CN103645114B - A kind of iron-bearing material gas-based reduction, slagging course experimental technique and device - Google Patents
A kind of iron-bearing material gas-based reduction, slagging course experimental technique and device Download PDFInfo
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- CN103645114B CN103645114B CN201310691946.2A CN201310691946A CN103645114B CN 103645114 B CN103645114 B CN 103645114B CN 201310691946 A CN201310691946 A CN 201310691946A CN 103645114 B CN103645114 B CN 103645114B
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Abstract
The present invention provides a kind of iron-bearing material gas-based reduction, slagging course experimental technique, is pressed into block as sample after being ground by iron-bearing material；Sample is put in the environment of simulation gas-based reduction, slagging, carry out gas-based reduction experiment；The weightlessness of sample and exhaust gas component data in real time record reduction process simultaneously；After gas-based reduction experiment terminates, sample carrying out high temperature slagging experiment, sample passes through shrend method to preserve its high temperature crystal structure after high-temperature fusion is dripped.The inventive method solves existing experimental technique and device cannot meet process detection and later stage sampling requirement, and use different equipment to study reproducibility and the Slag-formation characteristics of iron-bearing material, there is the problems such as inconvenient operation, it is the principle of continuous flow procedure according to blast furnace itself, closely related in conjunction with iron-bearing material gas-based reduction in cohesive zone, slagging course, creative propositions the inventive method is studied iron-bearing material and is reduced the affecting laws to slagging.Present invention also offers the experimental provision realizing said method.
Description
Technical field
The present invention relates to metallurgical engineering technical field, particularly relate to a kind of iron-bearing material gas-based reduction, slagging course experiment
Method, and a kind of device realizing the method.
Background technology
Measure the metallurgical performance of the iron-bearing material such as sintering deposit, pellet, lump ore be in metallurgical engineering experiment one important grind
Studying carefully content, it contributes to instructing ironmaking processes, and the burden structure that particularly blast furnace ironmaking process choosing is suitable is to reach to drop this increasing
The purpose of effect.Generally, the metallurgical performance of iron-containing charge mainly includes reproducibility, low-temperature reduction disintegration, loading also
Former softening-melted is dripping, and the experimental technique of each metallurgical performance detection and device the most independent.In contrast,
Blast furnace ironmaking process is actually a continuous print system, the most separate between different metallurgical performances, on the contrary by each other
The direct motion of the interphase interaction joint effect working of a furnace.Therefore, it is necessary to exploitation one is relatively more comprehensive, it is different to take into account iron-bearing material
The experimental technique of mutual relation and device between metallurgical performance.
In blast furnace ironmaking process, cohesive zone, as the key area " formed a connecting link " in stove, affects the secondary of Gas Flow
Distribution preliminarily forms with blast furnace slag, and the formation mechenism and the influence factor that study and grasp blast furnace melting with soft have for actual production
Important directive significance.For cohesive zone inside, iron-bearing material simultaneously participates in reduction and slagging is reacted, and relates to its reduction
Property, loading reduction soften the-melted metallurgical performance such as dripping, interaction relationship the most between the two is for resolving cohesive zone
Feature is most important.For existing detection means, the reproducibility of iron-bearing material mainly uses standard GB/T/T 13241-
Experimental technique and device described in 91 are tested, and loading reduction soften-melted dripping test do not has relevant domestic
Or international standard, what is more important lacks corresponding experimental technique and device at present with study tour above two metallurgical performance
Between interaction relationship.In addition, for the existing experimental technique for the detection of iron-bearing material metallurgical performance and device,
It is primarily present, and following some is not enough:Granularity required by sample is relatively big, solid particulate reagent layer internal diffusion and product
Nitride layer external diffusion becomes restricted link easily affects the measurement to sample metallurgical performance；Owing to single sample size is more, each
Grain is in different experimental situations, and the difference of caused metallurgical performance increases the difficulty of experiment later stage sampling work；High temperature
After experiment, sample cools down mainly by gas, and relatively low cooldown rate is unfavorable for preserving the slag structure under hot conditions；Single
Balance measurement requires that sample, hanging basket and gross mass wiry not can exceed that the range of balance, limits future to a certain extent
Further exploitation to the system of measurement.In sum, around studying iron-bearing material reduction in blast furnace melting with soft, slagging behavior
And interact, existing experimental technique and device cannot meet process detection and later stage sampling requirement.
Summary of the invention
For above-mentioned deficiency present in prior art, the purpose of the present invention essentially consists in a kind of experimental technique of offer to grind
Study carefully the interaction relationship of iron-bearing material reproducibility and slagability (i.e. soft heat-dripping), solve existing experimental technique and dress
Put and cannot meet process detection and later stage sampling requirement, and need the reproducibility using different equipment to study iron-bearing material
And Slag-formation characteristics, there is structure complexity, the problem of inconvenient operation.
Additionally, the present invention also provides for realizing iron-bearing material gas-based reduction, the device of slagging course experimental technique.
For achieving the above object, the present invention uses following technological means:
A kind of iron-bearing material gas-based reduction, slagging course experimental technique, it is characterised in that comprise the following steps:
1) it is pressed into block as sample after iron-bearing material being ground；
2) sample is put in the environment of simulation gas-based reduction, slagging, carry out gas-based reduction experiment；Real time record is also simultaneously
The weightlessness of sample and exhaust gas component data during former；Wherein, reducing gas composition, reaction temperature and response time carry out basis
Gas-based reduction requirement of experiment sets；
3) after gas-based reduction experiment terminates, sample being carried out slagging experiment, sample passes through water after high-temperature fusion is dripped
Method of quenching is to preserve its high temperature crystal structure；Wherein, gas componant, the heating rate of reaction temperature are wanted according to the experiment of high temperature slagging
Ask setting.
The gas componant that described step 3) sets depends on experimental program, (includes but not limited to if being set to inert atmosphere
N2, He), then the static reduction degree of the study tour sample action rule to its slagability；If be set to reducing atmosphere (include but
It is not limited to CO, H2), then the dynamic reduction degree of the study tour sample action rule to its slagability.
Described step 2) and 3) reaction temperature that sets each depends on experimental program, the gas-based reduction for iron-bearing material is anti-
Should, its reaction temperature is generally set to 800 ~ 1100 DEG C；And the high temperature slagging for iron-bearing material is reacted, its temperature is normally set up
At 1200 ~ 1500 DEG C.
Further, the present invention also provide for a kind of realize the iron-bearing material gas-based reduction of said method, slagging course experiment dress
Put, it is characterised in that include air supply system, reacting furnace and heating system thereof, Weighing system and sample collection tank；
Described air supply system includes CO, CO2、H2With multiple gas cylinders of noble gas, also include being connected with each gas cylinder respectively
Bottle valve and spinner flowmeter；The escape pipe of described gas cylinder is connected with main pipeline gas circuit and is provided with air valve and spinner flowmeter, does
Dry bottle, damping device and U-shaped differential manometer；
Described reacting furnace and heating system thereof include heating element heater and the upper furnace body controlling thermocouple thereof and lower furnace body；Upper stove
Being provided with reaction tube in the middle part of body, it is suitable for reading and seal lid, side end opening and seal lid and positive end opening and seal lid that reaction tube is provided with reaction tube；
Described sealing suitable for reading covers and is provided with nickel chromium triangle tinsel, and nickel chromium triangle lower end wiry is provided with the nickel chromium triangle hanging basket for placing sample,
Nickel chromium triangle upper end wiry is connected with meausring apparatus；Described side end opening and sealing lid are connected with main pipeline gas circuit, in this gas circuit also
It is provided with reaction tube intake valve；What described positive end opening and sealing were covered is arranged right below sample collection tank；The top of reaction tube also sets
Respond pipe outlet pipe and air outlet valve；The gas analyser for measuring tail gas and tail gas it is additionally provided with on reaction tube outlet pipe
Burner and combustion box；
Described Weighing system includes one-level sky gentle secondary electrons balance；Described one-level balance one end connects above-mentioned mounting and hangs
The nickel chromium triangle tinsel of basket and sample, the other end puts into the counterweight balanced therewith, the secondary electrons balance of counterweight end connection simultaneously；
Straight-through tail gas valve it is additionally provided with between the inlet, outlet pipeline of reacting furnace.
Further, described damping device includes pre-wetting bottle, main humidification bottle and additional wet bottle；Described main humidification bottle and additional
Wet bottle is placed in water-bath tank and is heated by resistive heater；Water-bath tank is provided with electronic thermometer.
Compared to existing technology, there is advantages that
1, the present invention solves existing experimental technique and device cannot meet process detection and later stage sampling requirement, and adopts
Study reproducibility and the Slag-formation characteristics of iron-bearing material with different equipment, there is the problems such as inconvenient operation, according to blast furnace originally
Body is the principle of continuous flow procedure, closely related in conjunction with iron-bearing material gas-based reduction, slagging course in cohesive zone, creative
Proposition the inventive method study the iron-bearing material reduction affecting laws to slagging.
2, the inventive method successively can detect reproducibility and the slagability of iron-bearing material in an experimentation successively,
Contribute to studying the former interactively to the latter, solve existing method and cannot directly set up two kinds of different metallurgical performance catch cropping
By the problem of relation.And humidify, by first dehumidification water-bath again, the steam that quantitatively makes up water in mixed gas, contribute to by controlling
Hydrogen and steam ratio regulate reduction potential height, solve existing method and cannot reduce when using hydrogen as reducing gas
The problem of its reduction potential.
3, after the inventive method is tested for high temperature slagging, sample directly uses the method for shrend to preserve sample, can be maximum
The high temperature crystal structure of the reserve sample of degree, contribute to further by X-ray diffractometer, that scanning electron microscope studies iron content is former
Expect by reduction to the transformation behavior of slagging, for resolving the thinking that blast furnace melting with soft formation mechenism provides new.
4, according to the thinking of the inventive method, low-temperature reduction, the device of high temperature slagging are designed.Reacting furnace and heating system thereof
It is designed with including heating element heater and controlling upper furnace body and lower furnace body composition, separate reaction zones and the gas preheating zone of thermocouple
Temperature control, also for research gas-solid countercurrent reaction during, mixed gas temperature and hysteresis are anti-to solid ferruginous raw material
Behavior is answered to provide new approach.
5, bottom mixed gas entrance and sample outlet use design from the bottom to top, it is achieved react Experimental reduction and mixed
Close the independent temperature control of gas preheating, the space that mixed gas is fully warmed-up can be met again.Use " h " shape corundum reaction tube the most permissible
Ensure that mixed gas is carried out reduction reaction by reacting tube side end opening after aluminium sesquioxide layers of balls preheats with sample, realize again reaction
Rear sample is fallen into equipped with realizing quickly cooling in the sample collection tank of water by the positive end opening of reaction tube.
6, Weighing system uses double skies flat structure, uses double skies flat structure of one-level sky gentle secondary electrons balance to come in real time
The weightless change of record experimentation sample, by change counterbalance mass and can arbitrarily balance coupling sample mass and without being subject to
The restriction of balance range, contributes to expanding the scope of application of apparatus of the present invention sample.
7, iron-bearing material gas-based reduction of the present invention, slagging course experimental provision mainly include air supply system, reacting furnace and
Heating system, Weighing system and sample collection tank, its reasonable in design, be skillfully constructed, and has simple in construction, convenient and practical
Feature.
Accompanying drawing explanation
Fig. 1 is the structural representation of iron-bearing material gas-based reduction slagging course experimental provision of the present invention.
In figure, 1-gas cylinder, 2-bottle valve and spinner flowmeter, 3-1-main pipeline air valve and spinner flowmeter, 3-2-
Reaction tube intake valve, 3-3-lead directly to exhaust valve, 3-4-reaction tube air outlet valve, 4-containing anhydrous CaCl2Drying bottle, 5-pre-wet
Bottle, 6-main humidification bottle, the additional wet bottle of 7-, 8-resistive heater, 9-water-bath tank, 10-electronic thermometer, 11-U type pressure reduction
Meter, 12-secondary electrons balance, 13-one-level balance, 14-" h " shape corundum reaction tube, 15-reaction tube are suitable for reading and sealing is covered,
16-sample and nickel chromium triangle hanging basket and connection nickel chromium triangle tinsel, 17-reacting furnace body of heater and heating element heater, 18-are according to reaction temperature
Choose K/R type thermocouple, 19-chooses K/R type thermocouple, 20-preheating furnace body of heater and heating unit according to reacting furnace heating-up temperature
Part, 21-aluminium sesquioxide layers of balls, 22-1-reaction tube side end opening and seal lid, the positive end opening of 22-2-reaction tube and seal lid,
23-according to preheating furnace heating-up temperature choose K/R type thermocouple, 24-aqueous specimen collect tank, 25-gas analyser,
26-tail gas burner and combustion box.
Detailed description of the invention
With embodiment, technical scheme is described in further detail below in conjunction with the accompanying drawings.
A kind of iron-bearing material gas-based reduction, slagging course experimental technique, comprise the steps:
1) iron-bearing material is milled to below 200 mesh, and to be pressed into basal diameter under 20 MPa pressure be 15 mm, thick
Degree is that the cylinder block of 5 mm is as sample；
2) sample is put in the environment of gas-based reduction, slagging, carry out gas-based reduction experiment；Real time record was reduced simultaneously
The weightlessness of sample and exhaust gas component data in journey；Wherein, reducing gas composition, reaction temperature and response time are carried out according to gas base
Reduction experiment requires to set；
3) by the sample after gas-based reduction, sample being carried out slagging experiment, sample passes through shrend after high-temperature fusion is dripped
Method is to preserve its high temperature crystal structure；Wherein, gas componant, reaction temperature and heating rate are according to high temperature slagging requirement of experiment
Set.
Realize the iron-bearing material gas-based reduction of said method, slagging course experimental provision, including air supply system, reacting furnace and
Its heating system, Weighing system；Described air supply system includes CO, CO2、H2With multiple gas cylinders 1 of noble gas, also include respectively
The bottle valve being connected with each gas cylinder 1 and spinner flowmeter 2；The escape pipe of described gas cylinder 1 is connected with main pipeline gas circuit and is provided with gas
Valve and spinner flowmeter 3-1, drying bottle 4, damping device and U-shaped differential manometer 11.
Described reacting furnace and heating system thereof include heating element heater 17 and the upper furnace body controlling thermocouple 19 thereof and include pre-
Heating element heater 20 and control thermocouple 23 lower furnace body thereof；Being provided with reaction tube 14 in the middle part of upper furnace body, reaction tube 14 is provided with on reaction tube
Mouth and sealing lid 15, side end opening and sealing lid 22-1 and just end opening and sealing cover 22-2；Described sealing lid 15 suitable for reading is provided with
Nickel chromium triangle tinsel 16, the lower end of nickel chromium triangle tinsel 16 is provided with the nickel chromium triangle hanging basket for placing sample, the upper end of nickel chromium triangle tinsel 16
It is connected with meausring apparatus；Described side end opening and sealing lid 22-1 are connected with main pipeline gas circuit, this gas circuit is additionally provided with reaction tube and enters
Air valve 3-2；Described positive end opening and seal lid 22-2 be arranged right below sample collection tank 24；The top of reaction tube 14 is additionally provided with
Reaction tube outlet pipe and air outlet valve 3-4；The gas analyser 25 for measuring tail gas it is additionally provided with on reaction tube 14 outlet pipe
With tail gas burner and combustion box 26；Straight-through tail gas valve 3-3 it is additionally provided with between the inlet, outlet pipeline of reacting furnace.
Described Weighing system includes one-level balance 13 and secondary electrons balance 12；Described one-level balance 13 one end connects above-mentioned
Mounting hanging basket and the nickel chromium triangle tinsel 16 of sample, the other end puts into the counterweight balanced therewith；Upper end connects secondary electrons sky simultaneously
Flat 12；The weightless change of real time record experimentation sample is carried out with double skies flat structure of one-level balance 13 and secondary electrons balance 12
Change.
Described damping device includes pre-wetting bottle 5, main humidification bottle 6 and additional wet bottle 7 and electronic thermometer 10；Described master adds
Wet 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 additionally provided with three
Al 2 O layers of balls 21.
The present invention uses " h " shape corundum reaction tube 14 both to can ensure that mixed gas was by reacting tube side end opening 22-1 through three oxygen
Carrying out reduction reaction with sample after changing two aluminum layers of balls 21 preheatings, after realizing reaction again, sample is fallen into by reaction tube positive end opening 22-2 and contains
Water sample is collected and is realized quickly cooling in tank 24.
Use described iron-bearing material gas-based reduction, slagging course experimental provision to carry out the method tested, comprise the following steps:
1) iron-bearing material is milled to below 200 mesh (less than 0.074 mm), and is pressed into bottom surface under 20 MPa pressure
A diameter of 15 mm, thickness is the cylinder block (hereinafter referred to as sample) of 5 mm；
2) sample is placed in nickel chromium triangle hanging basket, and is suspended on the middle part of reaction tube by nickel chromium triangle tinsel, nickel chromium triangle tinsel
Upper end connects one end of one-level balance, and this balance other end is placed identical with sample, hanging basket and connection tinsel gross mass
Counterweight, upper end connects secondary electrons balance simultaneously；
3) open the air inlet of argon gas cylinder and valve of giving vent to anger, after the emptying of question response inner air tube, close reaction tube escape pipe
Road and air outlet valve, open straight-through tail gas valve simultaneously, obtains the gas flow set, gas drying by regulation spinner flowmeter
After carry out water-bath humidification, after being humidified by mensuration, the gross pressure of gas determines the heating-up temperature of water-bath tank, to ensure gaseous mixture
In body, steam reaches the proportioning set；
4) open the heating element heater of reacting furnace and heating system thereof simultaneously and preheat the power supply of element, upper lower furnace body is entered
Row heating；After reduction reaction temperature and the gas preheating temperature that upper and lower two stoves respectively reach setting, according to setting proportional arrangement
Mixed gas, opens reaction tube air inlet and valve of giving vent to anger simultaneously closes off straight-through tail gas valve；
5), when iron-bearing material sample gas-based reduction is carried out, specimen is directly read by secondary electrons balance the most weightless
Data, after extracting partial reduction, tail gas is through gas analyser the real time measure compositional data simultaneously, and remaining tail gas enters burner combustion
Burn.
After reaching to set the response time, close each mixed gas gas cylinder air valve and open argon gas cylinder air valve simultaneously, open anti-
Should pipe top cover labyrinth and positive lower sealing cover, close reacting furnace and preheating furnace power supply, connection tinsel removed from one-level balance,
After reaction, sample falls into underface tank according to action of gravity, special with the reduction under research sample different phase by quickly cooling
Levy.
After reaching to set the response time, close each mixed gas gas cylinder air valve and open argon gas cylinder air valve simultaneously, open anti-
Positive lower sealing cover should be managed, close anti-preheating furnace power supply, continue to raise instead according to the heating rate set by current reaction temperature
Answering furnace temperature, sample progressively slagging after reaction, tank immediately below entrance after soft melting dropping, by quickly cooling to study examination
The slagging feature of sample difference reduction phase product.
Embodiment 1: a kind of iron-bearing material gas-based reduction, slagging course experimental technique, comprises the following steps:
1) take iron sesquioxide pure reagent (purity be more than 99%) 100 g, be milled to below 200 mesh, then take out wherein 5
G is placed in mould, and being pressed into basal diameter under 20 MPa pressure is 15 mm, and thickness is the cylinder block of 5 mm；
2) being placed in by sample in the hanging basket that molybdenum filament makes, and be suspended in the middle part of reacting furnace by metal molybdenum filament, top connects
One-level balance, this balance other end is put into 30 g counterweights (gross weight of hanging basket and metal molybdenum filament is 25 g), and is connected to two grades
On electronic balance, cover reaction tube top cover labyrinth and two lower sealing cover；
3) open nitrogen valve, the air in emptying reaction tube, open reacting furnace and preheating furnace power supply, by two stove mesh simultaneously
Mark temperature is disposed as 1000 DEG C；
4) after 1000 DEG C to be achieved, opening carbon monoxide valve, regulation nitrogen, the spinner of carbon monoxide are calculated as 2 L/
min；
5) sample starts reduction, and secondary electrons balance shows weight loss in real time and reads in computer, calculates real-time the going back of sample
Former degree；
6) after sample reduction degree reaches 50%, close carbon monoxide valve, reacting furnace target temperature is set to simultaneously
1200 DEG C, heating rate is 10 DEG C/min；
7) after 1200 DEG C to be achieved, further constant temperature 60 min；
8) after 60 min, aqueous specimen is collected tank and is placed on below reaction tube, open simultaneously reaction tube just under close
Capping, removes the metal molybdenum filament hanging with sample from one-level balance, allows sample fall under gravity into sample collection tank；
9) fast cooling samples acquired in, analyzes iron sesquioxide at 50% reduction degree by scanning electron microscope and X diffractometer
Slagging feature under level (topographic profile, thing are distributed mutually, component distributing etc.).
On the basis of above-mentioned experiment, by changing sample reduction degree level (60%, 70%, 80%, 90%) in step 6), with
Investigate the iron-bearing material static reduction degree in the different impacts on its slagability of the reduction degree level, i.e. iron-bearing material to its slagability
Action rule.
In above-mentioned iron-bearing material gas-based reduction slagging course experimental technique, described step 3) sets the selection of gas flow
Depend on that under experiment condition, in corundum reaction tube, the further of gas flow rate break through gas boundary region, i.e. gas flow rate increases no longer
Change the reaction rate of sample.Wherein, steam sets the selection of proportioning and depends on experimental program, by warm in controlling water-bath tank
Degree, measures the gross pressure of mixed gas before and after humidifying and calculates the dividing potential drop of steam, to investigate its proportioning in mixed gas
Whether meet the requirement of experimental program.
Embodiment 2: use said apparatus to carry out iron-bearing material gas-based reduction, slagging course experimental technique, including following step
Rapid:
1) ~ 5) with embodiment 1；
6) after sample reduction degree reaches 50%, reacting furnace target temperature being set to 1200 DEG C, heating rate is 10 DEG C/
min；
7) after 1200 DEG C to be achieved, further constant temperature 60 min；
8) after 60 min, close carbon monoxide valve, the final reduction degree level of record sample, aqueous specimen is collected
Tank is placed on below reaction tube, opens the positive lower sealing cover of reaction tube simultaneously, removes the metal hanging with sample from one-level balance
Molybdenum filament, allows sample fall under gravity into sample collection tank；
9) fast cooling samples acquired in, analyzes iron sesquioxide by scanning electron microscope and X diffractometer and is reaching 50% also
After former degree level, slagging feature under Carbon monoxide reduction atmosphere (topographic profile, thing are distributed mutually, component distributing etc.), and lead to
Crossing result obtained with embodiment 1 to contrast, the effect of its slagability is advised by the dynamic reduction degree of high spot reviews iron-bearing material
Rule.
Embodiment 3: use said apparatus to carry out iron-bearing material gas-based reduction, slagging course experimental technique, including following step
Rapid:
1) take Iron Ore Powder (Australia ore deposit, Brazil ore deposit or domestic fine ore) 100 g, be milled to below 200 mesh, then take
Going out wherein 5 g to be placed in mould, being pressed into basal diameter under 20 MPa pressure is 15 mm, and thickness is the cylinder block of 5 mm；
2) being placed in by sample in the hanging basket that molybdenum filament makes, and be suspended in the middle part of reacting furnace by metal molybdenum filament, top connects
One-level balance, this balance other end is put into 30 g counterweights (gross weight of hanging basket and metal molybdenum filament is 25 g), and is connected to two grades
On electronic balance, cover reaction tube top cover labyrinth and two lower sealing cover；
3) open nitrogen valve, the air in emptying reaction tube, close reaction tube air inlet and open directly with valve of giving vent to anger simultaneously
Logical tail gas valve, is calculated as 4 L/min by the spinner of regulation nitrogen, first carries out water-bath humidification after drying, and regulation water-bath adds
The temperature of heat is 46 DEG C, and after measuring humidification, the gross pressure of gas is about 111 kPa, and current atmospheric pressure is about 101 kPa, thus counts
Calculate the proportioning of steam in mixed gas and be about 9 %(volume fractions), open the power supply of reacting furnace and preheating furnace, by two stoves simultaneously
Target temperature is disposed as 1200 DEG C；
4) after 1200 DEG C to be achieved, opening hydrogen valve, regulation nitrogen, the spinner of hydrogen are calculated as 2 L/min, open
Reaction tube air inlet and valve of giving vent to anger simultaneously close off straight-through tail gas valve, and now in gaseous mixture, hydrogen and steam ratio are 5.56；
5) sample starts reduction, and secondary electrons balance shows weight loss in real time and reads in computer, calculates real-time the going back of sample
Former degree；
6) after sample reduction degree reaches 50%, close hydrogen valve and stop heating in water bath, simultaneously by reacting furnace target temperature
Degree is set to 1400 DEG C, and heating rate is 10 DEG C/min；
7) after 1400 DEG C to be achieved, further constant temperature 60 min；
8) after 60 min, aqueous specimen is collected tank and is placed on below reaction tube, open simultaneously reaction tube just under close
Capping, removes the metal molybdenum filament hanging with sample from one-level balance, allows sample fall under gravity into sample collection tank；
9) fast cooling samples acquired in, analyzes Iron Ore Powder in 50% reduction degree level by scanning electron microscope and X diffractometer
Under slagging feature (topographic profile, thing are distributed mutually, component distributing etc.).
On the basis of above-mentioned experiment, by changing sample reduction degree level (60%, 70%, 80%, 90%) in step 6), with
Investigate the iron-bearing material static reduction degree in the different impacts on its slagability of the reduction degree level, i.e. iron-bearing material to its slagability
Action rule；Contrasted by result obtained with embodiment 1, it is also possible to investigate under identical static reduction degree level,
The reducing agent impact on slagability.
Embodiment 4: use said apparatus to carry out iron-bearing material gas-based reduction, slagging course experimental technique, including following step
Rapid:
1) ~ 5) with embodiment 3；
6) after sample reduction degree reaches 50%, reacting furnace target temperature being set to 1400 DEG C, heating rate is 10 DEG C/
min；
7) after 1400 DEG C to be achieved, further constant temperature 60 min；
8) after 60 min, close hydrogen valve and stop heating in water bath, aqueous specimen being collected tank and is placed on reaction tube
Lower section, opens the positive lower sealing cover of reaction tube simultaneously, removes the metal molybdenum filament hanging with sample from one-level balance, allows sample at weight
Power effect falls into sample collection tank；
9) fast cooling samples acquired in, analyzes Iron Ore Powder in 50% reduction degree level by scanning electron microscope and X diffractometer
After, slagging feature under hydrogen/aqueous vapour reducing atmosphere (topographic profile, thing are distributed mutually, component distributing etc.), and by with reality
Execute the obtained result of example 3 to contrast, the dynamic reduction degree of the high spot reviews iron-bearing material action rule to its slagability.
Finally illustrating, above example is only in order to illustrate technical scheme and unrestricted, although with reference to relatively
The present invention has been described in detail by good embodiment, it will be understood by those within the art that, can be to the skill of the present invention
Art scheme is modified or equivalent, and without deviating from objective and the scope of technical solution of the present invention, it all should be contained at this
In the middle of the right of invention.
Claims (5)
1. an iron-bearing material gas-based reduction, slagging course experimental technique, it is characterised in that comprise the following steps:
1) iron-bearing material being milled to below 200 mesh, and to be pressed into basal diameter under 20 MPa pressure be 15 mm, thickness is 5
The cylinder block of mm is as sample；
2) sample is put in the environment of gas-based reduction, slagging, carry out gas-based reduction experiment；Simultaneously in real time record reduction process
The weightlessness of sample and exhaust gas component data；Wherein, reducing gas composition, reaction temperature and response time are carried out according to gas-based reduction
Requirement of experiment sets；
3) sample after gas-based reduction being carried out slagging experiment, sample passes through shrend method to preserve it after high-temperature fusion is dripped
High temperature crystal structure；Wherein, gas componant, reaction temperature and heating rate set according to high temperature slagging requirement of experiment；
If being set to inert atmosphere, include but not limited to N2, He, then the static reduction degree of study tour sample is to its slagability
Action rule；If being set to reducing atmosphere, include but not limited to CO, H2, then it is become by the dynamic reduction degree of study tour sample
The action rule of slag；
Described step 2) and 3) reaction temperature that sets each depends on experimental program, the gas-based reduction for iron-bearing material reacts,
Its reaction temperature is generally set to 800 ~ 1100 DEG C；And the high temperature slagging for iron-bearing material is reacted, its temperature is generally set to
1200~1500℃；
Described step 2) and 3) heating rate of response time of setting and setting each depends on experimental program, for the response time
For, it typically is 30 ~ 180 min, for heating rate, it typically is 3 ~ 20 DEG C/min.
2. realizing the iron-bearing material gas-based reduction of method described in claim 1, a slagging course experimental provision, its feature exists
In, including air supply system, reacting furnace and heating system thereof, Weighing system and sample collection tank (24)；
Described air supply system includes CO, CO2、H2With multiple gas cylinders (1) of noble gas, also include being connected with each gas cylinder (1) respectively
Bottle valve and the first rotor effusion meter (2)；The escape pipe of described gas cylinder (1) is connected with main pipeline gas circuit and is provided with air valve and
Two spinner flowmeters (3-1), drying bottle (4), damping device and U-shaped differential manometer (11)；
Described reacting furnace and heating system thereof include heating element heater (17) and the upper furnace body controlling the first thermocouple (19) thereof and bag
Include and preheat element (20) and control the lower furnace body of the second thermocouple (23)；Reaction tube (14) it is provided with, reaction in the middle part of upper furnace body
Pipe (14) be provided with reaction tube suitable for reading and seal lid (15), side end opening and seal lid (22-1) and positive end opening and seal cover
(22-2)；Described suitable for reading itself and seal lid (15) and be provided with nickel chromium triangle tinsel (16), the lower end of nickel chromium triangle tinsel (16) is provided with
For placing the nickel chromium triangle hanging basket of sample, the upper end of nickel chromium triangle tinsel (16) is connected with Weighing system；Described side end opening and sealing lid
(22-1) it is connected with main pipeline gas circuit, this gas circuit is additionally provided with air inlet pipeline and intake valve (3-2)；Described positive end opening and sealing thereof
Cover (22-2) is arranged right below sample collection tank (24)；The top of reaction tube (14) is additionally provided with reaction tube outlet pipe and goes out
Air valve (3-4)；Be additionally provided with on reaction tube (14) outlet pipe the gas analyser (25) for measuring tail gas and tail gas burner and
Combustion box (26)；
Described Weighing system includes one-level balance (13) and secondary electrons balance (12)；On described one-level balance (13) one end connects
Stating mounting hanging basket and the nickel chromium triangle tinsel (16) of sample, the other end puts into the counterweight balanced therewith；Secondary electrons balance (12) is straight
Connect one-level sky placing flat counterweight end in succession；
Straight-through tail gas valve (3-3) it is additionally provided with between the inlet, outlet pipeline of reacting furnace.
Iron-bearing material gas-based reduction, slagging course experimental provision the most according to claim 2, it is characterised in that described humidification
Device includes 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) is heated by resistive heater (8)；Water-bath tank (9) is provided with electronic thermometer (10).
Iron-bearing material gas-based reduction, slagging course experimental provision the most according to claim 2, it is characterised in that described first
The K/R type thermocouple according to reaction temperature is used with the second thermocouple (19,23).
Iron-bearing material gas-based reduction, slagging course experimental provision the most according to claim 2, it is characterised in that described reaction
The bottom of pipe (14) is additionally provided with aluminium sesquioxide layers of balls (21).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105136601A (en) * | 2015-08-14 | 2015-12-09 | 中南大学 | High-temperature thermal field and complex atmosphere environment static coupling device |
| 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 |
| 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 |
| CN109991125B (en) * | 2019-05-16 | 2022-09-23 | 重庆大学 | Method and equipment for testing variable-pressure type reflow dripping performance |
| CN110346538B (en) * | 2019-07-12 | 2021-03-09 | 重庆大学 | Method for measuring performance of iron ore under high-temperature continuous variable-pressure and variable-atmosphere conditions |
| CN110411852B (en) * | 2019-07-30 | 2021-09-07 | 重庆大学 | Method for measuring performance gradient of coke in blast furnace |
| CN110849931A (en) * | 2019-12-05 | 2020-02-28 | 中冶华天工程技术有限公司 | Visual determination device and determination method for iron ore softening and melting performance |
| CN112941262B (en) * | 2021-01-29 | 2022-07-29 | 钢铁研究总院 | Gas-based reduction simulation device and gas-based reduction simulation method |
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| EP0921200A1 (en) * | 1997-12-03 | 1999-06-09 | Sidmar N.V. | Process and apparatus for reducing iron oxides and melting iron |
| CN102212635A (en) * | 2011-05-20 | 2011-10-12 | 唐山奥特斯科技有限公司 | Process for producing granulated iron by directly reducing low-grade complex difficultly-processed ore |
| CN102768159A (en) * | 2012-07-17 | 2012-11-07 | 北京科技大学 | Device and method for detecting reducibility of iron ore |
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| JP5330636B2 (en) * | 2006-03-10 | 2013-10-30 | 株式会社リコー | Compound reducing agent |
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|---|---|---|---|---|
| EP0921200A1 (en) * | 1997-12-03 | 1999-06-09 | Sidmar N.V. | Process and apparatus for reducing iron oxides and melting iron |
| CN102212635A (en) * | 2011-05-20 | 2011-10-12 | 唐山奥特斯科技有限公司 | Process for producing granulated iron by directly reducing low-grade complex difficultly-processed ore |
| CN102768159A (en) * | 2012-07-17 | 2012-11-07 | 北京科技大学 | Device and method for detecting reducibility of iron ore |
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