure by pouring, spraying, tamping or bonding. The thickness of the refractory material is about 50-150mm. An airflow channel is left near the center of the cylinder. The diameter of the airflow channel is not less than 40mm. Then, it is cured, dried and calcined. S3: Install the end cap 3 and external pipe fittings 8, and fix the strip ribs 9 with bolts; S4: Place the cylindrical container 1 assembled in S3 into a tube furnace and heat it to the test temperature. Then, introduce different combinations of test gases with a certain pressure and preheating temperature into each chamber through the external pipe 8. If necessary, nitrogen or inert gas can be introduced in advance to replace the air before this step is performed. S5: After the reaction has been going on for a period of time, nitrogen or inert gas is introduced to remove the reaction gas from the cylindrical container 1. The container is then cooled to room temperature. The cylindrical container 1 is disassembled, and the refractory materials of each chamber are removed. The reaction depth, apparent porosity, pore size or strength of the refractory materials in each chamber are tested and compared to analyze the erosion resistance of the refractory materials in various gases and their combinations.
[0031] Example 1: like Figures 1-8 As shown, the present invention discloses a refractory material resistant to multi-component atmosphere erosion reaction device, comprising a cylindrical container 1 made of CH2132 heat-resistant steel, with a diameter of 450 mm and a height of 300 mm; the cylindrical container 1 is composed of four fan-shaped cylindrical panels 2, each panel being 8 mm thick; adjacent cylindrical panels 2 are connected by an Ω-shaped tenon and mortise interlocking structure; the cylindrical container 1 has external threads at its upper and lower ends; two end caps 3 have 20 mm long internal threads on their inner walls for connection with the external threads at the upper and lower ends of the cylindrical container 1; the inner surface of the cylindrical container 1 is coated with a high-temperature alumina coating; the inner edges of the cylindrical panels 2 extend along their length towards the center. A first baffle 4 extends along the axis of the cylindrical container 1. The first baffles 4 of two adjacent cylindrical panels 2 are joined together to form a slot 5. Second baffles 6 extend from the arcs at both ends of the cylindrical panels 2 toward the center. The two first baffles 4 and the two second baffles 6 together form a sample space for accommodating refractory material samples. A platinum sheet-like partition 7, 1 mm thick, can be inserted into the slot 5 to divide the internal space of the cylindrical container 1 into multiple independent reaction chambers. An external pipe 8 is connected to the end cap 3 and is used to introduce and discharge different reaction media into the four independent reaction chambers divided by the partition 7 inside the cylindrical container 1 and to control the pressure within them.
[0032] After applying grease to the inner walls of the four reaction chambers, a 20mm thick layer of low-cement corundum castable was poured into each chamber. After solidification, the prepared corundum mullite brick test blocks were bonded and embedded into the low-cement corundum castable using corundum putty. The corundum mullite test blocks were 65mm*65mm*114mm in size, with a square cross-section embedded in the low-cement castable, and the length direction pointing towards the axis of the cylindrical container 1. The corundum putty and corundum mullite bricks used for embedding were of uniform height, so that the corundum mullite bricks were flush with the upper surface of the corundum putty. Three test blocks were embedded in each chamber. After curing and drying, the next step of the experiment was carried out.
[0033] After inserting the partition plate 7 into the slot 5, assemble the cylindrical container 1 and place it in the tube furnace. Heat at a rate of 10℃ / min until it reaches 1000℃ and holds. While heating, evacuate the furnace, then introduce nitrogen into the four chambers, evacuate again, and introduce nitrogen again, maintaining the pressure until the holding temperature is reached. Then, introduce H2, CO, high-temperature water vapor, and a mixture of H2, CO, and high-temperature water vapor into each chamber respectively until the pressure reaches 0.7 MPa. Hold for 200 hours, then turn off the power to the tube furnace and switch the gas source to nitrogen. After purging with nitrogen for 30 minutes, turn off the gas source and allow the furnace to cool to room temperature.
[0034] Disassemble cylindrical container 1, remove the corundum-mullite brick specimen, and cut the specimen into two pieces (32mm × 65mm × 114mm) along the centerline. Measure the reaction layer depth of each chamber specimen and record the crack condition. Along the centerline of the cross-section, prepare a 20mm × 20mm × 20mm cube specimen every 10mm for apparent porosity testing. After drying, conduct a compressive strength test. Evaluate its resistance to erosion in reducing atmosphere based on changes in reaction layer depth, cracks, porosity, and compressive strength. Based on the performance characterization under different atmospheres, targeted improvements can be made to enhance the material's properties.
[0035] Example 2: like Figures 1-8As shown, the present invention discloses a refractory material resistant to multi-component atmosphere erosion reaction device, comprising a cylindrical container 1 made of 310S stainless steel, with a diameter of 300mm and a height of 200mm; the cylindrical container 1 is composed of two semi-circular cylindrical panels 2 of the same size, each panel being 5mm thick; adjacent cylindrical panels 2 are connected by an Ω-shaped tenon and mortise interlocking structure; the upper and lower ends of the cylindrical container 1 are provided with 15mm long external threads; two end caps 3 are provided with corresponding internal threads on their inner walls for connection with the upper and lower ends of the cylindrical container 1; the inner surface of the cylindrical container 1 is provided with a carbon-silicon nitride nano-coating; the two sides of the inner wall of the cylindrical panel 2 extend along the length direction towards the axis of the cylindrical container 1. A first baffle 4 is provided at the position extension, and the first baffle 4 of two adjacent cylindrical panels 2 are spliced together to form a slot 5; a second baffle 6 is provided at the two ends of the cylindrical panel 2 extending towards the center position in the arc direction, and the two first baffles 4 and the two second baffles 6 together form a sample space for accommodating refractory material samples; a quartz partition plate 7 can be inserted into the slot 5 to divide the internal space of the cylindrical container 1 into two independent reaction chambers; an external pipe 8 is connected to the end cap 3 and is used to introduce and discharge high temperature HCl, high temperature water vapor and HCl mixed gas into the two independent reaction chambers divided by the partition plate 7 in the cylindrical container 1 respectively; acid-resistant sprayed refractory material is installed in the sample space by spraying.
[0036] During the test, the inner walls of the two reaction chambers were coated with grease, and then a layer of flue acid-resistant coating with a thickness of about 100mm was sprayed on. After the surface was repaired, cured and dried, the next step of the test was carried out.
[0037] After inserting the partition plate 7 into the slot 5, assemble the cylindrical container 1 and place it in a tube furnace. Heat it at a rate of 10℃ / min until it reaches 600℃ and hold it thereafter. Then, introduce HCl, high-temperature water vapor, and HCl gas into the two chambers respectively until the pressure reaches 0.15 MPa. Hold the temperature for 50 hours, turn off the power to the tube furnace, and switch the gas source to argon. After 15 minutes, turn off the gas source and allow the furnace to cool to room temperature.
[0038] Disassemble cylindrical container 1, remove the acid-resistant coating sample block from the flue, and cut the sample into two identical pieces along the centerline of its length. Measure the reaction layer depth of each chamber sample and record the crack condition. Along the centerline of the cross-section, prepare cylindrical samples with a diameter of 20 mm and a height of 20 mm every 10 mm for apparent porosity testing. After repeated washing and drying, perform a compressive strength test and simultaneously test the pore size distribution at this location. Evaluate its acid atmosphere corrosion resistance performance based on changes in reaction layer depth, crack condition, porosity, compressive strength, and pore size distribution. Based on the performance characterization under different atmospheres, targeted improvements can be made to enhance the material's properties.
[0039] It is understood that the present invention has been described through some embodiments, and those skilled in the art will recognize that various changes or equivalent substitutions can be made to these features and embodiments without departing from the spirit and scope of the invention. Furthermore, under the teachings of the present invention, these features and embodiments can be modified to adapt to specific situations and materials without departing from the spirit and scope of the invention. Therefore, the present invention is not limited to the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are within the protection scope of the present invention.
Claims
1. A refractory material erosion-resistant multi-component atmosphere reaction device, comprising a cylindrical container, characterized in that, The cylindrical container is composed of two to four fan-shaped cylindrical panels, with adjacent cylindrical panels slidingly connected by an Ω-shaped tenon and mortise interlocking structure. End caps are threaded onto both the top and bottom ends of the cylindrical container. First baffles extend along the length of the inner walls of the cylindrical panels towards the axis of the cylindrical container, and the first baffles of two adjacent cylindrical panels are joined to form a groove. Second baffles extend from the arcs at both ends of the cylindrical panels towards the center, and partition plates are inserted into the grooves, dividing the internal space of the cylindrical container into multiple independent reaction chambers. External pipes are connected to the end caps.
2. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, The top height of the first baffle is greater than the top height of the second baffle, and the higher part of the first baffle bends inward to form a chamfer.
3. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, The two first baffles and the two second baffles together form a sample space for accommodating the refractory material sample.
4. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, The cylindrical container is made of heat-resistant steel, the partition is made of quartz or platinum, and the sealing strip is made of ceramic fiber rope woven with tar impregnated on the outside or folded and wrapped with carbon fiber cloth.
5. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, The inner surface of the cylindrical container and the inner surface of the end cap are both coated with an anti-corrosion and high-temperature resistant coating.
6. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 5, characterized in that, The corrosion-resistant and high-temperature resistant coating is a nano-ceramic coating.
7. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, The outer wall of the cylindrical panel is provided with a number of strip ribs extending along its circumference, and the strip ribs on adjacent cylindrical panels are connected by fastening bolts.
8. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, A sealing groove is provided at the joint of the Ω-shaped tenon and mortise structure of the cylindrical panel; a sealing strip is provided in the sealing groove.
9. The refractory material erosion-resistant multi-component atmosphere reaction device according to claim 1, characterized in that, The external tubing is used to introduce and discharge different reaction media into the reaction chamber and to control the pressure within it.
10. A test method for a reaction apparatus for refractory materials to resist erosion by a multi-component atmosphere, characterized in that, Includes the following steps: S1: Assemble the cylindrical panels into a cylinder, and install the corresponding partition plates and sealing strips to form a multi-cavity structure; S2: After uniformly applying grease to the inner wall and partition plate of the cylindrical panel, prepare unshaped refractory materials or embed shaped refractory product samples in the multi-cavity structure by pouring, spraying, tamping or bonding. The thickness of the refractory material is about 50-150mm. An airflow channel is left near the center of the cylinder. The diameter of the airflow channel is not less than 40mm. Then, it is cured, dried and calcined. S3: Install the end caps and external pipe fittings, and fix the strip ribs with bolts; S4: Place the cylindrical container assembled in S3 into a tube furnace and heat it to the test temperature. Then, introduce different combinations of test gases with a certain pressure and preheating temperature into each chamber through external pipes. If necessary, nitrogen or inert gas can be introduced in advance to replace the air before proceeding with this step. S5: After the reaction has proceeded for a period of time, nitrogen or inert gas is introduced to remove the reaction gas from the cylindrical container. The container is then cooled to room temperature. The cylindrical container is disassembled, and the refractory materials of each chamber are removed. The reaction depth, apparent porosity, pore size, or strength of the refractory materials in each chamber are tested and compared to analyze the erosion resistance of the refractory materials in various gases and their combinations.