CN115247222A - Control method for preparing 4N-grade high-purity iron and ultralow manganese through pyrogenic process purification - Google Patents
Control method for preparing 4N-grade high-purity iron and ultralow manganese through pyrogenic process purification Download PDFInfo
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- CN115247222A CN115247222A CN202110465926.8A CN202110465926A CN115247222A CN 115247222 A CN115247222 A CN 115247222A CN 202110465926 A CN202110465926 A CN 202110465926A CN 115247222 A CN115247222 A CN 115247222A
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 544
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 268
- 239000011572 manganese Substances 0.000 title claims abstract description 131
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 86
- 238000000746 purification Methods 0.000 title claims abstract description 80
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 230000008569 process Effects 0.000 title claims description 31
- 230000001698 pyrogenic effect Effects 0.000 title claims description 21
- 238000007664 blowing Methods 0.000 claims abstract description 145
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 89
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 76
- 239000001301 oxygen Substances 0.000 claims abstract description 75
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 74
- 229910052786 argon Inorganic materials 0.000 claims abstract description 45
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 45
- 238000007670 refining Methods 0.000 claims abstract description 45
- 230000003647 oxidation Effects 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 31
- 229910000805 Pig iron Inorganic materials 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 69
- 239000002893 slag Substances 0.000 claims description 65
- 238000003723 Smelting Methods 0.000 claims description 18
- 229910000831 Steel Inorganic materials 0.000 claims description 15
- 239000010959 steel Substances 0.000 claims description 15
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 10
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims description 8
- 230000009467 reduction Effects 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 5
- 239000010436 fluorite Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 4
- 238000013459 approach Methods 0.000 claims description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract 1
- 238000009850 CAS-OB (composition adjustment by sealed argon bubbling with oxygen blowing) Methods 0.000 description 18
- 230000001590 oxidative effect Effects 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000009847 ladle furnace Methods 0.000 description 3
- 239000011449 brick Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000617 Mangalloy Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-UHFFFAOYSA-N 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C1/00—Refining of pig-iron; Cast iron
- C21C1/04—Removing impurities other than carbon, phosphorus or sulfur
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C1/00—Refining of pig-iron; Cast iron
- C21C1/02—Dephosphorising or desulfurising
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
Abstract
The fire method purification preparation 4N level high purity iron ultra-low manganese control method, the 4N level high purity iron means the iron element wt% content is 99.97-99.99, the ultra-low manganese means the manganese wt% content is Mn ≤ 0.0015, and the ultra-low manganese index is the index of accomplishing the demanganization operation to the high purity pig iron molten iron output by the blast furnace, on the basis of demanganization by the molten iron blowing method, the combination is based on the top and bottom side composite blowing oxidation purification converter to oxidize the demanganization by the single furnace duplex method and based on the LF refining furnace and the ladle bottom blowing argon top blowing oxygen facility to strongly stir and strongly oxidize the demanganization, which is beneficial to realize the ultra-low manganese index control of Mn ≤ 0.0015 in the fire method purification preparation 4N level high purity iron, thereby better meeting the requirement of the large-scale fire method metallurgy production 4N level high purity iron to the ultra-low manganese.
Description
Technical Field
The invention relates to a high-purity iron demanganizing technology, in particular to a control method for preparing 4N-grade high-purity iron and ultralow manganese by pyrogenic process purification, wherein the content of iron element wt% of the 4N-grade high-purity iron is 99.97-99.99, the content of the ultralow manganese element wt% is Mn% or less than 0.0015, and the ultralow manganese index is an index for completing demanganizing operation on high-purity pig iron and molten iron output by a blast furnace, and the method is favorable for realizing ultralow manganese index control of Mn% or less than 0.0015 in the preparation of the 4N-grade high-purity iron by pyrogenic process purification and large-scale pyrometallurgically production by combining oxidative demanganizing based on a top-bottom composite blowing oxidative purification converter and strong-refining strong-oxidative demanganizing based on an LF furnace and a ladle bottom argon blowing top-blowing oxygen facility on the basis of molten iron and blowing stirring process demanganizing.
Background
In most steel products, the manganese element in the steel is added as a beneficial element in the steel, while some steel products, the manganese element is no longer a beneficial alloy element, and the manganese element is desirable to be contained in a lower content, for example, the requirement of the raw material pure iron for manganese is relatively strict. Pure iron is an iron alloy with extremely low carbon content, the pure iron is divided into electrician pure iron, raw material pure iron, industrial pure iron and the like according to different purposes, the content of manganese element wt% in the raw material pure iron is generally required to be not more than 0.02, and the lower the content, the better the content.
The manganese content of most blast furnace molten iron is between 0.10 and 0.50 in weight percent, a normal converter smelting process is adopted, or a double-slag method is adopted in the smelting process, the residual manganese content at the end point of the converter is relatively high, and the technical requirement of a final product on low manganese content cannot be met. In the aspect of producing blast furnace molten iron, the raw fuel input into the blast furnace is selected and reasonably proportioned, so that the high-purity pig iron molten iron produced by the blast furnace and the wt% content thereof reach the following indexes: c, less than or equal to 4.5; si, less than or equal to 0.5; mn is less than or equal to 0.05; p is less than or equal to 0.030; s is less than or equal to 0.020; cu is less than or equal to 0.001; ni is less than or equal to 0.0020; the balance being Fe. The blast furnace produced high-purity pig iron molten iron provides favorable conditions for preparing 4N-grade high-purity iron through pyrogenic process purification, the inventor utilizes the conditions to control ultralow manganese in the research and development of preparing 4N-grade high-purity iron through pyrogenic process purification, and tests are carried out on blast furnace molten iron containing Mn% of less than or equal to 0.05 for multiple times, so that the beneficial technical effects are obtained.
At present, the converter smelting low manganese steel generally adopts the following measures: ensuring the use of mineral powder with low manganese content as raw material of the blast furnace; the manganese content of the molten iron entering the converter is reduced to the lowest content; smelting by adopting a double-slag method to control the terminal oxygen activity and the molten slag amount of the converter and increase the slag steel distribution ratio of manganese; reducing the tapping temperature; the slag discharge amount of tapping is reduced, and the manganese oxide in the slag is prevented from being reduced and returned to manganese. The above measures for controlling manganese are very effective, so that the manganese at the end point of the converter is further reduced. However, for 4N grade high-purity iron (4N, that is, 4 to 9 purities, the fire purification of the present invention specifies that the 4N grade high-purity iron contains 99.97% to 99.99% of Fe), and Mn is an impurity element, and it is very difficult to remove Mn by the above process if the wt% content of Mn in the 4N grade high-purity iron is controlled to be less than 0.002.
Disclosure of Invention
Aiming at the defects or shortcomings in the prior art, the invention provides a control method for preparing 4N-grade high-purity iron and ultralow manganese by pyrometallurgical purification, wherein the content of iron element wt% of the 4N-grade high-purity iron is 99.97-99.99, the content of ultralow manganese is less than or equal to 0.0015, and the ultralow manganese index is an index for completing demanganization operation on high-purity pig iron and molten iron output by a blast furnace, and the method is characterized in that the method combines oxidation demanganization based on a top-bottom composite blowing oxidation purification converter and strong stirring strong oxidation demanganization based on an LF refining furnace (for regulating the temperature of molten iron) and a ladle bottom argon blowing top-blowing oxygen facility (namely CAS-OB refining equipment) on the basis of molten iron blowing oxygen and stirring method demanganization, so as to be beneficial to realize ultralow manganese index control with Mn% of less than or equal to 0.0015 in preparing 4N-grade high-purity iron by pyrometallurgical purification, thereby better meeting the requirement of producing 4N-grade high-purity iron by pyrometallurgical production on ultralow manganese.
The technical solution of the invention is as follows:
the control method for preparing 4N-grade high-purity iron and ultralow manganese through pyrogenic process purification is characterized by comprising the following steps: a, performing molten iron pretreatment demanganization on high-purity pig iron and molten iron output from a blast furnace into a molten iron tank to obtain a first-stage demanganized molten iron; step B, adding the first-stage demanganized iron liquid into a top-bottom side composite converting oxidation purification converter for oxidation purification and demanganization, pouring Mn and P removal slag out of the iron liquid, adding the iron liquid into the top-bottom side composite converting oxidation purification converter, continuing converting, reducing carbon and heating, and performing other smelting purification to obtain a second-stage demanganized iron liquid; and step C, injecting the second-stage demanganized iron liquid into a ladle of the LF refining furnace, adjusting the temperature and the top slag alkalinity of the iron liquid in the ladle, and then carrying out strong-stirring strong-oxidation demanganization by using a ladle bottom blowing argon top blowing oxygen facility (CAS-OB) to obtain a third-stage demanganized iron liquid, wherein the third-stage demanganized iron liquid reaches an ultralow manganese index that the manganese wt% content is less than or equal to 0.0015.
The manganese content in the high-purity pig iron molten iron in the step A is less than or equal to 0.05 percent by weight.
The high-purity pig iron and molten iron in the step A meet the following indexes in percentage by weight: c, less than or equal to 4.5; si, less than or equal to 0.5; mn is less than or equal to 0.05; p is less than or equal to 0.030; s is less than or equal to 0.020; cu is less than or equal to 0.001; ni is less than or equal to 0.0020; the balance being Fe.
The pretreatment demanganization in the step A is demanganization by a molten iron blowing method, the demanganization by the molten iron blowing method comprises a molten iron pretreatment oxygen blowing gun and a powder spraying stirring gun which are arranged at the top of the molten iron tank, and the molten iron pretreatment oxygen blowing gun blows oxygen to the molten iron liquid surface at a distance of 600-1200 mm close to the liquid surface of the high-purity pig iron molten iron so as to pass through Mn + O 2 ＝MnO 2 The preliminary removal of Mn in the molten iron is finished in a reaction mode, the nozzle end of the powder spraying stirring gun is inserted into the high-purity pig iron molten iron and blows fluidized lime powder to stir the molten ironThe demanganizing slag is formed in the process, and the condition of meeting the high demanganizing rate (more than 80%) is as follows: the temperature of molten iron is less than 1280 ℃, and the alkalinity R of the demanganized slag is = 0.45-0.65.
And when the first-stage demanganized iron liquid reaches the index of Mn% less than or equal to 0.010, removing demanganized slag on the liquid level of the molten iron and entering the next procedure.
The top-bottom side composite blowing oxidation purification converter in the step B comprises a bottom blowing gun arranged at the bottom of the furnace body, a side blowing gun arranged at the side of the furnace body, a top blowing oxygen gun and a compound gun arranged at the top of the furnace body, wherein the compound gun is used for measuring temperature, sampling, fixing carbon and/or fixing oxygen, the oxidation purification demanganization in the step B adopts a full iron method for smelting, the oxygen blowing purification smelting is finished for 8-12 min, mn and P removing slag is poured out from iron liquid, then the iron liquid is added into the top-bottom side composite blowing oxidation purification converter, the blowing is continued for 7-13 min, the carbon reduction and temperature rise are carried out for other purifications, and the demanganization iron liquid in the second stage reaches the index that Mn% is less than or equal to 0.004.
The top-blown oxygen supply intensity of the top-blown oxygen lance is 3.5Nm 3 Min, the bottom blowing air supply intensity of the bottom blowing gun is 0.15Nm 3 /t.min，Nm 3 Standard cubic meter, t is ton, min is minute.
And C, arranging a heating electrode capable of being inserted into a top slag layer at the top of the ladle of the LF refining furnace in the step C, connecting the top slag layer with a stock bin through a feeding device, arranging a bottom argon blowing interface at the bottom of the ladle, blowing argon into the molten iron through the bottom argon blowing interface for stirring, inputting fluorite and/or active lime into the top slag layer through the stock bin and the feeding device so as to enable the slagging thickness of the top slag to be 150-200 mm, enabling the alkalinity R = 1.6-2.5 of the top slag, and controlling the temperature of the molten iron to be 1570-1590 ℃ through electrode heating.
And C, the steel ladle bottom-blowing argon top-blowing oxygen facility comprises an impregnation cover and an oxygen-blowing lance which are arranged at the top of the steel ladle, the impregnation cover and the oxygen-blowing lance are coaxially arranged, and a bottom-blowing argon interface is arranged at the bottom of the steel ladle.
The strong stirring strong oxidation demanganization in the step C comprises the following steps: step C1, hoisting the ladle with the temperature adjusted by the LF refining furnace to CAS-OB treatmentA bit; step C2, starting bottom blowing argon through the bottom blowing argon interface, gradually increasing the intensity of the argon blowing until a slag-free area with phi of 800-1000 mm is formed on the surface of the molten iron in the steel ladle, lowering the dipping cover, and lowering the oxygen blowing lance until the oxygen blowing lance approaches to the surface of the molten iron to blow oxygen on the surface of the molten iron; step C3, when the mass fraction of the free oxygen in the molten iron reaches 600-900 ppm, lifting the dipping cover and the oxygen blowing lance, and increasing the argon blowing flow of the steel ladle to 50-100 Nm 3 The iron liquid is stirred strongly for 10 to 25min; and C4, detecting the manganese content in the molten iron, returning to the step C2 if the Mn% in the molten iron is more than 0.0015, stopping the demanganization treatment if the Mn% in the molten iron is less than or equal to 0.0015, performing deslagging operation after demanganization of the molten iron is finished, and removing demanganization top slag of the molten iron in the ladle. h is hours and min is minutes.
The invention has the following technical effects: according to the control method for preparing the 4N-grade high-purity iron ultralow manganese through the pyrogenic process purification, the ultralow manganese control is divided into three stages, and the first-stage demanganized iron liquid, the second-stage demanganized iron liquid and the third-stage demanganized iron liquid are respectively obtained, so that the demanganization effect can be conveniently implemented in a segmented manner. And the pretreatment demanganization, top-bottom side combined blowing oxidation purification demanganization, temperature adjustment and top slag alkalinity adjustment based on an LF refining furnace and strong oxidation strong stirring demanganization in a ladle based on a ladle bottom argon blowing top oxygen blowing facility are effectively combined, so that the ultralow manganese index control with the manganese weight percent content of Mn less than or equal to 0.0015 is realized in the preparation of 4N grade high-purity iron by pyrogenic process purification.
The invention has the following characteristics: (1) the purity of the high-purity iron is 99.97-99.99% (4N). Other impurity elements are removed by pyrometallurgical purification, and the 4N high-purity iron component meets (but is not limited to) the following requirements: less than or equal to 0.0005 percent of C, less than or equal to 0.001 percent of Si, less than or equal to 0.0015 percent of Mn, less than or equal to 0.0005 percent of P, less than or equal to 0.0005 percent of S, less than or equal to 0.0001 percent of Ti, less than or equal to 0.002 percent of Al, less than or equal to 0.0005 percent of Cr, less than or equal to 0.001 percent of Cu, less than or equal to 0.0020 percent of Ni, less than or equal to 0.002 percent of O, less than or equal to 0.030 percent of other elements except iron, and 99.97 to 99.99 percent of iron. (2) The invention relates to a method for producing molten iron with lower manganese content, namely, the method can further remove Mn element in the molten iron by adopting external refining to deeply purify the molten iron, and the requirement of 4N-grade high-purity iron is met. (3) And (3) carrying out pyrometallurgy, reasonably combining Mn removing facilities by adopting related refining equipment facilities according to thermodynamic and kinetic conditions favorable for manganese removal, fully playing the thermodynamic and kinetic conditions of manganese removal of the molten iron, removing Mn elements in the molten iron to the maximum extent, and meeting the requirements of raw material pure iron on products with low manganese content. (4) After the method is adopted to remove Mn from the molten iron and purify the molten iron, mn in the molten iron can be less than or equal to 0.0015 percent, and the requirement of high-purity iron and ultra-pure iron raw material products on low manganese control can be met.
Drawings
FIG. 1 is a schematic diagram of demanganization of molten iron by oxygen blowing and blowing stirring method in the control method for preparing 4N-grade high-purity iron by pyrogenic process purification. The arrows in fig. 1 indicate the main direction of movement of the lime powder in the molten iron.
FIG. 2 is a schematic diagram of the oxidative demanganization of a top-bottom side combined blowing oxidative purification converter in the control method for preparing 4N-grade high-purity iron ultra-low manganese by pyrogenic purification.
FIG. 3 is a schematic diagram showing the temperature adjustment of molten iron and the top slag alkalinity adjustment in an LF refining Furnace by implementing the control method for preparing 4N-grade high-purity iron and ultralow-manganese by pyrogenic purification according to the present invention (LF, ladle Furnace, ladle refining Furnace). And the LF refining furnace is used for adjusting the temperature of the molten iron and the alkalinity of the top slag.
FIG. 4 is a schematic diagram of strong oxidation strong stirring demanganization of a ladle bottom blowing argon top blowing oxygen facility in the control method for preparing 4N-grade high-purity iron ultralow manganese by pyrogenic process purification. The strong oxidative strong agitation demanganization in FIG. 4 was performed using a CAS-OB facility (CAS-OB, composition Adjustment by Sealed Argon blowing-Oxygen blowing Composition Adjustment).
The reference numbers are listed below: 1-a hot metal ladle; 2-molten iron; 3-liquid level; 4-blowing lance for molten iron pretreatment; 5-powder spraying stirring gun; 6-blowing, oxidizing and purifying converter at top and bottom sides; 7-bottom blowing gun; 8-side blowing gun; 9-top blowing gun; 10-complex gun (for measuring temperature, sampling, carbon determination, oxygen determination, etc.); 11-a ladle; 12-iron liquid; 13-air brick; 14-bottom blowing argon interface; 15-blowing oxygen lance; 16-dipping cover; 17-argon bubble; 20-a feeding device; 21-a storage bin; 22-a heating electrode; 23-top slag.
Detailed Description
The invention is described below with reference to the examples and the figures (fig. 1-4).
FIG. 1 is a schematic diagram of demanganization of molten iron by oxygen blowing and blowing stirring processes by implementing the control method for preparing 4N-grade high-purity iron by pyrogenic process purification according to the present invention with ultra-low manganese. FIG. 2 is a schematic diagram of the oxidative demanganization of a top-bottom side combined blowing oxidative purification converter in the control method for preparing 4N-grade high-purity iron ultra-low manganese by pyrogenic purification. FIG. 3 is a schematic diagram showing the temperature adjustment of molten iron and the top slag alkalinity adjustment in an LF refining Furnace by implementing the control method for preparing 4N-grade high-purity iron and ultralow-manganese by pyrogenic purification according to the present invention (LF, ladle Furnace, ladle refining Furnace). FIG. 4 is a schematic diagram of strong oxidation strong stirring demanganization of a ladle bottom-blown argon top-blown oxygen facility in the control method for preparing 4N-grade high-purity iron ultralow manganese by pyrogenic process purification. Referring to fig. 1 to 4, the control method for preparing 4N-grade high-purity iron and ultralow-manganese by pyrogenic purification comprises the following steps: a, performing molten iron pretreatment demanganization on high-purity pig iron molten iron (molten iron 2) output from a blast furnace into a molten iron tank 1 in the molten iron tank 1 to obtain a first-stage demanganized molten iron; step B, adding the first-stage demanganized iron liquid into a top-bottom side composite blowing oxidation purification converter 6 for oxidation purification demanganization, pouring Mn and P removal slag out of the iron liquid, adding the iron liquid into the top-bottom side composite blowing oxidation purification converter for carbon reduction, temperature rise and other smelting purification, and obtaining a second-stage demanganized iron liquid; and step C, injecting the second-stage demanganized iron liquid into a ladle 11 of the LF refining furnace, adjusting the temperature and the top slag alkalinity of the iron liquid in the ladle 11, and then performing strong-stirring strong-oxidation demanganization by using a ladle bottom Argon-blowing top-blowing Oxygen facility (such as a CAS-OB facility, CAS-OB, composition Adjustment by Sealed Argon-blowing Oxygen component Adjustment) to obtain a third-stage demanganized iron liquid, wherein the third-stage demanganized iron liquid reaches an ultralow-manganese index that the manganese wt% content is less than or equal to 0.0015. The manganese content in the high-purity pig iron molten iron in the step A is less than or equal to 0.05 percent by weight. The high-purity pig iron and molten iron in the step A meet the following indexes in percentage by weight: c, less than or equal to 4.5; si is less than or equal to 0.5; mn is less than or equal to 0.05; p is less than or equal to 0.030; s is less than or equal to 0.020; cu is less than or equal to 0.001; ni is less than or equal to 0.0020; the balance being Fe. The step A of the pretreatment demanganization is molten iron blowingDemanganization by molten iron blowing method comprises a molten iron pretreatment oxygen blowing gun 4 and a powder spraying stirring gun 5 which are arranged at the top of the molten iron tank 1, wherein the molten iron pretreatment oxygen blowing gun 4 blows oxygen to the molten iron liquid surface 3 at a distance of 600-1200 mm from the molten iron pretreatment oxygen blowing gun 4 to the molten iron liquid surface 3 so as to pass through Mn + O 2 ＝MnO 2 The preliminary removal of Mn in molten iron is completed in a reaction mode, the nozzle end of the powder spraying stirring gun 5 is inserted into the high-purity pig iron molten iron and blows fluidized lime powder to form demanganization slag in the stirred molten iron, and the conditions of high demanganization rate (more than 80%) are as follows: the temperature of molten iron is less than 1280 ℃, and the alkalinity R of the demanganized slag is = 0.45-0.65. And when the first-stage demanganized iron liquid reaches the index of Mn% less than or equal to 0.010, removing demanganized slag on the liquid level of the molten iron and entering the next procedure.
The top-bottom side composite blowing oxidation purification converter 6 in the step B comprises a bottom blowing gun 7 arranged at the bottom of the furnace body, a side blowing gun 8 arranged at the side part of the furnace body, a top blowing oxygen lance 9 and a compound gun 10 arranged at the top of the furnace body, wherein the compound gun 10 is used for measuring temperature, sampling, fixing carbon and/or fixing oxygen, the oxidation purification demanganization in the step B adopts a full iron method for smelting, the oxygen blowing purification smelting is finished for 8-12 min, mn and P removing slag is poured out from the discharged iron liquid, then the iron liquid is added into the top-bottom side composite blowing oxidation purification converter, the blowing is continued for 7-13 min, carbon reduction and temperature rise are carried out, other smelting purification are carried out, and the demanganization liquid in the second stage reaches the index that Mn is less than or equal to 0.004%. The top-blown oxygen supply intensity of the top-blown oxygen lance is 3.5 (Nm) 3 T.min), the bottom blowing gas supply intensity of the bottom blowing gun is 0.15 (Nm) 3 At t.min), wherein Nm 3 In standard cubic meters, t is ton. The top of the ladle 11 of the LF refining furnace in the step C is provided with a heating electrode 22 inserted into a top slag layer 23 (the bottom end of the heating electrode is located above the liquid level 3), the top slag layer 23 is connected with a storage bin 21 through a feeding device 20, the bottom of the ladle 11 is provided with a bottom argon blowing interface 14 (a gas permeable brick 13 can be adopted in the structure), argon is blown to the molten iron 12 through the bottom argon blowing interface 14 for stirring (argon bubbles 17 are formed in the molten iron 12), fluorite and/or active lime are input into the top slag layer 23 through the storage bin 21 and the feeding device 20 so that the slagging thickness of the top slag is 150-200 mm, and the alkalinity R = 1.6-2.5,the temperature of the molten iron is 1570-1590 ℃ through the heating electrode 22. The ladle bottom-blown argon top-blown oxygen facility in the step C comprises an immersion cover 16 and an oxygen-blowing lance 15 which are arranged on the top of the ladle 11, the immersion cover 16 is sleeved with the oxygen-blowing lance 15, the immersion cover 16 and the oxygen-blowing lance 15 are coaxially arranged, and a bottom-blown argon interface 14 is arranged at the bottom of the ladle 11. The strong stirring strong oxidation demanganization in the step C comprises the following steps: step C1, hoisting the ladle 11 of the LF refining furnace to a ladle bottom blowing argon top blowing oxygen facility (CAS-OB facility); step C2, starting bottom blowing argon through the bottom blowing argon interface 14 and gradually increasing the argon blowing intensity until a slag-free area with phi of 800-1000 mm is formed on the surface of the molten iron in the ladle 11, lowering the dipping cover 16, and lowering the oxygen blowing lance 15 until the surface of the molten iron is close to the surface of the molten iron to blow oxygen on the surface of the molten iron; step C3, when the mass fraction of the free oxygen in the molten iron 12 reaches 600-900 ppm, lifting the dipping cover 16 and the oxygen blowing lance 15, and increasing the argon blowing flow of the steel ladle to 50-100 Nm 3 Strong stirring the molten iron 12 for 10-25 min (forming argon bubbles 17 in the molten iron 12); and C4, detecting the manganese content in the molten iron 12, returning to the step C2 if the Mn in the molten iron is more than 0.0015%, stopping the manganese removal treatment if the Mn in the molten iron 12 is less than or equal to 0.0015%, completing the manganese removal of the molten iron and deslagging, and removing the demanganized top slag of the molten iron in the ladle 11.
The method for deep demanganization of molten iron comprises the following steps:
(1) the process route of the deep demanganization of the molten iron (combined with the pyrogenic process for purifying and preparing 4N-grade high-purity iron): blast Furnace high-purity pig iron molten iron, molten iron pretreatment desulfurization, molten iron pretreatment desiliconization demanganization, top and bottom side combined blowing oxidation purification converter desiliconization, manganese, phosphorus, carbon and the like, RH (Ruhrstahl-Heraeus-Vacuum refining, vacuum circulation Degassing refining), LF (Ladle Furnace, ladle refining Furnace), CASOB (Composition addition by Sealed Argon blowing Oxygen blowing component Adjustment), ladle (refining Ladle) deslagging and finishing preparation of the ultra-low manganese iron liquid.
(2) The blast furnace produces high-purity pig iron and molten iron. Raw fuel fed into a blast furnace is selected, ore is reasonably proportioned, and manganese in high-purity pig iron and molten iron is strictly controlled, wherein the content of Mn in the molten iron is less than or equal to 0.05 percent. The high-purity pig iron and molten iron comprises the following components: c, less than or equal to 4.5; si is less than or equal to 0.5; mn is less than or equal to 0.05; p is less than or equal to 0.030; s is less than or equal to 0.020; cu is less than or equal to 0.001; ni is less than or equal to 0.0020.
(3) And (4) removing Mn by pretreating molten iron. In a ladle (also called as a hot metal ladle), top-blown oxygen and blown fluidized lime powder are adopted for stirring, mn slag is removed after the stirring, and the preliminary removal of Mn in the hot metal is completed: mn + O2= MnO2. The process can control Mn in molten iron (also called as molten iron) to be less than or equal to 0.010 percent, and meets the conditions of high demanganization rate (more than 80 percent) as follows: the temperature of molten iron is less than 1280 ℃, and the alkalinity is controlled to be R = 0.45-0.65.
(4) The pretreated molten iron is added into a top-bottom combined blowing oxidation purification converter for purification and smelting, the top-bottom combined blowing oxidation purification converter is a multifunctional multipoint oxygen blowing furnace, and the top blowing oxygen supply intensity is 3.5Nm 3 At t.min, bottom blowing intensity of 0.15Nm 3 T.min. And (3) adding iron by adopting a full iron method, purifying and smelting for 8-12 min, pouring out Mn-removing and P-removing slag from the iron liquor, and adding the iron liquor into a top-bottom composite blowing oxidation purification converter for other smelting and purification. The process can purify manganese in the molten iron until Mn is less than or equal to 0.004 percent.
(5) And (4) deeply removing Mn in the LF furnace and CAS-OB. And the LF furnace is used for adjusting the temperature of the molten iron and the top slag reduction degree. After the iron liquid purified and demanganized by the top-bottom side composite converting oxidation purification converter by adopting a duplex method enters a refining ladle (namely a steel ladle), temperature adjustment and top slag alkalinity adjustment are carried out at an LF furnace station, 300-1000 kg of active lime and 50-300 kg of fluorite (according to the common steel ladle iron liquid capacity) are added, the slagging thickness is 150-200 mm, the iron liquid is properly heated by using an electrode to melt slag, and when the slag is melted, the alkalinity R = 1.6-2.5 of the top slag and the temperature of the iron liquid is 1570-1590 ℃, the treatment of the process is considered to be finished.
CAS-OB deep demanganization treatment. And lifting the refining package to a CAS-OB deep demanganization treatment position. Because the manganese oxide of the manganese oxide is alkaline, the alkalinity of top slag in the process of removing manganese through oxidation is moderate, low alkalinity and good fluidity are required, and in addition, the equilibrium constant k of the reaction of the Mn element and the ferric oxide is reduced along with the rise of the temperature, so that the proper temperature reduction is favorable for the oxidation removal of manganese. In the CAS-OB station treatment process, the strength of bottom blowing argon is properly increased, and when the surface of the refined molten iron forms a slag with the diameter of 800-1000 mmWhen the slag zone is in the state of slag, the dipping cover is lowered, the oxygen blowing lance is lowered to blow oxygen to the iron liquid, when the free oxygen content in the iron liquid reaches 600-900 ppm, the dipping cover and the oxygen blowing lance are lifted, the flow of argon blowing at the bottom of the refining ladle is increased, the iron liquid is stirred strongly for 10-25 min, and the flow of argon blowing at the bottom is 50-100 Nm 3 /h。
When the manganese content in the iron liquid is removed to the extent that Mn is less than or equal to 0.0015 percent, the manganese removal requirement is met, the treatment is stopped, and the manganese removal of the iron liquid is completed. Otherwise, repeating the above operations until the demanganization reaches the required target composition.
And after the demanganization and purification of the molten iron are finished, carrying out deslagging operation on the molten iron, namely removing demanganization top slag of the base liquid in the refining ladle.
(6) The method is adopted to remove manganese from the molten iron, and the manganese removal effect reaches that Mn is less than or equal to 0.0015%.
The main equipment and facilities for deeply removing manganese and purifying the molten iron of the invention are respectively as follows: the molten iron pretreatment equipment comprises a Mn removal and P removal facility by blowing, a top and bottom composite blowing oxidation purification converter, an LF refining facility and a CAS-OB oxygen blowing and argon blowing refining facility. Wherein, the molten iron pretreatment Mn-removing and P-removing blowing-blowing facility (as shown in figure 1) has the functions of desiliconization, mn-removing and P-removing; the top and bottom combined converting, oxidizing and purifying converter (as shown in figure 2) has the characteristic of multipoint strong oxidation and can oxidize and remove all easily oxidized impurity elements; adjusting the temperature of molten iron to 1570-1590 ℃ and the top slag alkalinity to R = 1.6-2.5 by an LF refining facility (or called as an LF refining furnace shown as a figure 3); the main function of CAS-OB oxygen and argon blowing refining facility (as shown in figure 4) on manganese removal is strong oxidation and strong stirring by blowing oxygen.
The invention relates to a novel method for performing deep demanganization on blast furnace molten iron by a top-bottom composite blowing oxidation purification converter after demanganization and slag skimming of the molten iron by adopting molten iron pretreatment, a single-furnace duplex method and an LF refining furnace and CAS-OB refining facility, which has the following characteristics:
(1) the refining process carries out deep demanganization operation in the refining ladle, can fully realize the thermodynamic and kinetic conditions of demanganization, and achieves the demanganization and purification of the molten iron to the maximum extent.
(2) The demanganization treatment time is sufficient, and the demanganization time for iron liquid purification is 10-40 min, so that the oxidation demanganization reaction tends to be balanced.
(3) And melting slag by using an LF refining furnace to promote the added lime and fluorite to be quickly melted into slag, and quickly forming low-alkalinity top slag. Meanwhile, the LF refining furnace can quickly adjust the temperature of the molten iron, so that the demanganization and purification operation of the molten iron at a lower temperature is ensured, and the oxidation removal of Mn is facilitated.
(4) The introduction of CAS-OB is one of the most effective refining facilities for demanganization, is very flexible in the demanganization process, can realize stirring with large gas amount, increase the kinetic conditions of demanganization, and can also perform oxygen blowing operation on molten iron, improve the oxidability of the molten iron and accelerate the rapid demanganization reaction. The CAS-OB is adopted to blow oxygen to the iron liquid, so that the oxygen content in the iron liquid is increased, and simultaneously, the pollution to the iron liquid caused by adding other oxides (such as ferric oxide and the like) is eliminated.
(5) The LF refining furnace and CAS-OB refining facilities are adopted to carry out deep demanganization refining treatment on the molten iron, so that the advantages of demanganization can be fully exerted: low alkalinity, low temperature, high oxidability, large slag amount and strong stirring. Realizing the deep demanganization and purification of the molten iron in the refining process.
(6) The Mn in the iron liquid is less than or equal to 0.0015 percent.
Those not described in detail in this specification are well within the skill of the art. It is pointed out here that the above description is helpful for the person skilled in the art to understand the invention, but does not limit the scope of the invention. Any and all equivalents, modifications, and/or omissions to the system described above may be made without departing from the spirit and scope of the invention.
Claims (10)
1. The control method for preparing the 4N-grade high-purity iron and ultralow manganese through pyrogenic process purification is characterized by comprising the following steps of: a, carrying out demanganization on high-purity pig iron and molten iron output from a blast furnace into a molten iron tank by adopting molten iron pretreatment in the molten iron tank to obtain a first-stage demanganized molten iron; step B, adding the first-stage demanganized iron liquid into a top-bottom side composite converting oxidation purification converter for oxidation purification demanganization, pouring Mn and P removal slag out of the iron liquid, adding the iron liquid into the top-bottom side composite converting oxidation purification converter for carbon reduction, temperature rise and other smelting purification, and obtaining a second-stage demanganized iron liquid; and step C, injecting the second-stage demanganized iron liquid into a ladle of the LF refining furnace, adjusting the temperature and the top slag alkalinity of the iron liquid in the ladle, and then carrying out strong-stirring strong-oxidation demanganization by using a ladle bottom-blowing argon top-blowing oxygen facility to obtain a third-stage demanganized iron liquid, wherein the third-stage demanganized iron liquid reaches an ultralow manganese index that the manganese content is less than or equal to 0.0015.
2. The fire purification preparation 4N-grade high-purity iron ultralow manganese control method according to claim 1, wherein the manganese content in the high-purity pig iron molten iron in the step A is less than or equal to 0.05 percent by weight.
3. The fire purification preparation 4N-grade high-purity iron ultralow manganese control method according to claim 1, characterized in that the high-purity pig iron and the molten iron composition and the wt% content thereof in the step A meet the following indexes: c, less than or equal to 4.5; si, less than or equal to 0.5; mn is less than or equal to 0.05; p is less than or equal to 0.030; s is less than or equal to 0.020; cu is less than or equal to 0.001; ni is less than or equal to 0.0020; the balance being Fe.
4. The control method for preparing 4N-grade high-purity iron with ultralow manganese through pyrometallurgical purification according to claim 1, wherein the pretreatment demanganization in the step A is hot metal blowing demanganization, the hot metal blowing demanganization comprises a hot metal pretreatment oxygen blowing gun and a powder spraying stirring gun which are arranged at the top of the hot metal tank, and the hot metal pretreatment oxygen blowing gun blows oxygen to the liquid level of the hot metal at a distance of 600-1200 mm from the liquid level of the high-purity pig iron so as to pass through Mn + O 2 ＝MnO 2 The preliminary removal of Mn in molten iron is finished in a reaction mode, the nozzle end of the powder-spraying stirring gun is inserted into the high-purity pig iron molten iron and blows fluidized lime powder to form demanganization slag in the stirred molten iron, and the conditions of high demanganization rate (more than 80%) are as follows: the temperature of molten iron is less than 1280 ℃, and the alkalinity R of the demanganized slag is = 0.45-0.65.
5. The fire purification control method for preparing 4N-grade high-purity iron with ultralow manganese according to claim 4, characterized in that the demanganization iron liquid in the first stage reaches the index of Mn% less than or equal to 0.05, and when the index is reached, demanganization slag on the liquid level of the molten iron is removed, and the next procedure is carried out.
6. The fire purification preparation 4N-grade high-purity iron ultralow manganese control method according to claim 1, wherein the top-bottom side combined blowing oxidation purification converter in the step B comprises a bottom blowing gun arranged at the bottom of the furnace body, a side blowing gun arranged at the side of the furnace body, a top blowing oxygen gun and a compound gun arranged at the top of the furnace body, wherein the compound gun is used for measuring temperature, sampling, carbon determination and/or oxygen determination, the oxidation purification demanganization in the step B adopts a full iron method for smelting, the oxygen blowing purification smelting is finished for 8-12 min, the discharged iron liquid is poured out with Mn and P removal slag, then the iron liquid is added into the top-bottom side combined blowing oxidation purification converter for other smelting purification such as carbon reduction and temperature rise, and the second-stage demanganization iron liquid reaches the index Mn less than or equal to 0.004.
7. The controlled method for preparing 4N-grade high-purity iron and ultralow-manganese by pyrometallurgical purification according to claim 6, wherein the top-blown oxygen supply intensity of the top-blown oxygen lance is 3.5 (Nm & lt/EN & gt) 3 Min) and the bottom blowing air supply intensity of the bottom blowing gun is 0.15 (Nm) 3 At t.min), wherein, nm 3 Expressed in standard cubic meters, t in tons and min in minutes.
8. The fire purification and preparation control method of 4N-grade high-purity iron and ultralow-manganese according to claim 1, characterized in that a heating electrode inserted into a top slag layer is arranged at the top of the ladle of the LF refining furnace in the step C, the top slag layer is connected with a storage bin through a feeding device, a bottom argon blowing interface is arranged at the bottom of the ladle, the molten iron is blown with argon through the bottom argon blowing interface and is stirred, fluorite and/or active lime are input into the top slag layer through the storage bin and the feeding device so that the slagging thickness of the top slag is 150-200 mm, the alkalinity R = 1.6-2.5 of the top slag, and the temperature of the molten iron is 1570-1590 ℃ through the heating electrode.
9. The fire purification preparation 4N-grade high-purity iron ultralow manganese control method according to claim 1, wherein the ladle bottom argon-blowing top-blowing oxygen facility in step C comprises an immersion cover and an oxygen-blowing lance which are arranged on the top of the ladle, the immersion cover is sleeved with the oxygen-blowing lance, the immersion cover and the oxygen-blowing lance are coaxially arranged, and a bottom argon-blowing interface is arranged at the bottom of the ladle.
10. The control method for preparing 4N-grade high-purity iron and ultralow-manganese through pyrogenic process purification according to claim 9, wherein the strong stirring and strong oxidation demanganization in step C comprises the following steps: c1, hoisting the ladle of the LF refining furnace to the ladle bottom argon-blowing top-blown oxygen facility; step C2, starting bottom blowing argon through the bottom blowing argon interface, gradually increasing the argon blowing intensity until a slag-free area with phi of 800-1000 mm is formed on the surface of the molten iron in the steel ladle, lowering the dipping cover, and lowering the oxygen blowing lance until the oxygen blowing lance approaches to the surface of the molten iron to blow oxygen on the surface of the molten iron; step C3, when the mass fraction of the free oxygen in the molten iron reaches 600-900 ppm, lifting the dipping cover and the oxygen blowing lance, and increasing the argon blowing flow of the steel ladle to 50-100 Nm 3 The iron liquid is stirred strongly for 10 to 25min; and C4, detecting the manganese content in the molten iron, returning to the step C2 if the Mn% in the molten iron is more than 0.0015, stopping the manganese removal treatment if the Mn% in the molten iron is less than or equal to 0.0015, completing the manganese removal of the molten iron, performing slag removal operation, and removing the manganese-removed top slag of the molten iron in the ladle.
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