CN103645114A - Iron-containing raw material gas-based reduction and slagging process experiment method and iron-containing raw material gas-based reduction and slagging device - Google Patents
Iron-containing raw material gas-based reduction and slagging process experiment method and iron-containing raw material gas-based reduction and slagging device Download PDFInfo
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- CN103645114A CN103645114A CN201310691946.2A CN201310691946A CN103645114A CN 103645114 A CN103645114 A CN 103645114A CN 201310691946 A CN201310691946 A CN 201310691946A CN 103645114 A CN103645114 A CN 103645114A
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Abstract
The invention provides an iron-containing raw material gas-based reduction and slagging process experiment method which comprises the steps of pressing a ground iron-containing raw material into a block which is taken as a sample; placing the sample in an environment of simulating gas-based reduction and slagging for performing a gas-based reduction experiment; meanwhile, recording weight loss and tail gas component data of the sample in a reduction process in real time; and after the gas-based reduction experiment is ended, performing a high-temperature slagging experiment on the sample, and preserving the sample in a high-temperature crustal structure by a water quenching method after dropping through high-temperature melting. According to the method, the problems that the existing experiment method and the existing device can not meet the process detection and later-period sampling requirements and the inconvenience is brought to the operation when the reducibility and the slagging characteristic of the iron-containing raw material are researched by adopting different equipment, and the like are solved, the method provided by the invention is creatively provided by combining with the case of closely relating to the gas-based reduction and slagging processes of the iron-containing raw material gas in a cohesive zone according to the principle that a blast furnace is a continuous production process for researching the influence rule of the reduction of the iron-containing raw material to slagging. The invention further provides an experiment device for realizing the method.
Description
Technical field
The present invention relates to metallurgical engineering technical field, relate in particular to a kind of iron-bearing material gas base reduction, slagging course experimental technique, and a kind of device of realizing the method.
Background technology
The metallurgical performance of measuring the iron-bearing materials such as sintering deposit, pellet, lump ore is an important research content in metallurgical engineering experiment, and it contributes to instruct ironmaking processes, and particularly the suitable burden structure of blast furnace ironmaking process choosing is to reach the object of cost efficiency.Generally, the metallurgical performance of iron-containing charge mainly comprises reductibility, low-temperature reduction disintegration, soften-melting of loading reduction drippage property etc. conventionally, and experimental technique and device that each metallurgical performance detects are comparatively independent.In contrast, blast furnace ironmaking process is actually a continuous system, not separate between different metallurgical performances, on the contrary by the direct motion of the joint effect working of a furnace that interacts to each other.Therefore, be necessary to develop a kind of relatively more comprehensive, experimental technique and device of taking into account mutual relationship between iron-bearing material difference metallurgical performances.
In blast furnace ironmaking process, cohesive zone is as the critical area of " forming a connecting link " in stove, affect the quadratic distribution of Gas Flow and beginning to take shape of blast furnace slag, formation mechanism and the influence factor of studying and grasp blast furnace melting with soft have important directive significance for actual production.With regard to cohesive zone inside, iron-bearing material participates in reduction and slagging reaction simultaneously, relate to its reductibility, loading reduction softening-metallurgical performances such as melting drippage property, particularly interaction relationship are between the two most important for parsing cohesive zone feature.With regard to existing detection means, the reductibility of iron-bearing material mainly adopts experimental technique and the device described in standard GB/T/T 13241-91 to test, and the test of soften-melting of loading reduction drippage property does not have relevant domestic or international standard, what is more important lacks at present corresponding experimental technique and installs with the interaction relationship between the above-mentioned two kinds of metallurgical performances of study tour.In addition, with regard to the existing experimental technique and device detecting for iron-bearing material metallurgical performance, mainly there is following some deficiency in it:
because the desired granularity of sample is larger, in solid particulate reagent layer, diffusion and product layer external diffusion become the easily measurement of impact to sample metallurgical performance of restricted link;
because single sample size is more, each particle is in different experimental situations, and the difference of the metallurgical performance that causes has increased the difficulty of experiment later stage sampling work;
after high temperature experiment, sample is mainly by gas cooled, and lower cooldown rate is unfavorable for preserving the slag structure under hot conditions;
single balance measurement requires sample, hanging basket and gross mass wiry can not surpass the range of balance, limits to a certain extent the following further exploitation to measuring system.In sum, reduction, slagging behavior and interaction thereof around research iron-bearing material in blast furnace melting with soft, existing experimental technique and device cannot meet process and detect and later stage sampling requirement.
Summary of the invention
For above shortcomings in prior art, object of the present invention is mainly to provide the interaction relationship of a kind of experimental technique with research iron-bearing material reductibility and slagability (being soft heat-drippage property), solve existing experimental technique and device and cannot meet process detection and later stage sampling requirement, and need to adopt different equipment to study reductibility and the Slag-formation characteristics of iron-bearing material, there is the problem of complex structure, inconvenient operation.
In addition, the present invention also provides the device of realizing the reduction of iron-bearing material gas base, slagging course experimental technique.
For achieving the above object, the present invention adopts following technological means:
The reduction of iron-bearing material gas base, a slagging course experimental technique, is characterized in that, comprises the following steps:
1) after grinding, iron-bearing material is pressed into bulk as sample;
2) sample is put into the environment of the reduction of simulation gas base, slagging, carried out gas base reduction experiment; Weightlessness and the exhaust gas component data of sample in while real time record reduction process; Wherein, reducing gas composition, temperature of reaction and reaction time carry out setting according to the requirement of gas base reduction experiment;
3) after gas base reduction experiment finishes, sample is carried out to slagging experiment, sample after high-temperature fusion drippage by shrend method to preserve its high temperature crystal structure; Wherein, the heating rate of gas componant, temperature of reaction is set according to high temperature slagging requirement of experiment.
The gas componant that described step 3) is set depends on experimental program, if be set to inert atmosphere, (includes but not limited to N
2, He), the action rule of the static reduction degree of study tour sample to its slagability; If be set to reducing atmosphere, (include but not limited to CO, H
2), the action rule of the dynamic reduction degree of study tour sample to its slagability.
Described step 2) and 3) temperature of reaction set all depends on experimental program, for the gas base reduction reaction of iron-bearing material, its temperature of reaction is set in 800 ~ 1100 ℃ conventionally; And react for the high temperature slagging of iron-bearing material, its temperature is set in 1200 ~ 1500 ℃ conventionally.
Further, the present invention also provides a kind of reduction of iron-bearing material gas base, slagging course experimental provision of realizing said method, it is characterized in that, comprises air supply system, reacting furnace and heating system thereof, Weighing system and sample collection tank;
Described air supply system comprises CO, CO
2, H
2with a plurality of gas cylinders of inert gas, also comprise the bottle valve and the spinner-type flowmeter that are connected with each gas cylinder respectively; The escape pipe of described gas cylinder is connected with main pipeline gas circuit and is provided with air valve and spinner-type flowmeter, drying bottle, damping device and U-shaped differential manometer;
Described reacting furnace and heating system thereof comprise heating element and control upper furnace body and the lower furnace body of thermopair; Upper furnace body middle part is provided with reaction tube, and reaction tube is provided with reaction tube suitable for reading and gland bonnet, side end opening and gland bonnet and positive end opening and gland bonnet; Described gland bonnet suitable for reading is provided with nickel chromium triangle tinsel, and nickel chromium triangle lower end wiry is provided with for placing the nickel chromium triangle hanging basket of sample, and nickel chromium triangle upper end wiry is connected with meausring apparatus; Described side end opening and gland bonnet are connected with main pipeline gas circuit, are also provided with reaction tube gas admittance valve in this gas circuit; Under described positive end opening and gland bonnet, be provided with sample collection tank; The top of reaction tube is also provided with reaction tube outlet pipe and air outlet valve; On reaction tube outlet pipe, be also provided with for measuring gas analyzer and tail gas burner and the combustion box of tail gas;
Described Weighing system comprises the gentle secondary electrons balance in one-level sky; Described one-level balance one end connects the above-mentioned nickel chromium triangle tinsel that articulates hanging basket and sample, and the other end is put into the counterweight of balance with it, and counterweight end connects secondary electrons balance simultaneously;
Between the inlet, outlet pipeline of reacting furnace, be also provided with straight-through tail gas valve.
Further, described damping device comprises pre-wetting bottle, main humidification bottle and additional wet bottle; Described main humidification bottle and additional wet bottle are placed in water-bath tank and are heated by resistive heater; In water-bath tank, be provided with electronic thermometer.
Compared to existing technology, the present invention has following beneficial effect:
1, the present invention solves existing experimental technique and installs and cannot meet process detection and later stage sampling requirement, and adopt different equipment to study reductibility and the Slag-formation characteristics of iron-bearing material, there is the problems such as inconvenient operation, it according to blast furnace itself, is the principle of continuous flow procedure, closely related in conjunction with iron-bearing material gas base reduction in cohesive zone, slagging course, creationary proposition the inventive method is studied the affect rule of iron-bearing material reduction on slagging.
2, the inventive method can successively detect successively reductibility and the slagability of iron-bearing material in an experimentation, contribute to study the former interactively to the latter, solved the problem that existing method cannot directly be set up interactively between two kinds of different metallurgical performances.And by first dehumidification again water-bath humidification to the steam that quantitatively makes up water in mixed gas, contribute to regulate reduction potential height by controlling hydrogen and water vapor ratio, solve existing method and at use hydrogen, cannot reduce the problem of its reduction potential during as reducing gas.
3, the inventive method directly adopts the method for shrend to preserve sample for the rear sample of high temperature slagging experiment, the maximum high temperature crystal structure of reserve sample, contribute to further by X-ray diffractometer, scanning electron microscope, to study iron-bearing material by reducing to the transformation behavior of slagging, for resolving blast furnace melting with soft formation mechanism, provide new thinking.
4, according to the thinking of the inventive method, the device of design low-temperature reduction, high temperature slagging.Reacting furnace and heating system design thereof adopt the upper furnace body and the lower furnace body that comprise heating element and control thermopair to form, the temperature of separate reaction zones and gas preheating zone is controlled, also in research gas-solid countercurrent reaction process, reflex action provides new approach to solid iron-bearing material for mixed gas temperature and thermo-lag.
5, bottom mixed gas entrance and sample outlet adopt design from the bottom to top, realize the independent temperature control to experiment reduction reaction and mixed gas preheating, can meet again the space of the abundant preheating of mixed gas.Adopt " h " shape corundum reaction tube both can guarantee that mixed gas carried out reduction reaction with sample by reaction tube side end opening after the preheating of alundum (Al2O3) ball layer, after realization response, sample falls into by the positive end opening of reaction tube the sample collection tank that water is housed and realizes cooling fast again.
6, Weighing system adopts two days flat structures, adopt two days flat structures of the gentle secondary electrons balance in one-level sky to come the weightlessness of real time record experimentation sample to change, by change counterbalance mass arbitrarily balance mate sample mass and without the restriction that is subject to balance range, contribute to expand the scope of application of apparatus of the present invention sample.
7, iron-bearing material gas base of the present invention reduction, slagging course experimental provision mainly comprise air supply system, reacting furnace and heating system thereof, Weighing system and sample collection tank, its reasonable in design, are skillfully constructed, and have simple in structure, convenient and practical feature.
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Accompanying drawing explanation
Fig. 1 is the structural representation of iron-bearing material gas base reduction slagging process experiment device of the present invention.
In figure, 1-gas cylinder, 2-bottle valve and spinner-type flowmeter, 3-1-main pipeline air valve and spinner-type flowmeter, 3-2-reaction tube gas admittance valve, the straight-through tail gas valve of 3-3-, 3-4-reaction tube air outlet valve, 4-are containing anhydrous CaCl
2drying bottle, 5-is wetting bottle in advance, the main humidification bottle of 6-, the additional wet bottle of 7-, 8-resistive heater, 9-water-bath tank, 10-electronic thermometer, 11-U type differential manometer, 12-secondary electrons balance, 13-one-level balance, 14-" h " shape corundum reaction tube, suitable for reading and the gland bonnet of 15-reaction tube, 16-sample is with nickel chromium triangle hanging basket and be connected nickel chromium triangle tinsel, 17-reacting furnace body of heater and heating element, 18-chooses K/R type thermopair according to temperature of reaction, 19-chooses K/R type thermopair according to reacting furnace heating-up temperature, 20-preheating furnace body of heater and heating element, 21-alundum (Al2O3) ball layer, 22-1-reaction tube side end opening and gland bonnet, the positive end opening of 22-2-reaction tube and gland bonnet, 23-chooses K/R type thermopair according to preheating furnace heating-up temperature, 24-aqueous specimen is collected tank, 25-gas analyzer, 26-tail gas burner and combustion box.
Embodiment
Below in conjunction with drawings and Examples, technical scheme of the present invention is described in further detail.
The reduction of iron-bearing material gas base, a slagging course experimental technique, comprise the steps:
1) iron-bearing material is milled to below 200 orders, and under 20 MPa pressure, to be pressed into bottom surface diameter be 15 mm, thickness is that the right cylinder piece of 5 mm is as sample;
2) sample is put into the environment of the reduction of gas base, slagging, carried out gas base reduction experiment; Weightlessness and the exhaust gas component data of sample in while real time record reduction process; Wherein, reducing gas composition, temperature of reaction and reaction time carry out setting according to the requirement of gas base reduction experiment;
3) by the sample after gas base reduction, sample is carried out to slagging experiment, sample after high-temperature fusion drippage by shrend method to preserve its high temperature crystal structure; Wherein, gas componant, temperature of reaction and heating rate are set according to high temperature slagging requirement of experiment.
The reduction of iron-bearing material gas base, the slagging course experimental provision of realizing said method, comprise air supply system, reacting furnace and heating system thereof, Weighing system; Described air supply system comprises CO, CO
2, H
2with a plurality of gas cylinders 1 of inert gas, also comprise the bottle valve and the spinner-type flowmeter 2 that are connected with each gas cylinder 1 respectively; The escape pipe of described gas cylinder 1 is connected with main pipeline gas circuit and is provided with air valve and spinner-type flowmeter 3-1, drying bottle 4, damping device and U-shaped differential manometer 11.
Described reacting furnace and heating system thereof comprise that the upper furnace body of heating element 17 and control thermopair 19 thereof preheats element 20 and controls thermopair 23 lower furnace bodies with comprising; Upper furnace body middle part is provided with reaction tube 14, and reaction tube 14 is provided with reaction tube suitable for reading and gland bonnet 15, side end opening and gland bonnet 22-1 and positive end opening and gland bonnet 22-2; Described gland bonnet suitable for reading 15 is provided with nickel chromium triangle tinsel 16, and the lower end of nickel chromium triangle tinsel 16 is provided with for placing the nickel chromium triangle hanging basket of sample, and the upper end of nickel chromium triangle tinsel 16 is connected with meausring apparatus; Described side end opening and gland bonnet 22-1 are connected with main pipeline gas circuit, are also provided with reaction tube gas admittance valve 3-2 in this gas circuit; Under described positive end opening and gland bonnet 22-2, be provided with sample collection tank 24; The top of reaction tube 14 is also provided with reaction tube outlet pipe and air outlet valve 3-4; On reaction tube 14 outlet pipes, be also provided with for measuring gas analyzer 25 and tail gas burner and the combustion box 26 of tail gas; Between the inlet, outlet pipeline of reacting furnace, be also provided with straight-through tail gas valve 3-3.
Described Weighing system comprises one-level balance 13 and secondary electrons balance 12; Described one-level balance 13 one end connect the above-mentioned nickel chromium triangle tinsel 16 that articulates hanging basket and sample, and the other end is put into the counterweight of balance with it; Upper end connects secondary electrons balance 12 simultaneously; With two days flat structures of one-level balance 13 and secondary electrons balance 12, come the weightlessness of real time record experimentation sample to change.
Described damping device comprises pre-wetting bottle 5, main humidification bottle 6 and additional wet bottle 7 and electronic thermometer 10; Described main humidification bottle 6 and additional wet bottle 7 are placed in water-bath tank 9 and are heated by resistive heater 8.The bottom of described reaction tube 14 is also provided with alundum (Al2O3) ball layer 21.
The present invention adopts " h " shape corundum reaction tube 14 both can guarantee that mixed gas carried out reduction reaction with sample by reaction tube side end opening 22-1 after 21 preheating of alundum (Al2O3) ball layer, and after realization response, sample falls into aqueous specimen by the positive end opening 22-2 of reaction tube and collects tank 24 and realize cooling fast again.
The method that adopts described iron-bearing material gas base reduction, slagging course experimental provision to test, comprises the following steps:
1) iron-bearing material is milled to 200 orders following (being less than 0.074 mm), and under 20 MPa pressure, to be pressed into bottom surface diameter be 15 mm, thickness is the right cylinder piece (being designated hereinafter simply as sample) of 5 mm;
2) sample is placed in nickel chromium triangle hanging basket, and by nickel chromium triangle tinsel, be suspended on the middle part of reaction tube, nickel chromium triangle tinsel upper end connects one end of one-level balance, the counterweight that this balance other end placement is identical with sample, hanging basket and connection metal silk gross mass, and upper end connects secondary electrons balance simultaneously;
3) open the air inlet of argon gas gas cylinder and the valve of giving vent to anger, after question response inner air tube is emptying, off-response pipe outlet pipe and air outlet valve, open straight-through tail gas valve simultaneously, by regulating spinner-type flowmeter to obtain the gas flow of setting, after gas is dry, carry out water-bath humidification, by measuring the general pressure of gas after humidification, determine the heating-up temperature of water-bath tank, to guarantee that water vapor in mixed gas reaches the proportioning of setting;
4) open the heating element and the power supply that preheats element of reacting furnace and heating system thereof simultaneously, upper lower furnace body is heated; After the reduction reaction temperature and gas preheat temperature that reaches respectively setting until upper and lower two stoves, according to preset proportion configuration mixed gas, open reaction tube air inlet and close straight-through tail gas valve with the valve of giving vent to anger simultaneously;
5) when the reduction of iron-bearing material sample gas base is carried out, by secondary electrons balance, directly read the real-time weightless data of sample process, after Extraction parts reduction simultaneously, tail gas is through gas analyzer the real time measure compositional data, and all the other tail gas enter burner combustion.
Reach and set after the reaction time, close each mixed gas gas cylinder air valve and open argon gas gas cylinder air valve simultaneously, open reaction tube top cover labyrinth and positive lower sealing cover, off-response stove and preheating furnace power supply, connection metal silk is removed from one-level balance, tank under the rear sample of reaction falls into according to Action of Gravity Field, by cooling with the reduction feature under research sample different phase fast.
Reach and set after the reaction time, close each mixed gas gas cylinder air valve and open argon gas gas cylinder air valve simultaneously, open the positive lower sealing cover of reaction tube, close anti-preheating furnace power supply, by current temperature of reaction, rise according to the heating rate of setting and continue rising reacting furnace temperature, the rear sample of reaction is slagging progressively, and tank under entering after soft melting dropping, by cooling to study the slagging feature of the different reduction phase products of sample fast.
embodiment 1:the reduction of iron-bearing material gas base, a slagging course experimental technique, comprise the following steps:
1) get di-iron trioxide pure reagent (purity is greater than 99%) 100 g, be milled to below 200 orders, then take out wherein 5 g and be placed in mould, under 20 MPa pressure, being pressed into bottom surface diameter is 15 mm, and thickness is the right cylinder piece of 5 mm;
2) sample is placed in the hanging basket of molybdenum filament making, and be suspended on reacting furnace middle part by metal molybdenum filament, top connects one-level balance, this balance other end is put into 30 g counterweights (general assembly (TW) of hanging basket and metal molybdenum filament is 25 g), and be connected on secondary electrons balance, cover reaction tube top cover labyrinth and two lower sealing cover;
3) open nitrogen valve, the air in emptying reaction tube is opened reacting furnace and preheating furnace power supply simultaneously, and two stove target temperatures are all set to 1000 ℃;
4) after reaching 1000 ℃, open carbon monoxide valve, regulating the spinner-type flowmeter of nitrogen, carbon monoxide is 2 L/min;
5) sample starts reduction, and secondary electrons balance shows in real time weight loss and reads in computer, calculates the real-time reduction degree of sample;
6) after sample reduction degree reaches 50%, close carbon monoxide valve, reacting furnace target temperature is set to 1200 ℃ simultaneously, and heating rate is 10 ℃/min;
7) after reaching 1200 ℃, further constant temperature 60 min;
8) after 60 min, aqueous specimen is collected to tank and be placed on reaction tube below, open the positive lower sealing cover of reaction tube simultaneously, from one-level balance, remove the metal molybdenum filament that hangs with sample, allow sample fall under gravity into sample collection tank;
9) fast cooling samples of obtaining, analyzes the slagging feature of di-iron trioxide under 50% reduction degree level (topographic profile, thing distribute mutually, component distributing etc.) by scanning electron microscope and X diffractometer.
On the basis of above-mentioned experiment, by changing sample reduction degree level (60%, 70%, 80%, 90%) in step 6), to investigate iron-bearing material impact on its slagability in different reduction degree levels, the i.e. action rule of the static reduction degree of iron-bearing material to its slagability.
In above-mentioned iron-bearing material gas base reduction slagging process experiment method, the selection of described step 3) setting gas flow depends on that under experiment condition, the interior gas flow rate of corundum reaction tube is broken through gas boundary layer, i.e. the further increase of gas flow rate no longer changes the reaction rate of sample.Wherein, experimental program is depended in the selection of water vapor setting proportioning, and by controlling temperature in water-bath tank, the general pressure of measuring humidification front and back mixed gas is calculated the dividing potential drop of water vapor, whether meets the requirement of experimental program to investigate its proportioning in mixed gas.
embodiment 2:adopt said apparatus to carry out the reduction of iron-bearing material gas base, slagging course experimental technique, comprise the following steps:
1) ~ 5) with embodiment 1;
6) after sample reduction degree reaches 50%, reacting furnace target temperature is set to 1200 ℃, and heating rate is 10 ℃/min;
7) after reaching 1200 ℃, further constant temperature 60 min;
8) after 60 min, close carbon monoxide valve, record the final reduction degree level of sample, aqueous specimen is collected to tank and be placed on reaction tube below, open the positive lower sealing cover of reaction tube simultaneously, from one-level balance, remove the metal molybdenum filament that hangs with sample, allow sample fall under gravity into sample collection tank;
9) fast cooling samples of obtaining, by scanning electron microscope and X diffractometer, analyze di-iron trioxide after reaching 50% reduction degree level, slagging feature under carbon monoxide reducing atmosphere (topographic profile, thing distribute mutually, component distributing etc.), and by contrasting with embodiment 1 result that obtains, the action rule of the dynamic reduction degree of high spot reviews iron-bearing material to its slagability.
embodiment 3:adopt said apparatus to carry out the reduction of iron-bearing material gas base, slagging course experimental technique, comprise the following steps:
1) get Iron Ore Powder (Australia ore deposit, Brazilian ore deposit or domestic fine ore all can) 100 g, be milled to below 200 orders, then take out wherein 5 g and be placed in mould, under 20 MPa pressure, being pressed into bottom surface diameter is 15 mm, and thickness is the right cylinder piece of 5 mm;
2) sample is placed in the hanging basket of molybdenum filament making, and be suspended on reacting furnace middle part by metal molybdenum filament, top connects one-level balance, this balance other end is put into 30 g counterweights (general assembly (TW) of hanging basket and metal molybdenum filament is 25 g), and be connected on secondary electrons balance, cover reaction tube top cover labyrinth and two lower sealing cover;
3) open nitrogen valve, air in emptying reaction tube, the air inlet of off-response pipe is opened straight-through tail gas valve with the valve of giving vent to anger simultaneously, by regulating the spinner-type flowmeter of nitrogen, be 4 L/min, first be dried and carry out afterwards water-bath humidification, regulating the temperature of heating water bath is 46 ℃, after mensuration humidification, the general pressure of gas is about 111 kPa, current atmospheric pressure is about 101 kPa, calculate thus the proportioning of water vapor in mixed gas and be about 9 %(volume fractions), open the power supply of reacting furnace and preheating furnace simultaneously, two stove target temperatures are all set to 1200 ℃;
4) after reaching 1200 ℃, open hydrogen valve, regulating the spinner-type flowmeter of nitrogen, hydrogen is 2 L/min, opens reaction tube air inlet and closes straight-through tail gas valve with the valve of giving vent to anger simultaneously, now in combination gas, hydrogen and water vapor ratio are 5.56;
5) sample starts reduction, and secondary electrons balance shows in real time weight loss and reads in computer, calculates the real-time reduction degree of sample;
6) after sample reduction degree reaches 50%, close hydrogen valve and stop heating water bath, reacting furnace target temperature is set to 1400 ℃ simultaneously, and heating rate is 10 ℃/min;
7) after reaching 1400 ℃, further constant temperature 60 min;
8) after 60 min, aqueous specimen is collected to tank and be placed on reaction tube below, open the positive lower sealing cover of reaction tube simultaneously, from one-level balance, remove the metal molybdenum filament that hangs with sample, allow sample fall under gravity into sample collection tank;
9) fast cooling samples of obtaining, analyzes the slagging feature of Iron Ore Powder under 50% reduction degree level (topographic profile, thing distribute mutually, component distributing etc.) by scanning electron microscope and X diffractometer.
On the basis of above-mentioned experiment, by changing sample reduction degree level (60%, 70%, 80%, 90%) in step 6), to investigate iron-bearing material impact on its slagability in different reduction degree levels, the i.e. action rule of the static reduction degree of iron-bearing material to its slagability; By contrasting with embodiment 1 result that obtains, can also investigate under identical static reduction degree level the impact of reductive agent on slagability.
embodiment 4:adopt said apparatus to carry out the reduction of iron-bearing material gas base, slagging course experimental technique, comprise the following steps:
1) ~ 5) with embodiment 3;
6) after sample reduction degree reaches 50%, reacting furnace target temperature is set to 1400 ℃, and heating rate is 10 ℃/min;
7) after reaching 1400 ℃, further constant temperature 60 min;
8) after 60 min, close hydrogen valve and stop heating water bath, aqueous specimen being collected to tank and be placed on reaction tube below, opening the positive lower sealing cover of reaction tube simultaneously, from one-level balance, remove the metal molybdenum filament that hangs with sample, allow sample fall under gravity into sample collection tank;
9) fast cooling samples of obtaining, by scanning electron microscope and X diffractometer, analyze Iron Ore Powder after 50% reduction degree level, slagging feature under hydrogen/aqueous vapour reducing atmosphere (topographic profile, thing distribute mutually, component distributing etc.), and by contrasting with embodiment 3 result that obtains, the action rule of the dynamic reduction degree of high spot reviews iron-bearing material to its slagability.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of claim scope of the present invention.
Claims (9)
1. iron-bearing material gas base reduction, a slagging course experimental technique, is characterized in that, comprises the following steps:
1) after grinding, iron-bearing material is pressed into bulk as sample;
2) sample is put into the environment of the reduction of simulation gas base, slagging, carried out gas base reduction experiment; Weightlessness and the exhaust gas component data of sample in while real time record reduction process; Wherein, reducing gas composition, temperature of reaction and reaction time carry out setting according to the requirement of gas base reduction experiment;
3) after gas base reduction experiment finishes, sample is carried out to slagging experiment, sample after high-temperature fusion drippage by shrend method to preserve its high temperature crystal structure; Wherein, gas componant, temperature of reaction and heating rate are set according to high temperature slagging requirement of experiment.
2. iron-bearing material gas base reduction according to claim 1, slagging course experimental technique, is characterized in that, concrete steps are:
1) iron-bearing material is milled to below 200 orders, and under 20 MPa pressure, to be pressed into bottom surface diameter be 15 mm, thickness is that the right cylinder piece of 5 mm is as sample;
2) sample is put into the environment of the reduction of gas base, slagging, carried out gas base reduction experiment; Weightlessness and the exhaust gas component data of sample in while real time record reduction process; Wherein, reducing gas composition, temperature of reaction and reaction time carry out setting according to the requirement of gas base reduction experiment;
3) sample after gas base reduction is carried out to slagging experiment, sample after high-temperature fusion drippage by shrend method to preserve its high temperature crystal structure; Wherein, gas componant, temperature of reaction and heating rate are set according to high temperature slagging requirement of experiment.
3. according to the reduction of iron-bearing material gas base, slagging course experimental technique described in claim 1 or 2, it is characterized in that, the gas componant that described step 3) is set depends on experimental program, if be set to inert atmosphere, (includes but not limited to N
2, He), the action rule of the static reduction degree of study tour sample to its slagability; If be set to reducing atmosphere, (include but not limited to CO, H
2), the action rule of the dynamic reduction degree of study tour sample to its slagability.
4. according to the reduction of iron-bearing material gas base, slagging course experimental technique described in claim 1 or 2, it is characterized in that, described step 2) and 3) temperature of reaction set all depends on experimental program, for the gas base reduction reaction of iron-bearing material, its temperature of reaction is set in 800 ~ 1100 ℃ conventionally; And react for the high temperature slagging of iron-bearing material, its temperature is set in 1200 ~ 1500 ℃ conventionally.
5. according to the reduction of iron-bearing material gas base, slagging course experimental technique described in claim 1 or 2, it is characterized in that, described step 2) and 3) reaction time of setting and the heating rate of setting all depend on experimental program, for the reaction time, it typically is 30 ~ 180 min, for heating rate, it typically is 3 ~ 20 ℃/min.
6. iron-bearing material gas base reduction, a slagging course experimental provision, is characterized in that, comprises air supply system, reacting furnace and heating system thereof, Weighing system and sample collection tank (24);
Described air supply system comprises CO, CO
2, H
2with a plurality of gas cylinders (1) of inert gas, also comprise the bottle valve and the spinner-type flowmeter (2) that are connected with each gas cylinder (1) respectively; The escape pipe of described gas cylinder (1) is connected with main pipeline gas circuit and is provided with air valve and spinner-type flowmeter (3-1), drying bottle (4), damping device and U-shaped differential manometer (11);
Described reacting furnace and heating system thereof comprise that the upper furnace body of heating element (17) and control thermopair (19) thereof preheats element (20) and controls thermopair (23) lower furnace body with comprising; Upper furnace body middle part is provided with reaction tube (14), and reaction tube (14) is provided with reaction tube suitable for reading and gland bonnet (15), side end opening and gland bonnet (22-1) and just end opening and gland bonnet (22-2); Described gland bonnet suitable for reading (15) is provided with nickel chromium triangle tinsel (16), and the lower end of nickel chromium triangle tinsel (16) is provided with for placing the nickel chromium triangle hanging basket of sample, and the upper end of nickel chromium triangle tinsel (16) is connected with Weighing system; Described side end opening and gland bonnet (22-1) are connected with main pipeline gas circuit, are also provided with reaction tube gas admittance valve (3-2) in this gas circuit; Under described positive end opening and gland bonnet (22-2), be provided with sample collection tank (24); The top of reaction tube (14) is also provided with reaction tube outlet pipe and air outlet valve (3-4); On reaction tube (14) outlet pipe, be also provided with gas analyzer (25) and tail gas burner and combustion box (26) for measuring tail gas;
Described Weighing system comprises one-level balance (13) and secondary electrons balance (12); Described one-level balance (13) one end connects the above-mentioned nickel chromium triangle tinsel (16) that articulates hanging basket and sample, and the other end is put into the counterweight of balance with it; Secondary electrons balance (12) directly connects one-level sky placing flat counterweight end;
Between the inlet, outlet pipeline of reacting furnace, be also provided with straight-through tail gas valve (3-3).
7. iron-bearing material gas base reduction according to claim 6, slagging course experimental provision, is characterized in that, described damping device comprises pre-wetting bottle (5), main humidification bottle (6) and additional wet bottle (7); Described main humidification bottle (6) and additional wet bottle (7) are placed in water-bath tank (9) and are heated by resistive heater (8); Water-bath tank (9) is provided with electronic thermometer (10).
8. iron-bearing material gas base reduction according to claim 6, slagging course experimental provision, is characterized in that, described control thermopair (18,19,23) adopts the K/R type thermopair according to temperature of reaction.
9. iron-bearing material gas base reduction according to claim 6, slagging course experimental provision, is characterized in that, the bottom of described reaction tube (14) is also provided with alundum (Al2O3) ball layer (21).
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| CN106645266A (en) * | 2016-11-28 | 2017-05-10 | 辽宁科技大学 | High-temperature molten slag basic performance test method and apparatus, and application method of apparatus |
| CN108593700A (en) * | 2018-05-11 | 2018-09-28 | 武汉钢铁有限公司 | It is a kind of simulation coke blast furnace melting with soft deterioration process test method and simulator |
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| CN108593700B (en) * | 2018-05-11 | 2020-12-11 | 武汉钢铁有限公司 | Test method and simulation device for simulating degradation process of coke in blast furnace reflow zone |
| CN109060587A (en) * | 2018-09-19 | 2018-12-21 | 辽宁科技大学 | A kind of detection of pyrometallurgy reducing property and sampler and method |
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| CN110346538A (en) * | 2019-07-12 | 2019-10-18 | 重庆大学 | A kind of continuous transformation of high temperature becomes iron ore performance measurement method under atmospheric condition |
| CN110411852A (en) * | 2019-07-30 | 2019-11-05 | 重庆大学 | The measuring method of coke property alternation in a kind of blast furnace |
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