CN114459985A - Method and device for testing slag and steam erosion resistance of refractory material - Google Patents
Method and device for testing slag and steam erosion resistance of refractory material Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B15/00—Measuring arrangements characterised by the use of electromagnetic waves or particle radiation, e.g. by the use of microwaves, X-rays, gamma rays or electrons
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The invention belongs to the technical field of refractory materials, and relates to a method and a device for testing slag and steam erosion resistance of a refractory material. Fixing a cylindrical sample of the refractory material to be detected, which is filled with a slag sample at the periphery, in a sealing assembly, placing one end of the sealing assembly in a hearth heating area, and extending the other end of the sealing assembly out of a furnace wall, forming slag and steam in the heating process of the heat-resistant steel sealing assembly, and generating a temperature gradient on the refractory material sample so as to evaluate the corrosivity of the slag and the steam to the refractory material in a specific temperature and time range; the sealing assembly is an L-shaped splicing body formed by 2 sections of cylinders and comprises a vertical section and a horizontal section which are communicated with each other, a refractory sample to be tested and loaded in the vertical section is immersed in slag liquid to resist slag corrosion of a melt, and a sample loaded in the horizontal section resists steam infiltration corrosion. The invention is easy to operate and visual, and the test device is simple and safe.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and mainly relates to a method and a device for testing slag and steam erosion resistance of a refractory material.
Background
The refractory material is an important component in the high-temperature kiln, has higher refractoriness, and is often used as a furnace lining material of a fire facing surface of the high-temperature kiln; because the high-temperature kiln is often used as a preparation container for metallurgy, coal gasification, glass and the like, the lining material is inevitably contacted with raw materials or slag in the kiln in the process, the process is a complex process with coupled multiple factors, and the specific expression comprises chemical erosion of the slag on the surface of the material; the solid, liquid and gas in the furnace physically permeate the material along the material pores; and physical and chemical property changes of the material caused by chemical erosion and physical infiltration, which may cause damage of the material finally. In order to prolong the service life of the refractory material in the high-temperature kiln, the test and evaluation of the high-temperature slag resistance of the refractory material are always one of important reference indexes of the service performance of the refractory material of the furnace lining.
The current national standard GB/T8931-2007 refractory material slag resistance test method provides a plurality of slag resistance test methods, wherein the most widely applied method is a static crucible method, the refractory material is prepared into a crucible with a certain specification, slag is filled in the crucible, the crucible is heated to a certain temperature, so that the slag directly contacts and reacts with the crucible wall at a high temperature and permeates into the crucible along a crucible gas hole, and the slag resistance of the material is judged according to the contact surface erosion area and the permeation layer area. The method is simple and easy to operate, can visually compare the erosion and permeability degrees of the slag on different refractory materials, has strong test repeatability, and has certain limitations: on one hand, the crucible is required to be integrally placed in a hearth during heat treatment and heated by a heating element of a furnace body, and the crucible wall has no temperature gradient, so that the reaction of slag and materials is under a single influence factor; on the other hand, tests can only simulate the erosion behaviour of the slag at high temperatures on the surface of the material and the infiltration behaviour inside the material, not correctly captured for the gas phase erosion or infiltration present in the actual production. Another common slag resistance test method is a rotary slag etching method, in which a plurality of refractory materials are cut and spliced into a hollow prismatic shape and are placed in a rotary furnace, a furnace body is heated by unidirectional flame, the furnace body rotates continuously in the test process, and the erosion and permeation behaviors of slag on the materials are simulated by manual slag adding and slag dumping. The method can simulate the scouring effect of the slag on the surface of the material, is a dynamic slag-resistant test method, is more suitable for the actual working condition than a static method, has limitations and mainly comprises the following steps: firstly, because the test material is prepared into a hollow prismatic shape, the whole test process is an open type, the temperature fluctuation is difficult to control, and the process atmosphere is difficult to regulate and control; secondly, the slag is only in direct contact with the material, so that a multiphase erosion process does not exist, and particularly, the gas phase can be lost along with an open environment; and thirdly, the test time span is long, the test cost is too high, and the test risk is larger.
The slag resistance is the key service performance of the refractory material, and as the action process of slag and the material is influenced by multiple factors, researchers make targeted optimization and improvement on the slag resistance test based on the current standard. Chinese patent a refractory material high temperature anti-erosion test method and test device (application No. 201110331284.9) propose one hang and soak the material in the crucible container wholly, the container is the slag, hang the material and rotate continuously to imitate the material and receive the effect that the slag erodees, it is a kind of dynamic slag resistance test method, it is more controllable than atmosphere and temperature of the rotary slag etching method, but still there is the problem that only liquid phase slag contacts with material; a refractory material slag-resistance test method (application number 201610018216.X) in Chinese patent provides a static slag-resistance test method by heating in an intermediate frequency furnace, wherein a material is made into an annular wall, a hollow ring is formed by surrounding the annular wall, an iron block and slag are filled in the ring, the iron block is melted by an intermediate frequency furnace electromagnetic heating mode, the temperature of the slag-resistance test is transmitted from inside to outside, the temperature gradient change on the annular wall of the material can be realized, but the slag-resistance test temperature of metals such as the iron block is higher than the melting temperature of the iron block due to the fact that the melting temperature of the metals such as the iron block is higher than 1450 ℃, and the use range of the metals is influenced.
The rotary kiln system for hazardous waste treatment is a hazardous waste kiln furnace type which is highly concerned in recent years, the working temperature of the rotary kiln furnace is generally 800-1200 ℃, and the rotary kiln system is used for treating various hazardous wastes such as plastics, papermaking waste liquid, sludge and the like. Because the types of the treated materials are complicated, the chemical composition of the burned ash is complex, and especially a large amount of alkali metal oxides and halogen salts exist in waste liquid of plastics and paper making industry, because the working temperature is lower, oxide phases in the ash are difficult to melt, but the alkali metal oxides and the halogen salts such as NaCl can be converted into liquid phase or even gas phase at a lower temperature about 800 ℃, the permeability of the substances is far higher than that of oxide slag, and the substances can directly permeate into intercrystalline spaces of material aggregates to react with crystalline grains, thereby damaging the structure of the aggregates; on the other hand, because the lining material of the high-temperature kiln generally has a temperature gradient from inside to outside, the contact form, the erosion reaction type and the product of the alkali metal oxide and the halogen salt and the material are greatly different at different temperatures, and the thermal expansion property change of the material caused by the difference can cause the thermal expansion mismatch of different parts of the material, thereby causing physical damage. The slag erosion and infiltration mechanism of the kiln is completely different from the slag erosion and infiltration mechanism of other existing high-temperature kilns, and the slag resistance of the refractory material for the hazardous waste rotary kiln is difficult to visually evaluate by relying on the existing slag resistance test method, and is mainly reflected in that: firstly, the forms of reactants are different, because the temperature of a kiln is low, substances which have the penetrating action in the hazardous waste rotary kiln are mainly alkali metal oxides with low melting points, halogen salts and the like, oxide substances are only possibly contacted with the surface of a material because the melting points are not reached, and the existing static crucible method is difficult to realize the multi-phase contact of solid, liquid and gas phase slag and the material; secondly, the influence of temperature gradient, in the existing slag resistance test method, most of the heat sources heat the crucible or the material sample from outside and inside, the material is at a certain specific test temperature, and the influence of the temperature gradient on the contact and reaction type of the material and the slag is difficult to evaluate, although the aforementioned Chinese patent 201618216. X adopts an internal heating mode to realize the influence of the temperature gradient, the influence is difficult to be applied to the lower working temperature of the dangerous waste rotary kiln due to the limitation of the melting point of the iron block.
Disclosure of Invention
In order to solve the above technical problems, the present invention provides a method and an apparatus for testing the erosion resistance of refractory material against slag and steam, which can simultaneously perform contact reaction of 3 forms of solid, liquid and gas of slag under a certain temperature gradient with refractory material, and evaluate the contact condition and reaction type of slag and refractory material under different temperature gradients.
The invention adopts the following technical scheme for achieving the purpose:
a refractory material slag and steam erosion resistance test method is used for representing chemical reaction, dissolution and permeation of high-temperature slag and steam generated by the high-temperature slag to a static refractory material sample under the conditions of gravity and temperature gradient;
the apparent porosity of the refractory material is 10-20%, and the normal-temperature compressive strength is more than or equal to 1.0 MPa; the slag is oxide mixture, inorganic salt or mixture of the oxide mixture and the inorganic salt; the test method comprises the steps of fixing a cylindrical sample of the refractory material to be detected, filled with a slag sample, in a sealing assembly, placing one end of the sealing assembly in a hearth heating area, extending the other end of the sealing assembly out of a furnace wall, forming slag and steam in the heating process of the heat-resistant steel sealing assembly, and generating a temperature gradient on the refractory material sample so as to evaluate the corrosivity of the slag and the steam to the refractory material in a specific temperature and time range; the sealing assembly is an L-shaped splicing body formed by 2 sections of cylinders and comprises a vertical section and a horizontal section which are communicated with each other, a refractory sample to be tested and loaded in the vertical section is immersed in slag liquid to resist slag corrosion of a melt, and a sample loaded in the horizontal section resists steam infiltration corrosion; the refractory material samples have temperature difference in the test, the vertical section samples are at constant temperature, and the horizontal section samples have temperature gradient from the part close to the vertical section to the part far away from the vertical section; the test result of the test method is processed by taking out vertical section and horizontal section samples after the temperature of the furnace reaches room temperature after the test is finished, measuring and calculating the mass change, volume change and diameter change of the samples before and after the test, and evaluating and comparing the slag and steam erosion resistance of different materials by assisting the analysis means of scanning electron microscope and X-ray diffraction instruments; the method for testing the slag and steam erosion resistance of the refractory material comprises the following specific steps:
firstly, preparing 2 cylindrical refractory material samples with the same material and size, wherein the size of a cylinder is phi 50-100 mm multiplied by h 100-230 mm, measuring the initial mass, volume and diameter of the samples, and sampling from samples with the same specification to carry out microstructure and phase composition analysis;
secondly, respectively placing the 2 cylinders into a vertical section and a horizontal section of a heat-resistant steel sealed container, then adding test slag into the vertical section, wherein the slag filling amount is 1/2-2/3 of the height of the cylinder of the vertical section, and sealing;
thirdly, placing the sealed container filled with the sample and the slag into a test device, placing the vertical section in a hearth with a heating body, and extending the horizontal section out of a kiln wall or a kiln door;
fourthly, heating the hearth to a test temperature and preserving heat, wherein the test temperature is 800-1200 ℃, and the preserving heat time is 3-24 hours;
and fifthly, taking out the sealed container from the test device after natural cooling, taking out the refractory material sample after dismantling for measuring the mass, the volume and the diameter, or analyzing by an instrument to give out the evaluation of erosion resistance.
A method for testing the slag and steam corrosion resistance of refractory materials, a fifth step of analysis by means of instruments,
cutting the vertical section sample along the side surface of the cylindrical sample according to the slag filling amount and the height of the vertical section sample according to the existence or non-existence of direct contact slag; equally cutting the cut samples which are not in direct contact with the slag and the samples which are in direct contact with the slag respectively along the axial direction of the samples; respectively calculating erosion area and penetration area of the directly contacted slag sample, analyzing the microstructure and phase composition of an erosion area and a penetration area of the directly contacted slag sample by adopting a scanning electron microscope and energy spectrum analysis equipment, calculating the steam penetration area of the indirectly contacted slag sample, and analyzing the microstructure and phase composition of the penetration area and the non-penetration area of the directly contacted slag sample by adopting the scanning electron microscope and the energy spectrum analysis equipment; and cutting the horizontal section sample along the side surface of the sample in trisection, drilling a cylindrical sample at the center of the cut cylinder respectively, testing the thermal expansion of the cylindrical sample, cutting the rest samples in trisection along the axial direction of the cylindrical sample, and analyzing the permeable area and the non-permeable area of the cylindrical sample by adopting the same method as the analysis method of the vertical section sample which is not directly contacted with the slag sample. And comprehensively evaluating the quality of the slag and steam corrosion resistance of the sample according to the analysis result of each sample.
A method for testing the erosion resistance of refractory material to molten slag and steam is provided, two L-shaped sealed containers at two ends are adopted to simultaneously accommodate two samples of a vertical section and a horizontal section, the vertical section is placed in a heatable hearth and the hearth is sealed by a furnace door brick, so that the whole vertical section sample of the sealed container is ensured to be at a certain set temperature, and the horizontal section extends out of the furnace door to create a natural temperature gradient from high to low in the horizontal direction and is closer to the actual working condition of the refractory material in a thermal device; the part of the horizontal section of the sealed container, which extends out of the furnace door brick, is filled with heat insulation materials so as to further fix the sealed container and avoid the temperature gradient distortion of the sample caused by the too fast heat dissipation of the horizontal section; the refractory material sample is required to be cylindrical, and the reason is that slag and steam are uniformly contacted with the sample at each position, so that permeation and erosion behaviors can be uniformly generated from outside to inside, uneven erosion caused by the shape of the sample is avoided, and the measurement accuracy of the volume, the diameter and the like of the refractory material sample before and after a test is facilitated; the refractory material sample is required to have a certain diameter because the phenomenon that the erosion area, the permeation area and the unreacted area are distinguished when the material analysis is influenced due to the fact that the erosion speed of slag and steam is too fast is avoided, the refractory material sample is required to have a certain height because the heat transfer process of the horizontal section sample is too fast and temperature gradient change is difficult to create due to the fact that the height is insufficient, the difficulty of preparing the sample is increased if the height is too high, the consumption of raw materials of a sealing container used in a matching mode and the size of a hearth are increased, and the control of test cost is not facilitated; the slag filling amount is required to be in a certain range, and the reasons are that the slag filling amount is prevented from being too small, the content of slag and steam is too low, the degree of corrosion and permeation is difficult to effectively evaluate, and the test requirement that a vertical section sample is contacted with solid, liquid and gas slag in 3 forms due to too much slag filling is also prevented from being inconsistent; the test temperature is required to be 800-1200 ℃, because if the temperature is too low, salts with lower melting points in the slag are difficult to liquefy or gasify, oxides with higher melting points are more difficult to form slag, which is contrary to the test purpose, and if the temperature is too high, the sealed container using heat-resistant steel as a raw material is softened, oxidized, peeled and the like, thereby affecting the test effect.
A refractory material slag and steam erosion resistance test device is provided, wherein a hearth is formed in an internal cavity of a normal-pressure heat treatment electric furnace of the test device; the inner wall of the hearth is provided with a heat-insulating furnace lining, and the heating mode is that a heating element is adopted to carry out electric heating in the hearth; monitoring the temperature of each temperature section by adopting a thermocouple and a temperature display device; the testing container is placed in the hearth, the testing container is made of alloy steel resistant to high temperature of 1200 ℃, the wall thickness of the container is 3-5mm, the container is a two-section cylindrical container and consists of a vertical section, a horizontal section and a base, the inner diameter phi of the vertical section is 70-120 mm, the height h is 140-270 mm, the upper opening of the vertical section is provided with a screwed cap, and the horizontal section is of a broken bridge type structure which adopts a corundum ceramic tube and is assembled with a testing container material: the first section, the third section and the fifth section are made of test container materials, wherein the first section is communicated with the vertical section, and the specification of the third section is as follows: phi is 70-120 mm multiplied by h 40-80 mm, the second section and the fourth section are corundum ceramic tubes, the inner diameter of each corundum ceramic tube is the same as the outer diameter of the rest three sections of materials, the specifications are that the inner diameter phi is 73-125 mm multiplied by h 20-30 mm, the wall thickness of each corundum ceramic tube is 3-5mm, and the side opening of the horizontal section is provided with a threaded screw cap which is provided with a hole and can be connected with a tail gas treatment device; the first, third and fifth sections of the horizontal section are provided with a baffle and a gasket; during the test, the furnace door is filled and plugged by furnace door bricks and refractory fibers which are made of the same materials as the heat-insulating lining and provided with holes, so that the furnace is insulated and the test container is fixed.
The base of the test container is a crucible made of alloy steel which can resist the high temperature of 1200 ℃; the purpose is to prevent the slag liquid from leaking out suddenly to pollute the hearth in the test.
The horizontal section of the test container is high in cold end and low in hot end, and an inclination angle of 5-10 degrees is formed between the horizontal section and the horizontal plane, so that condensed slag liquid or water can flow back conveniently.
The horizontal section of the test container, the part of which extends out of the furnace door brick, can be provided with an electric heating wire and a heating device or a water cooling tube and a water cooling system for controllably adjusting the temperature gradient, wherein the electric heating wire and the horizontal section need to be isolated by insulating fibers so as to prevent the heating device from being incapable of normally operating; the area of the horizontal section extending out of the furnace door brick is additionally provided with the heating wire and the water cooling pipe, controllable temperature gradient adjustment can be realized according to test requirements, temperature circulation and temperature fluctuation caused by furnace body rotation or opening and stopping in some practical kilns can be simulated, and the practical working conditions of the kilns are more fitted.
The refractory material slag and steam resistance test device can be used for simultaneously placing a plurality of groups of test containers according to the size of a hearth so as to perform parallel tests among multiple materials under the same test condition.
A refractory material slag and steam erosion resistance test device adopts two sections of cylindrical alloy steel materials which are communicated with each other as a test container, the cylindrical container is designed to create a uniform contact environment between a sample and slag, and the alloy steel is adopted as the container material to avoid the influence of the reaction between oxide slag and the test container after contacting the wall of the test container on the service life of the container and the test result; the vertical section and the horizontal section of the test container are required to have certain size specifications so as to ensure that the test material can be placed in the container and a certain slag filling space is reserved, and the influence on the test result caused by excessive or insufficient slag filling amount is avoided; the horizontal section of the test container is provided with a 'bridge-cut structure' which is formed by matching alloy steel materials and corundum ceramic tube materials, so that a heat bridge is formed in the horizontal section in order to avoid the situation that all the alloy steel materials and the corundum ceramic tube materials are made of metal materials, the normal temperature gradient of the test material is influenced to change from a hot end to a cold end, and the test sample can be fixed and less directly contacts the wall of the metal container by designing a baffle structure and a liner structure; the heating wires and the water cooling tubes are arranged at the horizontal section of the test container, so that the temperature gradient change can be controlled according to the test requirements, and the temperature data of the sample can be collected in real time by the thermocouples arranged at all positions of the device.
The invention provides a test method and a test device for slag and steam corrosion resistance of a refractory material, which can more closely simulate the corrosion and permeation of salt-containing melt and steam to the furnace wall of a furnace in practical application under a high-temperature environment, and more accurately and comprehensively evaluate the slag resistance of the refractory material in a medium-low temperature furnace. The test method is easy to operate and visual, and the test device is simple and safe.
Drawings
FIG. 1 is a schematic structural diagram of the testing apparatus of the present invention.
FIG. 2 is a schematic view showing an analysis method of a test sample in the test method of the present invention.
In the figure: 1. the device comprises a corundum-mullite furnace, 2, a heating element, 3, a rotary cover, 4, a test container, 5, a base, 6, a sample, 7, test slag, 8, a furnace door brick, 9, refractory fibers, 10, a baffle plate and a gasket, 11, an electric heating wire and a heating device, 12, a water cooling pipe and a water cooling system, 13, an exhaust gas treatment device, 14, a corundum ceramic pipe, 15, a thermocouple and a temperature display device, 16, a threaded rotary cover, 17, a vertical section sample, 18, a horizontal section sample, 19, an erosion area, 20, a permeation area, 21, a steam permeation area, 22, a cylindrical sample, 23 and a permeation area.
Detailed Description
The invention is described in detail with reference to the accompanying drawings and specific embodiments:
example 1:
as shown in figure 1, the refractory material slag and steam erosion resistance test device comprises a heating furnace, a furnace body and a heating element, wherein the heating furnace is an electric furnace with a cavity inside, the inner wall of the furnace cavity is a corundum mullite furnace lining 1, and a molybdenum disilicide rod is used as a heating element 2 of the heating furnace; a set of K-type thermocouple group 15 is arranged at the central position in the hearth to monitor the temperature in the hearth; a test container 4 made of 310s heat-resistant steel is placed in the hearth, the wall thickness of the container is 5mm, the container is a two-section cylindrical container and consists of a vertical section, a horizontal section and a base 5, the vertical section is of an internal diameter phi 80mm h180mm, the upper opening of the vertical section is of a threaded rotary cover 3 structure, the horizontal section is of a broken bridge type structure formed by combining and sleeving a corundum ceramic tube 14 and a test container material, the first section, the third section and the fifth section are test container materials, the first section is communicated with the vertical section, the third section is of a phi 80mm h65mm, the second section and the fourth section are corundum ceramic tubes, the internal diameter of the corundum ceramic tube is the same as the external diameter of the rest three sections, the specification is an internal diameter phi 85mm h30mm, the wall thickness of the corundum ceramic tube is 5mm, and the lengths of the first section, the third section and the fifth section which are sleeved with the corundum ceramic tube are 5 mm; the side port of the horizontal section is provided with a threaded screw cap 16 structure which is provided with a hole, an air pipe is connected into the hole and communicated with a tail gas treatment device 13 for filtering, collecting and balancing the internal and external pressure of the test container for waste gas generated in the test; the first, third and fifth sections of the horizontal section are provided with a baffle and liner 10 structure; during testing, the hearth is plugged by a corundum-mullite furnace door brick 8 with a hole, the diameter of the hole is 95mm, the punching angle is 5 degrees, a hole gap is plugged by refractory fibers after the furnace door brick is sleeved in a horizontal section of a testing container, the horizontal section of the testing container extending out of the furnace door brick is filled and fixed by refractory fibers 9, and two K-type thermocouple groups are respectively arranged in third and fifth sections of alloy steel material sections of the horizontal section for real-time temperature monitoring.
The test container base is made of a 310s heat-resistant steel crucible with the inner diameter phi of 90mm and the wall thickness of 5mm and is welded at the bottom of the vertical section of the test container;
the horizontal section of the test container has an inclination angle of 5 degrees, so that slag liquid, steam and the like can conveniently flow back after being condensed;
the vertical section upper opening screw cap, the horizontal section side opening screw cap, the horizontal section baffle and the horizontal section gasket are all made of 310s heat-resistant steel materials;
a third section of the horizontal section of the test container, which extends out of the furnace door brick, is provided with a nickel-chromium heating wire and heating device 11, a fifth section is provided with a cooling water pipe and a circulating water cooling system 12, wherein the outside of a third section of metal pipe is coated with insulating fibers, so that the heating wire is prevented from being in direct contact with the metal pipe;
the device can contain two sets of test containers for testing, and the arrangement mode, specification and size and matching devices of the two sets of test containers are consistent.
The highest operation temperature of the hazardous waste treatment rotary kiln system is about 1100 ℃, in the process of carrying out hazardous waste incineration treatment, a large amount of alkali metal oxides and inorganic salts exist in bottom slag and fly ash, the corrosion and the permeation of a furnace lining refractory material are serious, the influence of the inorganic salts on the physical properties of the material after the inorganic salts permeate, especially on the thermal expansion property is particularly serious, the temperature circulation and the temperature fluctuation caused by the rotation of a furnace body in the furnace are great, and the structural stability of the material is seriously influenced by the change of the thermal expansion property. The erosion resistance of the chromium corundum brick under the working condition with the apparent porosity of 16% and the normal-temperature compressive strength of 96MPa is evaluated by adopting the refractory material slag and steam erosion resistance test device.
The specific test steps are as follows:
firstly, analyzing the microstructure and phase composition of the chrome corundum brick to be tested, wherein the main phase of the chrome corundum brick comprises Al2O3-Cr2O3Solid solutions, corundum, and monoclinic zirconium; preparing the chrome corundum brick into 2 cylindrical samples with the diameter of 50mm x 150mm, respectively setting the samples as a sample A and a sample B, and measuring the mass and the diameters of the upper, middle and lower sides of the samples;
secondly, placing the sample A in a vertical section of a test container, placing the sample B in a horizontal section of the test container, after the sample is fixed and the position is proper, adding test slag into the vertical section, wherein the test slag is bottom slag and fly ash collected by the dangerous waste rotary kiln, the melting point of the slag is 1180 ℃, the slag filling amount is 75mm, namely 1/2 of the height of the sample A, and screwing and sealing an upper opening of the vertical section;
thirdly, placing the test container in a hearth of a heating furnace, wherein the horizontal section of the test container extends out of a furnace door, plugging the heating furnace by using a furnace door brick with a hole, screwing a side opening screw cover of the horizontal section of the test container, connecting an air pipe of a tail gas treatment system, and filling and fixing the part of the horizontal section extending out of the furnace door brick by using refractory fibers;
fourthly, setting the test temperature to be 1100 ℃, heating the hearth to 1100 ℃ and preserving heat for 5 hours;
fifthly, naturally cooling the hearth after heat preservation is finished, taking out a test container, taking out A, B samples, and respectively measuring the tested mass and the diameters of the upper side, the middle side and the lower side; the A, B sample was further analyzed by the instrument.
A. The changes in mass, diameter, etc. before and after the test of the two samples B are shown in Table 1.
TABLE 1 Change in Mass and diameter of samples before and after testing
Comparing the data, finding that the sample A, B is increased in weight after the test, wherein the sample A is increased in weight more, and the 1/2 sample of the sample A is directly contacted with the slag, so that the permeation of liquid-phase substances in the slag to the materials is the main reason for the weight increase; the diameter of the sample A in the middle section and the lower section is greatly changed, the middle section is positioned at the joint action position of 3 solid-liquid-gas slag, and the sample is expanded.
The A, B samples were further analyzed in conjunction with the instrument, as shown in FIG. 2, by cutting the vertical section A sample 17 equally along the side of the cylinder into the upper half of the A1 vertical section and the lower half of the A2 vertical section; equally cutting the cut upper and lower samples along the axial direction; respectively calculating an erosion area 19 and a penetration area 20 of an A1 sample to obtain an erosion area of 9.6% and a penetration area of 39.8%, analyzing the microscopic morphology and phase composition of an erosion area and a penetration area of the A1 sample by using a scanning electron microscope and energy spectrum analysis equipment, finding that erosion mainly occurs on the surface of the material, both the matrix and particles of the material are eroded to a certain degree, part of the particles have a dissolution tendency, the glass phase and NaCl mainly permeate into the material, and the phenomenon that the material in the penetration area is eroded is less; a2 sample is cut open, and a permeable area cannot be directly observed, so that a scanning electron microscope and an energy spectrum analysis device are adopted to analyze the microscopic morphology and phase composition of the permeable area and the non-permeable area, the sample is found to have a violent reaction of particles at a position close to the slag filling height, the phase penetrating into the material still takes a glass phase and NaCl as main components, the material particles have obvious expansion cracks, nepheline substances are formed, and the material has a permeation phenomenon both inside and outside, which indicates that the permeation degree of steam is very large. The B sample 18 is cut into a high temperature end of a B1 horizontal section, a middle section of a B2 horizontal section and a low temperature end of a B3 horizontal section along the side face of the sample in trisection, a cylindrical sample 22 with the specification of phi 10mm h50mm is respectively drilled at the center of a cut cylinder, and the thermal expansion rate of the cylindrical sample at 1100 ℃ is tested, and the result is as follows: b1:1.204 percent; 1.039% of B2; b3: 1.028%, and the thermal expansion rate of a comparative sample not tested is 1.005%, which shows that the physical properties of the material are influenced to a certain extent after the material is permeated by steam, and the thermal expansion rates of different sections of samples are not changed uniformly due to the existence of temperature gradient; the residual samples are respectively cut along the axial direction thereof in an equal way, the permeable area 23 and the non-permeable area are analyzed by the same method as the analysis method of the slag sample which is not directly contacted with the vertical section, and the result shows that the permeate phase mainly comprises NaCl, KCl and other salts, and part of Na2O and K2And O appears, the material is less affected by corrosion, and the structure of the material is not obviously changed.
Analysis of a sample can find that the material is most seriously corroded when contacting with 3 types of slag, namely gas, solid and liquid, the material obviously expands, and the structure is damaged; the salt and the alkali metal vapor are deeply permeated into the material, so that the thermal expansion of the material is mainly changed. Based on the erosion and infiltration mechanisms of different areas of the material, reference and theoretical basis can be provided for the optimization and improvement direction of the service performance of the material.
Example 2:
in order to compare the erosion resistance of the chromium corundum bricks and the silicon mullite bricks in the hazardous waste rotary kiln, the test method and the test device are adopted as in example 1, and the difference is that two sets of test containers are used, 2 groups of samples to be tested, namely the chromium corundum bricks and the silicon mullite bricks, are respectively placed, the test condition is 1200 ℃, and the temperature is kept for 12 hours.
Example 3:
in order to simulate the temperature fluctuation caused by the rotation of the furnace body in the dangerous waste rotary kiln, the test method and the device as in the embodiment 1 are adopted, and the difference is that the test temperature is set to be 1000 ℃, the temperature is kept for 12 hours, a heating wire is arranged at the third section of the horizontal section to heat for 20min and 1100 ℃, and the circulating heat treatment is stopped for 20 min.
Example 4:
to compare the erosion and permeability effects of different slags on the material, the test method and apparatus as in example 1 were used, with the difference that two sets of test vessels were used, the same chromium corundum brick was used as the sample material, and slag a with Cl content of 12.5%, Na content of 3.8%, slag B with Cl content of 1.6% and Na content of 21.7% were used as the test slag. The test condition is that the temperature is kept for 24 hours at 800 ℃.
Example 5:
to compare the resistance of the chromium corundum bricks with different contents of chromium oxide, in particular to the attack by slag, the test method and the apparatus as in example 1 were used, with the difference that
1 the test container and the furnace door brick adopt the following specifications:
the vertical section of the container is prepared by 2520 alloy, and the specification is as follows: inner diameter phi 120mm h140mm, wall thickness 3 mm; the first, third and fifth horizontal sections of the container are made of 2520 alloy, the wall thickness is 3mm, and the first section and the vertical section have the following specifications: inner diameter phi 120mm h50 mm; the second and fourth horizontal sections of the container are made of corundum ceramic tubes, the wall thickness is 3mm, and the specification is as follows: an inner diameter phi 123mm x h30 mm; the inclination angle of the horizontal section is 10 degrees, which is convenient for slag to rapidly flow back after being cooled; the diameter of the punched holes of the furnace door brick is 130mm, the inclination angle is 10 degrees, and the number of the punched holes is 3; the horizontal section of the container, the fifth section is provided with a nickel-chromium heating wire and a heating device, and the outside of the metal pipe of the fifth section is coated with insulating fiber to prevent the heating wire from directly contacting the metal pipe;
2, 3 sets of test containers can be placed in the hearth;
3, the samples to be detected are respectively chrome corundum materials with the chrome oxide content of 5%, 12% and 27%, and the specifications of the prepared cylinder samples are as follows: phi 100mm x 120 mm;
4, the slag filling amount of the test slag is 2/3 of the height of the test sample to be tested at the vertical section;
5, keeping the test temperature at 1200 ℃ for 5 h;
6, during the test, the fifth section of the electric heating wire continuously heats the wall of the container at 350 ℃ to create constant temperature of the cold end of the container;
and 7, measuring the mass and the diameter of the test material after the test, further performing equally-divided cutting on the vertical section sample along the axis, observing the erosion and infiltration conditions of the vertical section material by the slag, and performing a thermal expansion test on the horizontal section sample. And judging whether the slag resistance of each material is good or bad according to the area of the vertical section material eroded and penetrated by the slag.
Example 6:
in order to simulate the temperature gradient of the lining material of the hazardous waste rotary kiln under the real service condition, the test method and the device as in the embodiment 1 are adopted, and the differences are that:
1 the test container and the furnace door brick adopt the following specifications:
the vertical section of the container is prepared from 310s alloy steel, and the specification is as follows: inside diameter phi 75mm h270mm, wall thickness 5 mm; the first, third and fifth sections of the horizontal section of the container are made of 310s alloy steel, the wall thickness is 5mm, and the first section and the vertical section have the following specifications: inner diameter phi 75mm h80 mm; the second and fourth horizontal sections of the container are made of corundum ceramic tubes, the wall thickness is 3mm, and the specification is as follows: inner diameter phi 80mm h25 mm; the inclination angle of the horizontal section is 7 degrees; the diameter of the punched holes of the furnace door bricks is 87mm, and the inclination angle is 7 degrees; the horizontal section, the third section and the fifth section of the container are provided with a nickel-chromium heating wire and a heating device, and the metal pipe is coated with insulating fibers to prevent the heating wire from directly contacting with the metal pipe;
2, a set of test container can be placed in the hearth;
3 the specification of the cylinder sample prepared by the chrome corundum material to be measured is as follows: phi 65mm x h230 mm;
4, setting the test temperature condition as 1000 ℃ and keeping the temperature for 12 h;
5 in the test process, the external electric heating wire of the third section is heated at 750 ℃; and the electric heating wire outside the fifth section is heated at 500 ℃ to simulate the temperature gradient change condition under the real condition.
Claims (7)
1. A test method for the slag and steam erosion resistance of a refractory material is characterized by comprising the following steps: the test method is used for representing the chemical reaction, dissolution and permeation of the high-temperature slag and steam generated by the high-temperature slag to a static refractory material sample under the gravity and temperature gradient; the apparent porosity of the measured refractory material is 10-20%, and the normal-temperature compressive strength is more than or equal to 1.0 MPa; the test slag is oxide mixture, inorganic salt or mixture of the oxide mixture and the inorganic salt; the test method comprises the steps of fixing a cylindrical sample of the refractory material to be detected, filled with a slag sample, in a sealing assembly, placing one end of the sealing assembly in a hearth heating area, extending the other end of the sealing assembly out of a furnace wall, forming slag and steam in the heating process of the heat-resistant steel sealing assembly, and generating a temperature gradient on the refractory material sample so as to evaluate the corrosivity of the slag and the steam to the refractory material in a specific temperature and time range; the sealing assembly is an L-shaped splicing body formed by 2 sections of cylinders and comprises a vertical section and a horizontal section which are communicated with each other, a refractory sample to be tested and loaded in the vertical section is immersed in slag liquid to resist slag corrosion of a melt, and a sample loaded in the horizontal section resists steam infiltration corrosion; the refractory material samples have temperature difference in the test, the vertical section samples are at constant temperature, and the horizontal section samples have temperature gradient from being close to the vertical section to being far away from the vertical section; the test result of the test method is processed by taking out vertical section and horizontal section samples after the temperature of the furnace reaches room temperature after the test is finished, measuring and calculating the mass change, volume change and diameter change of the samples before and after the test, and evaluating and comparing the slag and steam erosion resistance of different materials by assisting the analysis means of scanning electron microscope and X-ray diffraction instruments; the method for testing the slag and steam erosion resistance of the refractory material comprises the following specific steps:
firstly, preparing 2 cylindrical refractory material samples with the same material and size, wherein the size of a cylinder is phi 50-100 mm multiplied by h 100-230 mm, measuring the initial mass, volume and diameter of the samples, and sampling from samples with the same specification to carry out microstructure and phase composition analysis;
secondly, respectively placing the 2 cylinders into a vertical section and a horizontal section of a heat-resistant steel sealed container, then adding test slag into the vertical section, wherein the slag filling amount is 1/2-2/3 of the height of the cylinder of the vertical section, and sealing;
thirdly, placing the sealed container filled with the sample and the slag into a test device, placing the vertical section into a hearth with a heating body, and extending the horizontal section out of a kiln wall or a kiln door;
fourthly, heating the hearth to a test temperature and preserving heat, wherein the test temperature is 800-1200 ℃, and the preserving heat time is 3-24 hours;
and fifthly, taking out the sealed container from the test device after natural cooling, taking out the refractory material sample after dismantling for measuring the mass, the volume and the diameter, or analyzing by an instrument to give out the evaluation of erosion resistance.
2. The method of claim 1, wherein the method comprises: analyzing by an instrument, and cutting the vertical section sample along the side surface of the cylindrical sample according to the slag filling amount and the direct contact slag; equally cutting the cut samples which are not in direct contact with the slag and the samples which are in direct contact with the slag respectively along the axial direction of the samples; respectively calculating erosion area and penetration area of the directly contacted slag sample, analyzing the microstructure and phase composition of an erosion area and a penetration area of the directly contacted slag sample by adopting a scanning electron microscope and energy spectrum analysis equipment, calculating the steam penetration area of the indirectly contacted slag sample, and analyzing the microstructure and phase composition of the penetration area and the non-penetration area of the directly contacted slag sample by adopting the scanning electron microscope and the energy spectrum analysis equipment; and cutting the horizontal section sample along the side surface of the sample in trisection, drilling a cylindrical sample at the center of the cut cylinder respectively, testing the thermal expansion of the cylindrical sample, cutting the rest of the samples in trisection along the axial direction of the cylindrical sample respectively, and analyzing the permeable area and the non-permeable area of the cylindrical sample by adopting the same method as the analysis method of the vertical section sample which is not in direct contact with the slag. And comprehensively evaluating the quality of the slag and steam corrosion resistance of the sample according to the analysis result of each sample.
3. A test apparatus according to claim 1 or 2, for a method of testing the resistance of a refractory material to slag and steam attack, characterized in that: the inner cavity of the normal-pressure heat treatment electric furnace of the test device forms a hearth; the inner wall of the hearth is provided with a heat-insulating furnace lining, and the heating mode is that a heating element is adopted to carry out electric heating in the hearth; monitoring the temperature of each temperature section by adopting a thermocouple and a temperature display device; the testing container is placed in the hearth, the testing container is made of alloy steel resistant to high temperature of 1200 ℃, the wall thickness of the container is 3-5mm, the container is a two-section cylindrical container and consists of a vertical section, a horizontal section and a base, the inner diameter phi of the vertical section is 70-120 mm, the height h is 140-270 mm, the upper opening of the vertical section is provided with a screwed cap, and the horizontal section is of a broken bridge type structure which adopts a corundum ceramic tube and is assembled with a testing container material: the first section, the third section and the fifth section are made of test container materials, wherein the first section is communicated with the vertical section, and the specification of the third section is as follows: phi is 70-120 mm multiplied by h 40-80 mm, the second section and the fourth section are corundum ceramic tubes, the inner diameter of each corundum ceramic tube is the same as the outer diameter of the rest three sections of materials, the specifications are that the inner diameter is phi 73-125 mm multiplied by h 20-30 mm, the wall thickness of each corundum ceramic tube is 3-5mm, and the side opening of the horizontal section is provided with a threaded screw cap which is provided with a hole and can be connected with a tail gas treatment device; the first, third and fifth sections of the horizontal section are provided with a baffle and a gasket; during the test, the furnace door is filled and plugged by furnace door bricks and refractory fibers which are made of the same materials as the heat-insulating lining and provided with holes, so that the furnace is insulated and the test container is fixed.
4. A test apparatus for testing the resistance of a refractory material to slag and steam erosion as set forth in claim 3, wherein: the base of the test container is a crucible made of alloy steel which can resist the high temperature of 1200 ℃.
5. A test apparatus for testing the resistance of a refractory material to slag and steam erosion as set forth in claim 3, wherein: the horizontal section of the test container is high in cold end and low in hot end, and an inclination angle of 5-10 degrees is formed between the horizontal section and the horizontal plane.
6. A test apparatus for testing the resistance of a refractory material to slag and steam erosion as set forth in claim 3, wherein: the horizontal section of the test container, the part of which extends out of the furnace door brick, can be provided with an electric heating wire and a heating device or a water cooling tube and a water cooling system for controllably adjusting the temperature gradient, wherein the electric heating wire and the horizontal section need to be isolated by insulating fibers.
7. A test apparatus for testing the resistance of a refractory material to slag and steam erosion as set forth in claim 3, wherein: the refractory material slag and steam resistance test device can be used for simultaneously placing a plurality of groups of test containers according to the size of a hearth so as to perform parallel tests among multiple materials under the same test condition.
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| JP2007298433A (en) * | 2006-05-01 | 2007-11-15 | Nippon Steel Corp | Method of evaluating corrosion resistance, abrasion resistance and oxidation resistance of carbon-containing refractory material |
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