CN102914616B - Blast furnace slag desulfuration capability detection and evaluation method - Google Patents
Blast furnace slag desulfuration capability detection and evaluation method Download PDFInfo
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Abstract
The invention provides a blast furnace slag desulfuration capability detection and evaluation method which includes the steps of slag sample desulfuration and iron sample preparation, slag-iron sample reaction and furnace slag desulfuration capability evaluation. The ratio of the absolute sulfur content of furnace slag to the absolute sulfur content in molten iron is used for representing the distribution coefficient Ls of sulfur in slag iron, Ls=(S)*Z/1000*[S], in the formula, (S) refers to the percentage % of sulfur in the furnace slag, Z refers to the blast furnace slag ratio kg/t, [S] refers to the percentage % of sulfur in pig iron, and the larger the Ls is, the higher the desulfuration capability is. The blast furnace slag desulfuration capability evaluation is more accordant with actual production situations, and the method is of great instructive significance to blast furnace improvement and slagging system optimization, stable and smooth blast furnace production guarantee and fuel consumption reduction.
Description
Technical field
The invention belongs to metallurgical materialization technical field of measurement and test, be specifically related to a kind of blast furnace slag desulphurizing ability determination and evaluation method.
Background technology
In blast furnace process, the key reducing pig iron sulfur content improves the desulphurizing ability of slag.Under certain crude fuel and smelting condition, the Main way and the approach that reduce pig iron sulfur content improve the distribution ratio of sulphur between slag, iron (Ls), and in therefore producing, conventional Ls evaluates the desulphurizing ability of slag.Wherein improve furnace temperature and improve slag chemistry composition and can improve desulphurizing ability.Under the metastable condition of temperature of the furnace hearth, slag desulfurization capacity is mainly by slag chemistry composition influence.Therefore, analog blast furnace slag iron desulphurization reaction condition, determination and evaluation blast furnace slag chemical composition are on the impact of slag desulfurization capacity, and improve blast furnace operating person and optimize slagging regime, stable smooth operation of furnace has important directive significance.
The slag desulfurization capacity of test in laboratory and evaluation different chemical composition, usually preparation slag specimen on-the-spot blast furnace slag and chemically pure reagent (CaO, SiO
2, Al
2o
3, MgO) allocate, the preparation of high-sulfur iron sample is directly supposed to enter the pig iron into stove sulphur analysis 95%, with FeS reagent and the on-the-spot pig iron carry out preparing [Wang Zhumin, Lv Qing etc. the experimental study of Handan Iron and Steel Co blast furnace slag desulphurizing ability. steel research, 2008(3)].A certain amount of on-the-spot slag is allocated into due to during preparation slag specimen, this part slag is derived from blast furnace itself also containing a certain amount of sulphur, therefore, prior art all enters the pig iron according to enter stove sulphur analysis 95% and carries out the preparation of high-sulfur iron sample, and obvious and actual conditions exist comparatively big error.
Slag iron desulphurization reaction, prior art adopts upper and lower two-layer graphite crucible as slag iron reactor usually, high-sulfur iron sample is held in upper crucible, have an aperture in the middle of bottom, before iron sample does not melt, clog aperture with graphite rod, after the fusing of iron sample, remove graphite rod, molten iron to be drained to hold in the lower crucible of slag [prime minister Song, Zhou Guofan etc. high Al
2o
3blast-furnace slag desulfurization performance is studied. Henan Metallurgical, 2007(6)].This device can in analog blast furnace slag to the state of desulfurizing iron and condition, but only have one to leak iron aperture in the middle of bottom Sheng iron crucible, lower crucible is dropped onto after the fusing of iron sample, only come in contact reaction with the slag blanket in the middle of crucible, and the submarginal slag blanket of surrounding is difficult to the molten iron touching drippage, cause slag iron desulphurization reaction abundant not.And the existence of plug-hole graphite rod is also made troubles to experimental implementation under high temperature.A kind of two crucible experimental apparatus [CN 201110079670.3] of high temperature experiment solve the erosion problem of reactant to crucible, also the macroscopic property simultaneously studying slag and molten metal is possessed, but this design slag crucible is positioned at molten metal top can not drip the state of passing through slag blanket by analog blast furnace molten iron, and using Sheng slag crucible to use metal molybdenum manufacture, experimental cost is higher.
At measurement blast furnace desulphurizing ability, i.e. the partition factor Ls of sulphur in slag, iron, prior art represents with the ratio of slag (S) content and molten iron [S] content merely, can not reflect the real size of slag desulfurization capacity when the quantity of slag changes.Evaluate blast furnace slag comprehensive alkali, desulphurizing ability method [CN201110192916.8] with the size of potassium sulfide capability value to evaluate the comprehensive alkali of blast furnace slag, a size for desulphurizing ability, obtain meet simultaneously desulfurization, row alkali suitable thermodynamic condition.But this experimental implementation is comparatively complicated, and experimental period is long, and K steam and CO gas can be produced in experiment, can constitute a threat to the personal safety of test operation person.Utilize gas-slag-melt equilibration technology to measure the method [CN 200710062317.8] of five yuan of slag system sulfur capacities, Fe can be contained by Accurate Determining
tthe sulfur capacity of O slag, can be CaO-SiO
2-Al
2o
3-MgO-Fe
to five yuan of slag systems provide reliable thermodynamic data, but experimentation needs to use CO, SO
2gas is all a major challenge to the sealing of high temperature furnace and operator's technology.
In a word, prior art is to the test and repair of blast furnace slag desulphurizing ability, and existence preparation high-sulfur iron sample error is large, simulation slag iron desulphurization reaction is insufficient, and experimental implementation requires high and detection time is long, and harmful gas has the shortcomings such as potential hazard to operator's health.
Prior art characterizes slag desulfurization capacity size based on adopting the mass percentage ratio of sulphur in slag iron under quantity of slag permanence condition.But in blast furnace actual production, ton scum amount changes with working of a furnace fluctuation usually, and obvious prior art can not truly reflect slag desulfurization capacity size.Not enough for prior art, the present invention adopts the ratio of absolute sulfur content in the absolute sulfur content of slag and molten iron to represent the partition factor Ls of sulphur in slag iron, can solve because of the error that cause of quantity of slag variation to desulphurizing ability, scientific and precise more in the evaluation of practical application to desulphurizing ability.
, in formula, (S) is the percentage composition of sulphur in slag, %; Z is blast furnace slag ratio, kg/t; The percentage composition of sulphur in [S] pig iron, %, Ls are larger, and desulphurizing ability is stronger.
The method of above-mentioned detecting and assessing blast furnace slag desulphurizing ability, the preparation of described high-sulfur iron sample or choose to consider desulfurization before the sulfur content brought of slag specimen, more realistic.
The method of above-mentioned detecting and assessing blast furnace slag desulphurizing ability, described slag iron reactor, upper strata crucible bottom is evenly arranged 6 ~ 8 circular holes, and Circularhole diameter is 8 ~ 10mm.
The method of above-mentioned detecting and assessing blast furnace slag desulphurizing ability, described sulphur is partition factor L in slag iron
sthe ratio of definitely sulfur content in the absolute sulfur content of slag and molten iron is adopted to characterize.
Application the present invention carries out blast furnace slag desulphurizing ability detecting and assessing, in analog blast furnace, slag iron desulphurization reaction process is more true and reliable, evaluate blast furnace slag desulphurizing ability and more meet production actual conditions, improve instructing blast furnace and optimize slagging regime, ensure blast fumance stable smooth operation, reduce fuel consumption significant.In addition, adopting this method detection blast furnace slag desulphurizing ability to have experiment detects easy and simple to handle, to advantages such as operator's body harm are little.
Summary of the invention
The object of the present invention is to provide a kind of blast furnace slag desulphurizing ability determination and evaluation method, analog blast furnace slag iron desulphurization reaction process, determination and evaluation blast-furnace slag desulphurizing ability, improve to instruct blast furnace and optimize slagging regime, ensureing blast fumance stable smooth operation, reducing fuel consumption.
The present invention includes desulfurization slag specimen and iron sample preparation, slag iron sample reaction and slag desulfurization capacity evaluate three steps.
1 slag specimen and the preparation of iron sample:
With on-the-spot blast furnace slag average chemical constitution for benchmark, according to sample CaO, SiO
2, Al
2o
3with MgO mass percentage be 36% ~ 44%, 30% ~ 36%, 10% ~ 17% and 7% ~ 15% and slag iron take pure chemistry reagent (CaO, SiO respectively than 0.27 ~ 0.30
2, Al
2o
3, MgO) and on-the-spot blast furnace slag and to put into graphite crucible after fully mixing stand-by.
The choosing of high-sulfur iron sample will take into full account the sulfur content of slag specimen before desulfurization, is converted to test iron sample sulfur content with the 95% deduction slag specimen entering stove sulphur analysis after the sulfur content brought into again, then carries out weighing according to setting slag iron ratio and to prepare and to load graphite crucible stand-by.
2 slag iron reactions
Slag iron reactor adopts upper and lower two-layer graphite crucible, and for prior art slag iron can not fully contact reaction be not enough, the present invention contains bottom iron crucible and is provided with the identical circular hole of multiple diameter, and is evenly distributed in whole crucible bottom.The design of circular hole size should consider that can produce drippage effect after molten iron passes through considers that the surface tension of molten iron and circular hole causes molten iron to block circular hole again, experimentally verify, Circularhole diameter is 8 ~ 10mm, and the number in hole suitably can be arranged according to the size of crucible floorage.This device mainly can occur in when molten iron drips downwards through during cupola well slag blanket and the state of cupola well slag iron interface and condition the desulphurization reaction of molten iron by slag in analog blast furnace.During experiment, first Sheng slag crucible is placed in electric tube furnace and heats up, and start to pass into N from furnace bottom
2gas shielded, after slag specimen melts completely and is warming up to 1450 DEG C, stirs; splendid attire iron sample crucible is placed in electric furnace on slag crucible, treat that iron sample melts, molten iron drips through crucible bottom circular hole again; drip after finishing completely; in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction more than 25min, then takes out lower crucible; after cooling; get slag iron sample, chemically examine the sulfur content of slag iron sample respectively, and calculate sulphur content distribution coefficient Ls.
3 slag desulfurization capacity evaluations
Accompanying drawing explanation
Accompanying drawing 1 experimental provision schematic diagram.
In Fig. 1, each part numbers is as follows: 1. graphite crucible; 2. high-sulfur iron sample; 3. crucible bottom circular hole; 4. graphite crucible; 5. slag; 6. graphite protection tube; 7. alundum tube; 8. thermometric galvanic couple; 9. refractory brick pad.
Embodiment
Experimental provision schematic diagram of the present invention as shown in Figure 1; slag iron fusing reaction experiment carries out in U-shaped molybdenum disilicide electric tube furnace; reaction tube is high-purity corundum pipe 7; built-in graphite protection tube 6, plays insulation and the effect of protection alundum tube, in graphite protection tube 6; be respectively graphite crucible 1(up and down and hold high-sulfur iron sample 2; bottom has leaks iron circular hole 3) and graphite crucible 4(hold slag 5), be refractory brick pad bottom graphite crucible 4, play support crucible effect.On-the-spot blast furnace slag chemical composition is in table 1, and high-sulfur iron sample ingredient is in table 2.
On-the-spot certain blast-furnace slag chemical composition/% of table 1
| CaO | SiO 2 | MgO | Al 2O 3 | FeO | TiO 2 | MnO | S |
| 40.04 | 34.69 | 7.50 | 14.84 | 0.66 | 0.62 | 0.42 | 0.99 |
On-the-spot certain the blast furnace high-sulfur pig iron composition/% of table 2
| S | C | Si | Mn | P | Ti |
| 0.079 | 4.41 | 0.18 | 0.14 | 0.06 | 0.010 |
Embodiment 1
With blast furnace slag on-the-spot shown in table 1 for benchmark, according to slag iron than composition slag 30g shown in 0.30 preparation table 3, pure chemistry agent and on-the-spot slag are fully mixed rear loading graphite crucible 4.Take the sample of iron shown in table 2 100g according to slag iron than 0.30 and load graphite crucible 1, it is 3.0kg/t that certain blast furnace on-the-spot on average enters stove sulphur analysis, and after the sulfur content brought into by slag specimen before measuring and calculating deduction desulphurization reaction, this iron sample ingredient can meet simulated experiment requirement.
Table 3 embodiment 1 slag specimen composition/%
| CaO | SiO 2 | MgO | Al 2O 3 | FeO | TiO 2 | MnO | S |
| 41.49 | 33.35 | 7.50 | 14.84 | 0.63 | 0.60 | 0.40 | 0.95 |
First Sheng slag crucible is placed in electric furnace and heats up, and start to pass into N from furnace bottom
2gas shielded; after slag specimen melts completely and is warming up to 1450 DEG C; stir; again splendid attire iron sample crucible to be placed in electric furnace on slag crucible; treat that iron sample melts; molten iron drips through crucible bottom circular hole; slag blanket through lower crucible is deposited on bottom; drip completely after finishing, in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction 25min; then lower crucible is taken out; get slag iron sample after cooling and be separated slag iron, chemically examine its sulfur content respectively and calculate sulphur content distribution coefficient Ls, evaluating the power of blast furnace slag desulphurizing ability according to the size of Ls.Ls value is larger, and the desulphurizing ability of this slag specimen is stronger.Testing slag iron ratio in this embodiment is 0.30, i.e. Z=300kg/t, iron sample [S]=0.032% after chemical examination reaction, slag specimen (S)=1.08%, then: Ls=(S) * Z/ ([S] * 1000)=1.08%*300/ (0.032%*1000)=10.1.
Embodiment 2
With blast furnace slag on-the-spot shown in table 1 for benchmark, according to slag iron than composition slag 27g shown in 0.27 preparation table 4, pure chemistry agent and on-the-spot slag are fully mixed rear loading graphite crucible 4.Take the sample of iron shown in table 2 100g according to slag iron than 0.27 and load graphite crucible 1, it is 3.0kg/t that certain blast furnace on-the-spot on average enters stove sulphur analysis, and after the sulfur content brought into by slag specimen before measuring and calculating deduction desulphurization reaction, this iron sample ingredient can meet simulated experiment requirement.
Table 4 embodiment 2 slag specimen composition/%
| CaO | SiO 2 | MgO | Al 2O 3 | FeO | TiO 2 | MnO | S |
| 42.25 | 32.65 | 7.50 | 14.84 | 0.62 | 0.58 | 0.40 | 0.93 |
First Sheng slag crucible is placed in electric furnace and heats up, and start to pass into N from furnace bottom
2gas shielded; after slag specimen melts completely and is warming up to 1500 DEG C; stir; again splendid attire iron sample crucible to be placed in electric furnace on slag crucible; treat that iron sample melts; molten iron drips through crucible bottom circular hole; slag blanket through lower crucible is deposited on bottom; drip completely after finishing, in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction 26min; then lower crucible is taken out; get slag iron sample after cooling and be separated slag iron, chemically examine its sulfur content respectively and calculate sulphur content distribution coefficient Ls, evaluating the power of blast furnace slag desulphurizing ability according to the size of Ls.Ls value is larger, and the desulphurizing ability of this slag specimen is stronger.Testing slag iron ratio in this embodiment is 0.27, i.e. Z=270kg/t, iron sample [S]=0.014% after chemical examination reaction, slag specimen (S)=1.04%, then: Ls=(S) * Z/ ([S] * 1000)=1.04%*270/ (0.014%*1000)=20.1.
Embodiment 3
With blast furnace slag on-the-spot shown in table 1 for benchmark, according to slag iron than composition slag 29g shown in 0.29 preparation table 5, pure chemistry agent and on-the-spot slag are fully mixed rear loading graphite crucible 4.Take the sample of iron shown in table 2 100g according to slag iron than 0.29 and load graphite crucible 1, it is 3.0kg/t that certain blast furnace on-the-spot on average enters stove sulphur analysis, and after the sulfur content brought into by slag specimen before measuring and calculating deduction desulphurization reaction, this iron sample ingredient can meet simulated experiment requirement.
Table 5 embodiment 3 slag specimen composition/%
| CaO | SiO 2 | MgO | Al 2O 3 | FeO | TiO 2 | MnO | S |
| 44.12 | 36.76 | 8.10 | 10.00 | 0.23 | 0.25 | 0.10 | 0.62 |
First Sheng slag crucible is placed in electric furnace and heats up, and start to pass into N from furnace bottom
2gas shielded; after slag specimen melts completely and is warming up to 1460 DEG C; stir; again splendid attire iron sample crucible to be placed in electric furnace on slag crucible; treat that iron sample melts; molten iron drips through crucible bottom circular hole; slag blanket through lower crucible is deposited on bottom; drip completely after finishing, in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction 26min; then lower crucible is taken out; get slag iron sample after cooling and be separated slag iron, chemically examine its sulfur content respectively and calculate sulphur content distribution coefficient Ls, evaluating the power of blast furnace slag desulphurizing ability according to the size of Ls.Ls value is larger, and the desulphurizing ability of this slag specimen is stronger.Testing slag iron ratio in this embodiment is 0.29, i.e. Z=290kg/t, iron sample [S]=0.027% after chemical examination reaction, slag specimen (S)=0.75%, then: Ls=(S) * Z/ ([S] * 1000)=0.75%*290/ (0.027%*1000)=8.1.
Embodiment 4
With blast furnace slag on-the-spot shown in table 1 for benchmark, according to slag iron than composition slag 29g shown in 0.29 preparation table 6, pure chemistry agent and on-the-spot slag are fully mixed rear loading graphite crucible 4.Take the sample of iron shown in table 2 100g according to slag iron than 0.29 and load graphite crucible 1, it is 3.0kg/t that certain blast furnace on-the-spot on average enters stove sulphur analysis, and after the sulfur content brought into by slag specimen before measuring and calculating deduction desulphurization reaction, this iron sample ingredient can meet simulated experiment requirement.
Table 6 embodiment 4 slag specimen composition/%
| CaO | SiO 2 | MgO | Al 2O 3 | FeO | TiO 2 | MnO | S |
| 37.91 | 31.59 | 13.00 | 16.50 | 0.29 | 0.22 | 0.09 | 0.90 |
First Sheng slag crucible is placed in electric furnace and heats up, and start to pass into N from furnace bottom
2gas shielded; after slag specimen melts completely and is warming up to 1470 DEG C; stir; again splendid attire iron sample crucible to be placed in electric furnace on slag crucible; treat that iron sample melts; molten iron drips through crucible bottom circular hole; slag blanket through lower crucible is deposited on bottom; drip completely after finishing, in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction 28min; then lower crucible is taken out; get slag iron sample after cooling and be separated slag iron, chemically examine its sulfur content respectively and calculate sulphur content distribution coefficient Ls, evaluating the power of blast furnace slag desulphurizing ability according to the size of Ls.Ls value is larger, and the desulphurizing ability of this slag specimen is stronger.Testing slag iron ratio in this embodiment is 0.29, i.e. Z=290kg/t, iron sample [S]=0.028% after chemical examination reaction, slag specimen (S)=1.11%, then: Ls=(S) * Z/ ([S] * 1000)=1.11%*290/ (0.028%*1000)=11.5.
Embodiment 5
With blast furnace slag on-the-spot shown in table 1 for benchmark, according to slag iron than composition slag 28g shown in 0.28 preparation table 4, pure chemistry agent and on-the-spot slag are fully mixed rear loading graphite crucible 4.Take the sample of iron shown in table 2 100g according to slag iron than 0.28 and load graphite crucible 1, it is 3.0kg/t that certain blast furnace on-the-spot on average enters stove sulphur analysis, and after the sulfur content brought into by slag specimen before measuring and calculating deduction desulphurization reaction, this iron sample ingredient can meet simulated experiment requirement.
Table 7 embodiment 5 slag specimen composition/%
| CaO | SiO 2 | MgO | Al 2O 3 | FeO | TiO 2 | MnO | S |
| 36.83 | 30.7 | 15.00 | 16.50 | 0.28 | 0.21 | 0.08 | 0.87 |
First Sheng slag crucible is placed in electric furnace and heats up, and start to pass into N from furnace bottom
2gas shielded; after slag specimen melts completely and is warming up to 1480 DEG C; stir; again splendid attire iron sample crucible to be placed in electric furnace on slag crucible; treat that iron sample melts; molten iron drips through crucible bottom circular hole; slag blanket through lower crucible is deposited on bottom; drip completely after finishing, in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction 30min; then lower crucible is taken out; get slag iron sample after cooling and be separated slag iron, chemically examine its sulfur content respectively and calculate sulphur content distribution coefficient Ls, evaluating the power of blast furnace slag desulphurizing ability according to the size of Ls.Ls value is larger, and the desulphurizing ability of this slag specimen is stronger.Testing slag iron ratio in this embodiment is 0.28, i.e. Z=280kg/t, iron sample [S]=0.026% after chemical examination reaction, slag specimen (S)=1.09%, then: Ls=(S) * Z/ ([S] * 1000)=1.09%*280/ (0.026%*1000)=11.7.
Claims (2)
1. a blast furnace slag desulphurizing ability determination and evaluation method, is characterized in that: comprise desulfurization slag specimen and iron sample preparation, slag iron sample reaction and slag desulfurization capacity evaluate three steps:
1) slag specimen and the preparation of iron sample
With on-the-spot blast furnace slag average chemical constitution for benchmark, according to sample CaO, SiO
2, Al
2o
3with MgO mass percentage be 36% ~ 44%, 30% ~ 36%, 10% ~ 17% and 7% ~ 15% and slag iron take CaO, SiO respectively than 0.27 ~ 0.30
2, Al
2o
3, MgO pure chemistry reagent and on-the-spot blast furnace slag and to put into graphite crucible after fully mixing stand-by;
High-sulfur iron sample is converted to test iron sample sulfur content again with after 95% sulfur content brought into of deduction slag specimen entering stove sulphur analysis, then carries out weighing according to setting slag iron ratio and to prepare and to load graphite crucible stand-by;
2) slag iron reaction
Slag iron reactor adopts upper and lower two-layer graphite crucible, and contain bottom iron crucible and be provided with the identical circular hole of multiple diameter, Circularhole diameter is 8 ~ 10mm, and is evenly distributed in whole crucible bottom; During experiment, first Sheng slag crucible is placed in electric tube furnace and heats up, and start to pass into N from furnace bottom
2gas shielded, treats that slag specimen melts completely and is warming up to more than 1450 DEG C, stirs, splendid attire iron sample crucible is placed in electric furnace on slag crucible, treat that iron sample melts, molten iron drips through crucible bottom circular hole again, drip after finishing completely, in taking-up, crucible waits until the next time of use again, and in stove, slag iron continues reaction more than 25min, then takes out lower crucible, after cooling, get slag iron sample, chemically examine the sulfur content of slag iron sample respectively, and calculate sulphur content distribution coefficient Ls;
3) slag desulfurization capacity evaluation
The ratio of definitely sulfur content in the absolute sulfur content of slag and molten iron is adopted to represent the partition factor Ls of sulphur in slag iron,
in formula, (S) is the percentage composition of sulphur in slag, %; Z is blast furnace slag ratio, kg/t; The percentage composition of sulphur in [S] pig iron, %, Ls are larger, and desulphurizing ability is stronger.
2. a kind of blast furnace slag desulphurizing ability determination and evaluation method according to claim 1, it is characterized in that: described slag iron reactor, upper strata crucible bottom is evenly arranged 6 ~ 8 circular holes.
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