CN113624794A - Test device and method for evaluating molten iron corrosion resistance of blast furnace carbon brick - Google Patents
Test device and method for evaluating molten iron corrosion resistance of blast furnace carbon brick Download PDFInfo
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Abstract
The embodiment of the invention discloses a test device and an evaluation method for evaluating molten iron corrosion resistance of a blast furnace carbon brick, belonging to the technical field of performance test and accurate evaluation of refractory materials. The testing device comprises a high-temperature reaction tubular furnace, a high-purity argon gas cylinder and a precise temperature controller are arranged beside the high-temperature reaction tubular furnace, a long constant-temperature area is arranged at the middle position of a furnace tube of the high-temperature reaction tubular furnace, and an upper furnace cover and a lower furnace cover with central openings are respectively arranged at the upper end and the lower end of the high-temperature reaction tubular furnace; a corundum crucible is arranged in the long constant temperature area, a stirring device is inserted in the center of the upper furnace cover, the lower end of the stirring device is connected with a corundum rod sleeved with blast furnace carbon bricks, an air inlet pipe is inserted in the center of the lower furnace cover, and the air inlet pipe is connected with a rotameter and an air bottle. The invention accurately evaluates the molten iron corrosion resistance of the blast furnace carbon brick by introducing the structure of the device, the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburizing rate.
Description
Technical Field
The invention belongs to the technical field of refractory material performance testing and accurate evaluation, and relates to a test device and an evaluation method for evaluating molten iron corrosion resistance of a blast furnace carbon brick.
Background
With the development of Chinese blast furnaces toward large-scale and high-efficiency, the long service life of the blast furnace has become an important technical characteristic of an iron-making process. The long-life technology of blast furnace is a comprehensive technology relating to the design of furnace type, operation system, cooling system and quality of refractory material.
In recent years, with the rapid development of iron-making technology, the utilization coefficient of blast furnaces is continuously improved, and higher requirements are made on the quality of refractory materials and the capacity of a cooling system of the blast furnaces. Wherein: the application technology of the copper cooling wall is gradually mature, so that the restriction link of the service life of the blast furnace is gradually transferred from a furnace body to a furnace hearth, and the quality of refractory materials is one of the most important factors influencing the service life of the furnace hearth.
The carbon brick is subjected to the high-temperature scouring action of molten iron and furnace slag at the hearth part of the blast furnace, the carbon component in the carbon brick is easily dissolved in unsaturated molten iron, the oxide component is easily dissolved in the furnace slag, the carbon brick is seriously corroded and peeled, the viscosity of the molten iron is low, and the scouring of the carbon brick is more serious.
The blast furnace hearth is in a periodic tapping process, and molten iron is in a continuous circulating flow state in the blast furnace hearth, namely molten iron circulation is formed, so that an iron-carbon interface is continuously updated, and the molten iron circulation becomes the most main influence factor for carbon brick corrosion.
At present, due to the fact that commercial carbon bricks at the hearth part of a blast furnace are numerous in types, how to systematically and accurately evaluate the molten iron corrosion resistance of the carbon bricks and provide a reference standard for reasonably selecting the carbon bricks for the blast furnace become a technical problem to be solved urgently by technical staff in the field. Although the existing technical schemes for evaluating the molten iron corrosion resistance of the carbon bricks by simulating the actual service conditions of the blast furnace hearth carbon bricks are many, how to develop a method for evaluating the molten iron corrosion resistance of the blast furnace carbon bricks more accurately and comprehensively and systematically is not considered in the prior art on the basis of simulating the actual service conditions of the blast furnace hearth carbon bricks.
The concrete description is as follows:
(1) although the medium steel group drafts the national standard GB/T24201-2009 test method for molten iron corrosion resistance of blast furnace carbon blocks, the method has the following defects:
1) according to the test method, the molten iron is stirred by blowing nitrogen, the molten iron flowing state of an iron-carbon interface is obviously different from the molten iron flowing state of the side wall of the blast furnace hearth in actual production, and the periodic dynamic scouring effect of the molten iron circulation in the blast furnace hearth on the blast furnace carbon bricks cannot be reflected;
2) the whole set of sample preparation process is complex, the difficulty that the sample can not leak gas from the bonding part of the corundum tube and the suspender is high, and the potential danger of falling off of the blast furnace carbon brick sample exists in the test process;
3) the characterization means of the test method only comprises the molten iron corrosion rate, namely the ratio of the mass difference value of the blast furnace carbon bricks before and after the test to the mass of the blast furnace carbon bricks before the test, and because the blast furnace carbon bricks are porous materials, molten iron can enter the interior of the blast furnace carbon bricks and is retained in the pores of the blast furnace carbon bricks after being cooled in water.
Therefore, the single quality change in GB/T24201-.
(2) Although the invention patent CN201711384943.9 granted by zhangjialiang et al of beijing university of science and technology discloses a test device and method for evaluating the molten iron corrosion resistance of refractory material, the method has the following disadvantages:
1) according to the test method, small-particle coke is placed above molten iron to simulate the permeation and abrasion effects of the movement of the coke in the blast furnace hearth on the side wall carbon bricks, although the experimental conditions are closer to the actual production process, the coke carburization can interfere the carburization process of the blast furnace carbon bricks, the real molten iron corrosion resisting process of the blast furnace carbon bricks cannot be reflected, and the representation of the test result on the molten iron carburization rate can be influenced;
2) in the test process, corundum rods are adopted for stirring to enable molten iron to move to simulate the molten iron circulation in a blast furnace hearth, so that the relative flow velocity of the molten iron on a blast furnace carbon brick interface cannot be determined;
3) after the test is finished, the iron in the blast furnace carbon brick crucible is not easy to take out and remove, and the inner diameter and the outer diameter of the blast furnace carbon brick crucible are not easy to measure.
In summary, it is necessary to invent a device capable of deeply simulating the erosion process of the blast furnace carbon brick by the molten iron circulation in the blast furnace hearth, and comprehensively evaluating the molten iron erosion resistance of the blast furnace carbon brick in the blast furnace hearth by adopting various characterization means, and the structural arrangement of the corresponding simulation test device and the corresponding using method are important.
Disclosure of Invention
The invention solves the technical problems that the existing test method for evaluating the molten iron corrosion resistance of the blast furnace carbon brick is complex, the evaluation system is not sound, the evaluation process parameters are selected from one surface, and the molten iron corrosion resistance of the blast furnace carbon brick is difficult to be comprehensively, systematically and accurately evaluated.
The invention aims to provide a test device and an evaluation method for simulating the molten iron corrosion resistance of a blast furnace carbon brick under the actual condition of a blast furnace aiming at the problems of a test method and an evaluation method for the molten iron corrosion resistance of the blast furnace carbon brick, provide a system evaluation index for the molten iron corrosion resistance of the blast furnace carbon brick and standardize an evaluation system. The test device and the evaluation method are simple, the operation is easy, and the proposed evaluation indexes are comprehensive and accurate.
In order to solve the technical problems and achieve the purposes, the invention provides a test device for evaluating molten iron corrosion resistance of a blast furnace carbon brick, which comprises a high-temperature reaction tubular furnace, wherein a high-purity argon gas cylinder and a precise temperature controller are arranged beside the high-temperature reaction tubular furnace, a long constant temperature area is arranged at the middle position of a furnace tube of the high-temperature reaction tubular furnace, and the upper end and the lower end of the high-temperature reaction tubular furnace are respectively provided with an upper furnace cover and a lower furnace cover with central openings;
wherein: the furnace is characterized in that a corundum crucible is arranged in the long constant-temperature area, molten iron is arranged in the corundum crucible, a stirring device is inserted in the center of the upper furnace cover, the lower end of the stirring device is connected with a corundum rod sleeved with blast furnace carbon bricks, an air inlet pipe is inserted in the center of the lower furnace cover, and the air inlet pipe is connected with a rotor flow meter and an air bottle.
Preferably, the high-temperature reaction tube furnace is a BTML-1700 ℃ high-temperature reaction tube furnace, and the precise temperature controller is an SRS13A precise temperature controller.
Preferably, the stirring device comprises a constant speed electric stirrer, a stirring motor and a motor support, wherein: the stirring device is characterized in that the motor support is erected on the high-temperature reaction tube furnace, the stirring motor is arranged on the motor support, and the lower end of a rotating shaft of the stirring motor is connected with a stirring blade or a corundum rod sleeved with blast furnace carbon bricks.
Preferably, the diameter of the corundum rod sleeved with the blast furnace carbon brick is 8mm, and the length of the corundum rod is determined according to the distance between the motor and the molten iron liquid level; the blast furnace carbon brick is a cylinder with a concentric through hole, the outer diameter of the cylinder is 30mm, the height of the cylinder is 50mm, and the diameter of an inner concentric round hole is 8 mm.
Preferably, one end of the corundum rod sleeved with the blast furnace carbon brick is lathed with 60mm long threads and is provided with a matched nut, and the corundum rod sleeved with the blast furnace carbon brick is prepared by inserting the threaded end of the corundum rod into a concentric circular hole of the blast furnace carbon brick and screwing the nut.
Preferably, the furnace tube of the high-temperature reaction tube furnace is made of corundum, the inner diameter of the furnace tube is 80mm, and the height of the furnace tube is 900 mm.
Preferably, the length of the long constant-temperature area is 100mm, the heating temperature interval is 0-1700 ℃, and a refractory material brick pad is arranged below the constant-temperature area.
Preferably, the precise temperature controller comprises an FP93 meter, a voltmeter, an ammeter, an indicator light, an operation key and a lead, is used for setting a test program, monitoring the temperature, the voltage, the current and the like in the test process, and is connected with the high-temperature reaction tube furnace through the lead.
Preferably, the length of the corundum rod is determined by the depth of the blast furnace carbon brick sample immersed in molten iron and the distance between the horizontal plane of the lower end of the chuck of the stirring motor and the liquid level of the molten iron.
The method for evaluating the molten iron corrosion resistance of the blast furnace carbon brick by using the test device comprises the following steps:
(1) sample preparation: manufacturing blast furnace carbon bricks into a cylindrical sample, sequentially grinding, polishing, cleaning and drying the surface of the cylindrical sample, fixing the cylindrical sample on a corundum rod, connecting the corundum rod with a stirring device, and simulating the corrosion condition of molten iron circulation in a hearth of a medium-high furnace to the blast furnace carbon bricks by adjusting the rotating speed of an electric stirrer by adopting a rotating cylinder method;
(2) and (4) evaluating the result: the molten iron corrosion resistance of the blast furnace carbon brick is evaluated through the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburization rate of the blast furnace carbon brick.
Preferably, the evaluation method comprises the following specific steps:
the method comprises the following steps: manufacturing a blast furnace carbon brick into a concentric cylindrical sample, sequentially grinding, polishing and cleaning the surface of the concentric cylindrical sample, measuring the volume of the concentric cylindrical sample by adopting a drainage method, and drying the concentric cylindrical sample in a drying box;
step two: weighing the mass of the concentric cylindrical sample by using a balance, measuring the diameter of the concentric cylindrical sample by using a vernier caliper, photographing the concentric cylindrical sample, and observing the macroscopic morphology of the concentric cylindrical sample before corrosion;
step three: fixing the concentric cylindrical sample on a corundum rod, randomly sampling from the blast furnace carbon brick, and preparing a scanning electron microscope sample for SEM-EDS analysis;
step four: before corrosion, a group of blank tests are carried out so as to be compared and analyzed with the molten iron corrosion resistance test result of the blast furnace carbon brick, and the influence degree of a high-temperature environment on the concentric cylindrical sample is eliminated;
step five: drying a reagent adopted for preparing an iron sample in a drying box, preparing the iron sample according to actual molten iron components, uniformly mixing, and sealing for storage;
step six: putting the iron sample obtained in the step five into a corundum crucible, and placing the corundum crucible in the middle of a constant-temperature area of the high-temperature reaction tube furnace length to prevent the corundum crucible from being bonded with the side wall of the furnace tube;
step seven: starting a precision temperature controller, setting a temperature program, and checking the set program after the program is set; opening an argon gas cylinder, setting a flow meter, starting a heating key high-temperature reaction tube furnace and starting heating;
step eight: after the temperature of the high-temperature reaction tube furnace is raised to 1500 ℃, keeping the temperature and stirring by adopting a quartz tube so as to ensure that the iron sample is completely melted and the components are uniform; then keeping the temperature constant, putting the corundum rod at the lower end of the stirring device into a furnace tube of a high-temperature reaction tube furnace for preheating, then slowly moving the corundum rod downwards and immersing the corundum rod below the liquid level of molten iron, and adjusting the rotating speed and time according to the test requirement;
step nine: in the corrosion process, a pipette and a quartz tube are adopted to extract an iron sample at intervals, and water quenching is rapidly carried out for 4 times; when the iron sample is extracted, the stirring motor is suspended from rotating, and the extraction time is controlled within 1 min;
step ten: after the corrosion is finished, lifting the corundum rod for fixing the concentric cylindrical sample to separate the corundum rod from molten iron, starting a stirring motor to rotate to spin off iron beads attached to the surface of the sample, stopping ventilation after the program is cooled to room temperature, closing the high-temperature reaction tube furnace, taking out the concentric cylindrical sample, and performing subsequent performance evaluation;
step eleven: weighing the mass of the corroded concentric cylindrical sample by using a balance, measuring the diameter of the corroded concentric cylindrical sample by using a vernier caliper, and calculating the mass change rate, the corrosion degree and the corrosion rate of the corroded concentric cylindrical sample;
step twelve: photographing the corroded concentric cylindrical sample, and observing the difference and the similarity between the reacted macroscopic morphology of the corroded concentric cylindrical sample and the macroscopic morphology of the corroded concentric cylindrical sample before corrosion; measuring the volume of the corroded concentric cylindrical sample by adopting a drainage method, and calculating the volume change rate of the sample by combining the first step;
step thirteen: drying in a drying oven, manufacturing a scanning electron microscope sample, carrying out SEM-EDS analysis, observing the microscopic morphology and structural characteristics of the sample after reaction, analyzing a phase formed after the reaction through the EDS, carrying out line scanning to observe the content distribution rule of iron elements from outside to inside, and carrying out surface scanning to observe the distribution rule of different elements in the whole surface so as to clarify the corrosion mechanism of the molten iron on the blast furnace carbon brick and the damage degree of the molten iron on the structure of the blast furnace carbon brick;
fourteen steps: and (4) extracting the carbon content in the iron sample for nine times in the detection step, and determining the carburization rate of the molten iron so as to obtain the corrosion speed of the molten iron on the blast furnace carbon brick.
Preferably, the distance between the corundum rod slowly moving downwards and the molten iron surface is 30 mm.
Preferably, the molten iron composition: [ Fe ]: 95.87%, [ C ]: 3.50%, [ Si ]: 0.30%, [ Mn ]: 0.15%, [ P ]: 0.15%, [ S ]: 0.03 percent; temperature of molten iron: 1500 ℃; rotating speed: 60 r/min.
Preferably, the specific evaluation indexes for evaluating the molten iron corrosion resistance of the blast furnace carbon brick through the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburization rate of the blast furnace carbon brick are as follows:
(1) macroscopic appearance of blast furnace carbon brick after corrosion
The macroscopic morphology of the carbon brick samples before and after corrosion is greatly different under the influence of the chemical components and the forming mode of the blast furnace carbon brick, the components of molten iron, the temperature, the rotating speed and the like.
And (4) photographing the carbon brick sample after corrosion, analyzing corrosion contour lines, surface roughness and surface carbon aggregate particle peeling degree, and preliminarily evaluating the molten iron corrosion resistance of the blast furnace carbon brick.
(2) Rate of change of mass
And removing iron beads fixedly connected to the surface of the matrix after the carbon brick sample is corroded, and measuring the mass of the corroded carbon brick sample by using a balance. If the carbon brick sample has no other subsequent detection requirements, before the balance measurement, the iron element solidified on the surface of the carbon brick sample after corrosion can be removed by acid cleaning, and then the carbon brick sample is dried and weighed.
Mass rate of change definitional equation:
in the formula,. eta. -mass change rate,%;
m1-mass before carbon brick test, g;
m2-mass after carbon brick test, g.
(3) Degree of corrosion
And measuring the diameter of the carbon brick sample after corrosion by using a vernier caliper.
Erosion degree definition formula:
in the formula, delta d is the corrosion degree of the carbon brick, and is mm/h;
d0the diameter of the carbon brick before reaction is mm;
dfthe diameter of the carbon brick after reaction is mm;
t-reaction time, h.
(4) Rate of erosion
Erosion rate definition formula:
wherein v is the erosion rate of the carbon brick, g/(h.cm)2)；
l-the depth of the carbon brick immersed in the molten iron is cm;
rho-carbon brick density, g/cm3；
wCCarbon content of the carbon brick,%;
s-contact area of reaction, cm2。
(5) Rate of change of volume
And measuring the volumes of the carbon brick sample before and after corrosion by adopting a drainage method. The carbon brick samples may be first soaked in water for a certain period of time before measurement, taking into account the water absorption of the samples.
Volume rate of change definitional equation:
in the formula, lambda represents the volume change rate,%;
V1volume before carbon brick test, cm3；
V2Volume, cm after carbon brick test3。
(6) SEM + EDS characterization
The carbon brick samples before and after corrosion are made into scanning electron microscope samples for microscopic analysis, the penetration depth of molten iron on a reaction interface and the appearance of a permeable layer including hole distribution, aperture change, microcrack condition and the like are observed through SEM, and the phase and element distribution rule of the reaction interface after corrosion are analyzed through EDS so as to clarify the corrosion mechanism of the molten iron on the blast furnace carbon brick and the damage degree of the molten iron on the structure of the blast furnace carbon brick.
(7) Rate of carburization of molten iron
In the test process of the molten iron corrosion resistance detection of the blast furnace carbon brick, 3-5 g of iron samples are extracted at intervals according to the total test time, and the carbon content in the iron samples is detected to determine the carburizing rate of the molten iron.
Preferably, the iron sample is prepared by adopting reduced iron powder, graphite powder, silicon powder, manganese powder, phosphorus powder and ferrous disulfide powder and is placed in a cylindrical corundum crucible, and the cylindrical corundum crucible is placed in a long constant temperature region.
Preferably, the iron sample is extracted not less than 4 times.
The technical scheme provided by the embodiment of the invention at least has the following beneficial effects:
the invention has the technical advantages of simple sample preparation, simple and convenient operation, high test success rate and comprehensive and accurate evaluation index. The method specifically comprises the following two aspects:
on one hand, the erosion condition of the molten iron composition, the temperature and the flow rate of the blast furnace hearth on the side wall carbon brick under the actual working condition can be well simulated, and the test result is closer to the actual service environment of the carbon brick;
on the other hand, the introduced evaluation indexes are comprehensive and accurate, the corrosion degree of the molten iron in the blast furnace hearth on the carbon bricks can be systematically evaluated, and the mechanism of the whole corrosion process is analyzed.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a test device for evaluating molten iron corrosion resistance of a blast furnace carbon brick according to the present invention;
FIG. 2 is a schematic diagram of a cutting structure of a blast furnace briquette sample of the present invention, unit, mm;
FIG. 3 is a schematic diagram of the plan structure of a corundum rod of the present invention, in units of mm;
the reference numerals are explained below:
1-a stirring device;
2-a silicon molybdenum heating rod;
3-a high-purity argon cylinder;
4-SRS13A precision temperature controller;
5-temperature thermocouple.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
A test device for evaluating molten iron corrosion resistance of blast furnace carbon bricks comprises a high-temperature reaction tubular furnace, wherein a high-purity argon gas cylinder and a precise temperature controller are arranged beside the high-temperature reaction tubular furnace, a long constant-temperature area is arranged at the middle position of a furnace tube of the high-temperature reaction tubular furnace, and the upper end and the lower end of the high-temperature reaction tubular furnace are respectively provided with an upper furnace cover and a lower furnace cover with central openings;
wherein: the furnace is characterized in that a corundum crucible is arranged in the long constant-temperature area, molten iron is arranged in the corundum crucible, a stirring device is inserted in the center of the upper furnace cover, the lower end of the stirring device is connected with a corundum rod sleeved with blast furnace carbon bricks, an air inlet pipe is inserted in the center of the lower furnace cover, and the air inlet pipe is connected with a rotor flow meter and an air bottle.
Particularly, the high-temperature reaction tube furnace is a BTML-1700 ℃ high-temperature reaction tube furnace, and the precise temperature controller is an SRS13A precise temperature controller.
In particular, the stirring device comprises a constant speed electric stirrer, a stirring motor and a motor support, wherein: the stirring device is characterized in that the motor support is erected on the high-temperature reaction tube furnace, the stirring motor is arranged on the motor support, and the lower end of a rotating shaft of the stirring motor is connected with a stirring blade or a corundum rod sleeved with blast furnace carbon bricks.
Particularly, the diameter of the corundum rod sleeved with the blast furnace carbon brick is 8mm, and the length of the corundum rod is determined according to the distance between the motor and the molten iron liquid level; the blast furnace carbon brick is a cylinder with a concentric through hole, the outer diameter of the cylinder is 30mm, the height of the cylinder is 50mm, and the diameter of an inner concentric round hole is 8 mm.
Specifically, one end of the corundum rod sleeved with the blast furnace carbon brick is lathed with 60mm long threads and is provided with a matched nut, and the corundum rod sleeved with the blast furnace carbon brick is prepared by inserting the threaded end of the corundum rod into a concentric circular hole of the blast furnace carbon brick and screwing the nut.
Particularly, the furnace tube of the high-temperature reaction tube furnace is made of corundum, the inner diameter of the furnace tube is 80mm, and the height of the furnace tube is 900 mm.
Particularly, the length of the long constant-temperature area is 100mm, the heating temperature interval is 0-1700 ℃, and a refractory material brick pad is arranged below the constant-temperature area.
Particularly, the precise temperature controller comprises an FP93 meter, a voltmeter, an ammeter, an indicator light, an operation key and a lead, is used for setting a test program and monitoring the temperature, voltage, current and the like in the test process, and is connected with the high-temperature reaction tube furnace through the lead.
Particularly, the length of the corundum rod is determined by the depth of the blast furnace carbon brick sample immersed in molten iron and the distance between the horizontal plane of the lower end of a chuck of the stirring motor and the liquid level of the molten iron.
The method for evaluating the molten iron corrosion resistance of the blast furnace carbon brick by using the test device comprises the following steps:
(1) sample preparation: manufacturing blast furnace carbon bricks into a cylindrical sample, sequentially grinding, polishing, cleaning and drying the surface of the cylindrical sample, fixing the cylindrical sample on a corundum rod, connecting the corundum rod with a stirring device, and simulating the corrosion condition of molten iron circulation in a hearth of a medium-high furnace to the blast furnace carbon bricks by adjusting the rotating speed of an electric stirrer by adopting a rotating cylinder method;
(2) and (4) evaluating the result: the molten iron corrosion resistance of the blast furnace carbon brick is evaluated through the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburization rate of the blast furnace carbon brick.
Specifically, the evaluation method comprises the following specific steps:
the method comprises the following steps: manufacturing a blast furnace carbon brick into a concentric cylindrical sample, sequentially grinding, polishing and cleaning the surface of the concentric cylindrical sample, measuring the volume of the concentric cylindrical sample by adopting a drainage method, and drying the concentric cylindrical sample in a drying box;
step two: weighing the mass of the concentric cylindrical sample by using a balance, measuring the diameter of the concentric cylindrical sample by using a vernier caliper, photographing the concentric cylindrical sample, and observing the macroscopic morphology of the concentric cylindrical sample before corrosion;
step three: fixing the concentric cylindrical sample on a corundum rod, randomly sampling from the blast furnace carbon brick, and preparing a scanning electron microscope sample for SEM-EDS analysis;
step four: before corrosion, a group of blank tests are carried out so as to be compared and analyzed with the molten iron corrosion resistance test result of the blast furnace carbon brick, and the influence degree of a high-temperature environment on the concentric cylindrical sample is eliminated;
step five: drying a reagent adopted for preparing an iron sample in a drying box, preparing the iron sample according to actual molten iron components, uniformly mixing, and sealing for storage;
step six: putting the iron sample obtained in the step five into a corundum crucible, and placing the corundum crucible in the middle of a constant-temperature area of the high-temperature reaction tube furnace length to prevent the corundum crucible from being bonded with the side wall of the furnace tube;
step seven: starting a precision temperature controller, setting a temperature program, and checking the set program after the program is set; opening an argon gas cylinder, setting a flow meter, starting a heating key high-temperature reaction tube furnace and starting heating;
step eight: after the temperature of the high-temperature reaction tube furnace is raised to 1500 ℃, keeping the temperature and stirring by adopting a quartz tube so as to ensure that the iron sample is completely melted and the components are uniform; then keeping the temperature constant, putting the corundum rod at the lower end of the stirring device into a furnace tube of a high-temperature reaction tube furnace for preheating, then slowly moving the corundum rod downwards and immersing the corundum rod below the liquid level of molten iron, and adjusting the rotating speed and time according to the test requirement;
step nine: in the corrosion process, a pipette and a quartz tube are adopted to extract an iron sample at intervals, and water quenching is rapidly carried out for 4 times; when the iron sample is extracted, the stirring motor is suspended from rotating, and the extraction time is controlled within 1 min;
step ten: after the corrosion is finished, lifting the corundum rod for fixing the concentric cylindrical sample to separate the corundum rod from molten iron, starting a stirring motor to rotate to spin off iron beads attached to the surface of the sample, stopping ventilation after the program is cooled to room temperature, closing the high-temperature reaction tube furnace, taking out the concentric cylindrical sample, and performing subsequent performance evaluation;
step eleven: weighing the mass of the corroded concentric cylindrical sample by using a balance, measuring the diameter of the corroded concentric cylindrical sample by using a vernier caliper, and calculating the mass change rate, the corrosion degree and the corrosion rate of the corroded concentric cylindrical sample;
step twelve: photographing the corroded concentric cylindrical sample, and observing the difference and the similarity between the reacted macroscopic morphology of the corroded concentric cylindrical sample and the macroscopic morphology of the corroded concentric cylindrical sample before corrosion; measuring the volume of the corroded concentric cylindrical sample by adopting a drainage method, and calculating the volume change rate of the sample by combining the first step;
step thirteen: drying in a drying oven, manufacturing a scanning electron microscope sample, carrying out SEM-EDS analysis, observing the microscopic morphology and structural characteristics of the sample after reaction, analyzing a phase formed after the reaction through the EDS, carrying out line scanning to observe the content distribution rule of iron elements from outside to inside, and carrying out surface scanning to observe the distribution rule of different elements in the whole surface so as to clarify the corrosion mechanism of the molten iron on the blast furnace carbon brick and the damage degree of the molten iron on the structure of the blast furnace carbon brick;
fourteen steps: and (4) extracting the carbon content in the iron sample for nine times in the detection step, and determining the carburization rate of the molten iron so as to obtain the corrosion speed of the molten iron on the blast furnace carbon brick.
In particular, the corundum rod is slowly moved downward and immersed below the liquid level of the molten iron by a distance of 30 mm.
Specifically, the molten iron composition: [ Fe ]: 95.87%, [ C ]: 3.50%, [ Si ]: 0.30%, [ Mn ]: 0.15%, [ P ]: 0.15%, [ S ]: 0.03 percent; temperature of molten iron: 1500 ℃; rotating speed: 60 r/min.
Particularly, specific evaluation indexes for evaluating the molten iron corrosion resistance of the blast furnace carbon brick through the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburization rate of the blast furnace carbon brick are as follows:
(1) macroscopic appearance of blast furnace carbon brick after corrosion
The macroscopic morphology of the carbon brick samples before and after corrosion is greatly different under the influence of the chemical components and the forming mode of the blast furnace carbon brick, the components of molten iron, the temperature, the rotating speed and the like.
And (4) photographing the carbon brick sample after corrosion, analyzing corrosion contour lines, surface roughness and surface carbon aggregate particle peeling degree, and preliminarily evaluating the molten iron corrosion resistance of the blast furnace carbon brick.
(2) Rate of change of mass
And removing iron beads fixedly connected to the surface of the matrix after the carbon brick sample is corroded, and measuring the mass of the corroded carbon brick sample by using a balance. If the carbon brick sample has no other subsequent detection requirements, before the balance measurement, the iron element solidified on the surface of the carbon brick sample after corrosion can be removed by acid cleaning, and then the carbon brick sample is dried and weighed.
Mass rate of change definitional equation:
in the formula,. eta. -mass change rate,%;
m1-mass before carbon brick test, g;
m2-mass after carbon brick test, g.
(3) Degree of corrosion
And measuring the diameter of the carbon brick sample after corrosion by using a vernier caliper.
Erosion degree definition formula:
in the formula, delta d is the corrosion degree of the carbon brick, and is mm/h;
d0the diameter of the carbon brick before reaction is mm;
dfthe diameter of the carbon brick after reaction is mm;
t-reaction time, h.
(4) Rate of erosion
Erosion rate definition formula:
wherein v is the erosion rate of the carbon brick, g/(h.cm)2)；
l-the depth of the carbon brick immersed in the molten iron is cm;
rho-carbon brick density, g/cm3；
wCCarbon content of the carbon brick,%;
s-reactive contactArea, cm2。
(5) Rate of change of volume
And measuring the volumes of the carbon brick sample before and after corrosion by adopting a drainage method. The carbon brick samples may be first soaked in water for a certain period of time before measurement, taking into account the water absorption of the samples.
Volume rate of change definitional equation:
in the formula, lambda represents the volume change rate,%;
V1volume before carbon brick test, cm3；
V2Volume, cm after carbon brick test3。
(6) SEM + EDS characterization
The carbon brick samples before and after corrosion are made into scanning electron microscope samples for microscopic analysis, the penetration depth of molten iron on a reaction interface and the appearance of a permeable layer including hole distribution, aperture change, microcrack condition and the like are observed through SEM, and the phase and element distribution rule of the reaction interface after corrosion are analyzed through EDS so as to clarify the corrosion mechanism of the molten iron on the blast furnace carbon brick and the damage degree of the molten iron on the structure of the blast furnace carbon brick.
(7) Rate of carburization of molten iron
In the test process of the molten iron corrosion resistance detection of the blast furnace carbon brick, 3-5 g of iron samples are extracted at intervals according to the total test time, and the carbon content in the iron samples is detected to determine the carburizing rate of the molten iron.
Particularly, the iron sample is prepared from reduced iron powder, graphite powder, silicon powder, manganese powder, phosphorus powder and ferrous disulfide powder and is placed in a cylindrical corundum crucible which is placed in a long constant temperature area.
In particular, the iron sample is extracted not less than 4 times.
Example 1
As shown in figure 1, the invention provides a test device for evaluating molten iron corrosion resistance of a blast furnace carbon brick, which comprises a BTML-1700 ℃ high-temperature reaction tube furnace, a stirring device 1, a high-purity argon gas cylinder 3 and an SRS13A precision temperature controller 4.
A corundum furnace tube is arranged in the BTML-1700 ℃ high-temperature reaction tube furnace, and a silicon-molybdenum heating rod 2 is adopted for heating; and a temperature thermocouple 5 is used for monitoring the temperature, a constant temperature area with the length of about 100mm is arranged in the middle of the corundum furnace tube, and a corundum crucible is placed in the constant temperature area to heat and melt an iron sample into molten iron.
The stirring device 1 comprises a JJ-1B constant-speed electric stirrer, a stirring motor and a motor support, wherein the stirring motor is fixed on the upper part of the motor support, and is placed above a BTML-1700 ℃ high-temperature reaction tubular furnace for stirring and controlling the speed of molten iron.
The high-purity argon gas cylinder 3 stores high-purity argon gas and is connected with the BTML-1700 ℃ high-temperature reaction tubular furnace through a gas inlet pipe and a rotor flow meter, and the rotor flow meter is connected between the high-purity argon gas cylinder 3 and the BTML-1700 ℃ high-temperature reaction tubular furnace to control the flow of the gas;
the SRS13A precision temperature controller 4 comprises an FP93 meter, a voltmeter, an ammeter, an indicator light, an operation key and a lead, is used for setting a test program, monitoring the temperature, voltage, current and the like in the test process, and is connected with the tube furnace through the lead.
As shown in FIG. 2, the blast furnace briquette sample is a cylinder having a concentric through-hole, and has an outer diameter of 30mm, a height of 50mm and an inner concentric circular hole diameter of 8 mm.
As shown in figure 3, the diameter of the customized corundum rod is 8mm, the length of the customized corundum rod is determined according to the distance between a motor and the liquid level of molten iron, a 60mm long thread is turned at one end of the customized corundum rod, a matched nut is arranged, the corundum rod with the turned threaded end penetrates into a concentric circular hole of a carbon brick sample, and the nut is screwed to fix the sample.
The specific operation steps of the test are as follows:
(1) randomly drilling 5 concentric cylindrical test samples with the outer diameter of 30mm, the inner diameter of 8mm and the height of 50mm from a complete blast furnace carbon brick; grinding the surface, polishing, cleaning (alcohol), measuring the volume of the sample by adopting a drainage method, drying in a drying oven for 12h, and taking out;
(2) weighing the dried sample by using a balance, measuring the diameter of the sample by using a vernier caliper, photographing the sample, and observing the macro morphology of the sample before reaction; fixing the sample on a customized corundum rod, randomly sampling from the complete blast furnace carbon brick, and preparing a scanning electron microscope sample for SEM-EDS analysis;
(3) before the test, a group of blank tests are firstly carried out so as to be compared and analyzed with the blast furnace carbon brick molten iron corrosion resistance test result, and the influence degree of the high-temperature environment on the carbon brick sample is eliminated.
(4) The reagents of reduced iron powder, graphite powder, silicon powder, manganese powder, phosphorus powder and ferrous disulfide powder adopted for preparing the iron sample are put into a drying oven to be dried for 4 hours at the temperature of 110 +/-5 ℃, 770.77g of iron sample is prepared according to the ingredients of molten iron set by the test, and the iron sample is sealed and stored after being uniformly mixed.
(5) 770.77g of iron sample is put into a corundum crucible with the outer diameter of 62mm, the height of 300mm and the wall thickness of 3mm, and the whole corundum crucible is placed in the middle of a constant temperature area of a tubular furnace to prevent the corundum crucible from being bonded with the side wall of the furnace tube.
(6) And starting the SRS13A precision temperature controller, setting a temperature program, and setting the heating rate and the cooling rate to be 5 ℃/min. The specific temperature-raising and temperature-lowering procedures are as follows:
firstly, heating from 0 ℃ to 300 ℃ for 60 min;
secondly, heating from 300 ℃ to 1000 ℃ for 140 min;
thirdly, heating from 1000 ℃ to 1500 ℃ for 100 min;
fourthly, preserving heat at 1500 ℃ for 180 min;
fifthly, cooling from 1500 ℃ to 1000 ℃ for 100 min;
sixthly, cooling from 1000 ℃ to 300 ℃ for 140 min;
and seventhly, cooling from 300 ℃ to 25 ℃ for 55 min.
The temperature of the remaining 33 steps was then set to 25 ℃ for 0 min. After the program setting is completed, the set program is checked.
(7) Opening an argon gas cylinder, and setting a flow meter to be 3L/min; starting a heating key, and starting the tube furnace by pressing the RUN key for 3-5 s.
(8) When the temperature of the tube furnace is raised to 1500 ℃, keeping the temperature for 1h and stirring by adopting a quartz tube so as to ensure that the iron sample is completely melted and the components are uniform.
(9) After the constant temperature is kept for 40min, the non-sample end of the corundum rod is connected with a stirring device, the sample end is placed in a tube furnace tube to be preheated for 20min, then the corundum rod is slowly moved downwards and is immersed 30mm below the liquid level of molten iron, the rotating speed of a stirrer is set to be 60r/min, a switch is opened after the time is 120min to start a test, and the rotating speed and the time can be adjusted according to the test requirement.
(10) And (3) extracting 3-5 g of iron sample by adopting a pipette and a quartz tube every 30min in the test process, and quickly quenching with water for 4 times. And when the iron sample is extracted, the stirring motor is suspended from rotating, and the extraction time is controlled within 1 min.
(11) And after stirring is finished, lifting the cylindrical carbon brick sample to separate the cylindrical carbon brick sample from molten iron, starting a stirring motor to rotate for 5min to remove iron beads attached to the surface of the sample, stopping ventilation after the program is cooled to room temperature, closing the tubular furnace, taking out the carbon brick sample, and performing subsequent performance evaluation.
(12) The mass of the sample was weighed using a balance, the diameter of the sample was measured using a vernier caliper, and the rate of change in mass, the degree of erosion, and the rate of erosion of the sample were calculated. And (4) photographing the sample, and observing the macroscopic morphology change of the sample after reaction. The volume of the sample was measured by a drainage method, and the rate of change in volume of the sample was calculated.
(13) And drying the sample in a drying oven for 12 hours, taking out the dried sample, manufacturing a scanning electron microscope sample, carrying out SEM-EDS analysis, observing the microscopic morphology and structural characteristics of the reacted sample, analyzing a phase formed after the reaction through the EDS, carrying out line scanning to observe the content distribution rule of iron elements from outside to inside, and carrying out surface scanning to observe the distribution rule of different elements in the whole surface so as to clarify the corrosion mechanism of the molten iron on the blast furnace carbon brick and the damage degree of the molten iron on the structure of the blast furnace carbon brick.
(14) And detecting the carbon content in the extracted iron sample, and determining the carburization rate of the molten iron, namely the erosion speed of the molten iron on the carbon bricks.
(15) The larger the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburization rate are, the poorer the molten iron corrosion resistance of the blast furnace carbon brick is.
In summary, the technical solution provided by the embodiment of the present invention at least has the following beneficial effects:
the invention has the technical advantages of simple sample preparation, simple and convenient operation, high test success rate and comprehensive and accurate evaluation index. The method specifically comprises the following two aspects:
on one hand, the erosion condition of the molten iron composition, the temperature and the flow rate of the blast furnace hearth on the side wall carbon brick under the actual working condition can be well simulated, and the test result is closer to the actual service environment of the carbon brick;
on the other hand, the introduced evaluation indexes are comprehensive and accurate, the corrosion degree of the molten iron in the blast furnace hearth on the carbon bricks can be systematically evaluated, and the mechanism of the whole corrosion process is analyzed.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A test device for evaluating molten iron corrosion resistance of blast furnace carbon bricks is characterized by comprising a high-temperature reaction tubular furnace, wherein a high-purity argon gas cylinder and a precise temperature controller are arranged beside the high-temperature reaction tubular furnace, a long constant-temperature area is arranged at the middle position of a furnace tube of the high-temperature reaction tubular furnace, and the upper end and the lower end of the high-temperature reaction tubular furnace are respectively provided with an upper furnace cover and a lower furnace cover with central openings;
wherein: the furnace is characterized in that a corundum crucible is arranged in the long constant-temperature area, molten iron is arranged in the corundum crucible, a stirring device is inserted in the center of the upper furnace cover, the lower end of the stirring device is connected with a corundum rod sleeved with blast furnace carbon bricks, an air inlet pipe is inserted in the center of the lower furnace cover, and the air inlet pipe is connected with a rotor flow meter and an air bottle.
2. The test apparatus as claimed in claim 1, wherein the high temperature reaction tube furnace is a BTML-1700 ℃ high temperature reaction tube furnace, and the precise temperature controller is an SRS13A precise temperature controller.
3. The testing device of claim 1, wherein the stirring device comprises a constant speed electric stirrer, a stirring motor, and a motor mount, wherein: the stirring device is characterized in that the motor support is erected on the high-temperature reaction tube furnace, the stirring motor is arranged on the motor support, and the lower end of a rotating shaft of the stirring motor is connected with a stirring blade or a corundum rod sleeved with blast furnace carbon bricks.
4. The test device according to claim 1, wherein the diameter of the corundum rod sleeved with the blast furnace carbon brick is 8mm, and the length of the corundum rod is determined according to the distance between the motor and the molten iron liquid level; the blast furnace carbon brick is a cylinder with a concentric through hole, the outer diameter of the cylinder is 30mm, the height of the cylinder is 50mm, and the diameter of an inner concentric round hole is 8 mm.
5. The test device according to claim 4, wherein the corundum rod sheathed with the blast furnace carbon brick is threaded with 60mm long threads at one end and is provided with a matching nut, and the corundum rod sheathed with the blast furnace carbon brick is prepared by inserting the threaded end of the corundum rod into the concentric circular holes of the blast furnace carbon brick and screwing the nut.
6. The test apparatus as claimed in any one of claims 1 to 2, wherein the tube of the high temperature reaction tube furnace is made of corundum, and has an inner diameter of 80mm and a height of 900 mm.
7. The testing device according to claim 1, wherein the length of the long constant temperature area is 100mm, the heating temperature range is 0-1700 ℃, and a refractory brick pad is arranged below the constant temperature area.
8. A method for evaluating molten iron corrosion resistance of a blast furnace carbon brick by using the test device of any one of claims 1 to 7, the method comprising:
(1) sample preparation: manufacturing blast furnace carbon bricks into a cylindrical sample, sequentially grinding, polishing, cleaning and drying the surface of the cylindrical sample, fixing the cylindrical sample on a corundum rod, connecting the corundum rod with a stirring device, and simulating the corrosion condition of molten iron circulation in a hearth of a medium-high furnace to the blast furnace carbon bricks by adjusting the rotating speed of an electric stirrer by adopting a rotating cylinder method;
(2) and (4) evaluating the result: the molten iron corrosion resistance of the blast furnace carbon brick is evaluated through the mass change rate, the corrosion degree, the corrosion rate, the volume change rate, the molten iron penetration depth and the molten iron carburization rate of the blast furnace carbon brick.
9. The evaluation method according to claim 8, wherein the evaluation method comprises the following specific steps:
the method comprises the following steps: manufacturing a blast furnace carbon brick into a concentric cylindrical sample, sequentially grinding, polishing and cleaning the surface of the concentric cylindrical sample, measuring the volume of the concentric cylindrical sample by adopting a drainage method, and drying the concentric cylindrical sample in a drying box;
step two: weighing the mass of the concentric cylindrical sample by using a balance, measuring the diameter of the concentric cylindrical sample by using a vernier caliper, photographing the concentric cylindrical sample, and observing the macroscopic morphology of the concentric cylindrical sample before corrosion;
step three: fixing the concentric cylindrical sample on a corundum rod, randomly sampling from the blast furnace carbon brick, and preparing a scanning electron microscope sample for SEM-EDS analysis;
step four: before corrosion, a group of blank tests are carried out so as to be compared and analyzed with the molten iron corrosion resistance test result of the blast furnace carbon brick, and the influence degree of a high-temperature environment on the concentric cylindrical sample is eliminated;
step five: drying a reagent adopted for preparing an iron sample in a drying box, preparing the iron sample according to actual molten iron components, uniformly mixing, and sealing for storage;
step six: putting the iron sample obtained in the step five into a corundum crucible, and placing the corundum crucible in the middle of a constant-temperature area of the high-temperature reaction tube furnace length to prevent the corundum crucible from being bonded with the side wall of the furnace tube;
step seven: starting a precision temperature controller, setting a temperature program, and checking the set program after the program is set; opening an argon gas cylinder, setting a flow meter, starting a heating key high-temperature reaction tube furnace and starting heating;
step eight: after the temperature of the high-temperature reaction tube furnace is raised to 1500 ℃, keeping the temperature and stirring by adopting a quartz tube so as to ensure that the iron sample is completely melted and the components are uniform; then keeping the temperature constant, putting the corundum rod at the lower end of the stirring device into a furnace tube of a high-temperature reaction tube furnace for preheating, then slowly moving the corundum rod downwards and immersing the corundum rod below the liquid level of molten iron, and adjusting the rotating speed and time according to the test requirement;
step nine: in the corrosion process, a pipette and a quartz tube are adopted to extract an iron sample at intervals, and water quenching is rapidly carried out for 4 times; when the iron sample is extracted, the stirring motor is suspended from rotating, and the extraction time is controlled within 1 min;
step ten: after the corrosion is finished, lifting the corundum rod for fixing the concentric cylindrical sample to separate the corundum rod from molten iron, starting a stirring motor to rotate to spin off iron beads attached to the surface of the sample, stopping ventilation after the program is cooled to room temperature, closing the high-temperature reaction tube furnace, taking out the concentric cylindrical sample, and performing subsequent performance evaluation;
step eleven: weighing the mass of the corroded concentric cylindrical sample by using a balance, measuring the diameter of the corroded concentric cylindrical sample by using a vernier caliper, and calculating the mass change rate, the corrosion degree and the corrosion rate of the corroded concentric cylindrical sample;
step twelve: photographing the corroded concentric cylindrical sample, and observing the difference and the similarity between the reacted macroscopic morphology of the corroded concentric cylindrical sample and the macroscopic morphology of the corroded concentric cylindrical sample before corrosion; measuring the volume of the corroded concentric cylindrical sample by adopting a drainage method, and calculating the volume change rate of the sample by combining the first step;
step thirteen: drying in a drying oven, manufacturing a scanning electron microscope sample, carrying out SEM-EDS analysis, observing the microscopic morphology and structural characteristics of the sample after reaction, analyzing a phase formed after the reaction through the EDS, carrying out line scanning to observe the content distribution rule of iron elements from outside to inside, and carrying out surface scanning to observe the distribution rule of different elements in the whole surface so as to clarify the corrosion mechanism of the molten iron on the blast furnace carbon brick and the damage degree of the molten iron on the structure of the blast furnace carbon brick;
fourteen steps: and (4) extracting the carbon content in the iron sample for nine times in the detection step, and determining the carburization rate of the molten iron so as to obtain the corrosion speed of the molten iron on the blast furnace carbon brick.
10. The evaluation method according to claim 9, wherein the slowly downwardly moving corundum rod is immersed below the molten iron level by a distance of 30 mm.
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Inventor after: Wang Cui Inventor after: Zhang Jianliang Inventor after: Chen Qianwan Inventor after: Li Xiaolei Inventor after: Pang Zhenping Inventor after: Wang Tongsheng Inventor after: Jiao Kexin Inventor after: Wang Zhongyi Inventor before: Zhang Jianliang Inventor before: Wang Cui Inventor before: Chen Qianwan Inventor before: Li Xiaolei Inventor before: Pang Zhenping Inventor before: Wang Tongsheng Inventor before: Jiao Kexin Inventor before: Wang Zhongyi |