CN115247222B - Control method for preparing 4N-grade high-purity iron ultralow manganese through fire purification - Google Patents
Control method for preparing 4N-grade high-purity iron ultralow manganese through fire purification Download PDFInfo
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- CN115247222B CN115247222B CN202110465926.8A CN202110465926A CN115247222B CN 115247222 B CN115247222 B CN 115247222B CN 202110465926 A CN202110465926 A CN 202110465926A CN 115247222 B CN115247222 B CN 115247222B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 479
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 238
- 239000011572 manganese Substances 0.000 title claims abstract description 111
- 229910052748 manganese Inorganic materials 0.000 title claims abstract description 72
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000746 purification Methods 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000007664 blowing Methods 0.000 claims abstract description 131
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 105
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 85
- 239000001301 oxygen Substances 0.000 claims abstract description 84
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 80
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 54
- 229910052786 argon Inorganic materials 0.000 claims abstract description 53
- 230000003647 oxidation Effects 0.000 claims abstract description 50
- 238000007670 refining Methods 0.000 claims abstract description 44
- 238000003756 stirring Methods 0.000 claims abstract description 30
- 229910000805 Pig iron Inorganic materials 0.000 claims abstract description 22
- 239000002893 slag Substances 0.000 claims description 70
- 239000007788 liquid Substances 0.000 claims description 55
- 238000003723 Smelting Methods 0.000 claims description 17
- 239000002131 composite material Substances 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000002347 injection Methods 0.000 claims description 13
- 239000007924 injection Substances 0.000 claims description 13
- 239000000843 powder Substances 0.000 claims description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000010079 rubber tapping Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 9
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 9
- 238000007598 dipping method Methods 0.000 claims description 9
- 239000004571 lime Substances 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 7
- 239000010959 steel Substances 0.000 claims description 7
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000010436 fluorite Substances 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 4
- 238000013459 approach Methods 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 3
- 238000002360 preparation method Methods 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 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
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 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 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000009847 ladle furnace Methods 0.000 description 3
- 238000013019 agitation Methods 0.000 description 2
- 239000011449 brick Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- DALUDRGQOYMVLD-UHFFFAOYSA-N iron manganese Chemical compound [Mn].[Fe] DALUDRGQOYMVLD-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
- 238000009853 pyrometallurgy Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007921 spray Substances 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
- 241001062472 Stokellia anisodon Species 0.000 description 1
- NJFMNPFATSYWHB-UHFFFAOYSA-N ac1l9hgr Chemical compound [Fe].[Fe] NJFMNPFATSYWHB-UHFFFAOYSA-N 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 235000011116 calcium hydroxide Nutrition 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
- 238000012217 deletion Methods 0.000 description 1
- 230000037430 deletion Effects 0.000 description 1
- 238000007599 discharging Methods 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
- 238000009434 installation Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000009290 primary effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 230000001698 pyrogenic effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
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
Landscapes
- 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 control method for preparing the 4N-grade high-purity iron by fire purification comprises the steps that the weight percent of 4N-grade high-purity iron is 99.97-99.99, the weight percent of manganese is less than or equal to 0.0015, the ultralow manganese index is an index for finishing the demanganization operation of high-purity pig iron output by a blast furnace, and the combination of the single-furnace duplex oxidation demanganization based on a top-bottom side combined blowing oxidation purification converter and the strong-stirring strong-oxidation demanganization based on an LF refining furnace and a ladle bottom-blowing argon top-blowing oxygen facility is beneficial to realizing the ultralow manganese index control of less than or equal to 0.0015 of Mn in the preparation of the 4N-grade high-purity iron by fire purification, so that the requirement of the 4N-grade high-purity iron on ultralow manganese in large-scale fire metallurgy production is better met.
Description
Technical Field
The invention relates to a high-purity iron demanganization technology, in particular to a control method for preparing 4N-grade high-purity iron ultra-low manganese by fire purification, wherein the weight percent of 4N-grade high-purity iron is 99.97-99.99, the weight percent of manganese is Mn-less than or equal to 0.0015, the ultra-low manganese index is an index for finishing demanganization operation on high-purity pig iron output by a blast furnace, and the oxidation demanganization based on a top-bottom side composite blowing oxidation purification converter and the strong stirring strong oxidation demanganization based on an LF refining furnace and a ladle bottom-blowing argon top-blowing oxygen facility are combined on the basis of molten iron oxygen blowing and blowing stirring demanganization, so that the ultra-low manganese index control of Mn-less than or equal to 0.0015 is realized in the fire purification preparation of 4N-grade high-purity iron, thereby better meeting the requirement of 4N-grade high-purity iron on ultra-low manganese in large-scale pyrometallurgical production.
Background
In most steel products, manganese in the steel is added as a beneficial element to the steel, while manganese in some steel products is no longer a beneficial alloying element, and it is desirable that the lower the content is, the better the manganese requirements are, such as the raw material pure iron. Pure iron is an iron alloy with extremely low carbon content, and is classified into electric pure iron, raw pure iron, industrial pure iron and the like according to different purposes, and the weight percent of manganese element in the raw pure iron is generally required to be not more than 0.02, and the lower the manganese element is, the better the manganese element is.
The weight percent of manganese in most blast furnace molten iron is between 0.10 and 0.50, and the technical requirement of the final product on low manganese content cannot be met by adopting a normal converter smelting process or adopting a double slag method in the smelting process, wherein the residual manganese at the end point of the converter is relatively high. In the aspect of producing the blast furnace molten iron, the raw fuel input into the blast furnace is carefully selected, reasonably blended, and the like, so that the components of the high-purity pig iron molten iron produced by the blast furnace and the weight percent content thereof reach the following indexes: 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, 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 invention discloses a method for preparing 4N-grade high-purity iron by using a high-purity pig iron produced by a blast furnace, which provides favorable conditions for preparing the 4N-grade high-purity iron by a fire purification method.
At present, the converter is adopted to smelt low manganese steel generally by adopting the following measures: ensuring the use of mineral powder with low manganese content for blast furnace raw materials; the manganese content of molten iron entering the converter is reduced to the lowest content; smelting and controlling the final oxygen activity and slag amount of the converter by adopting a double slag method, and increasing the slag steel distribution ratio of manganese; lowering the tapping temperature; reducing the slag discharging amount of tapping and preventing manganese oxide in slag from undergoing reduction reaction to return manganese. The above manganese control measures are very effective, so that the manganese at the end point of the converter is further reduced. However, in the case of 4N-grade high-purity iron (4N, i.e., 4 to 9 purity, the present invention provides a fire purification in which 4N-grade high-purity iron is defined as having an Fe content of 99.97% to 99.99%), mn is an impurity element, and it is very difficult to remove Mn element by the above-mentioned process to control the wt% content of Mn in 4N-grade high-purity iron to 0.002 or less, and it is hardly possible to achieve the above-mentioned removal.
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 by fire purification, wherein the weight percent of 4N-grade high-purity iron is 99.97-99.99, the weight percent of manganese is less than or equal to 0.0015, and the ultralow manganese index is an index for finishing the demanganization operation of high-purity pig iron output by a blast furnace, and the method is used for better meeting the requirement of 4N-grade high-purity iron on ultralow manganese by large-scale fire metallurgy production by combining the oxidation demanganization based on a top-bottom side composite blowing oxidation purification converter and the strong stirring strong oxidation demanganization based on an LF refining furnace (temperature adjustment of molten iron) +ladle bottom-blowing argon top-blowing oxygen installation (namely CAS-OB refining equipment).
The technical scheme of the invention is as follows:
the control method for preparing 4N-grade high-purity iron ultralow manganese by fire purification is characterized by comprising the following steps of: step A, carrying out molten iron pretreatment demanganization on high-purity pig iron output from a blast furnace into a molten iron tank to obtain demanganizing molten iron in a first stage; b, adding the first-stage manganese-removed iron liquid into a top-bottom side composite converting oxidation purification converter for oxidation purification, pouring Mn-removed and P-removed slag out of the iron liquid, adding the iron liquid into the top-bottom side composite converting oxidation purification converter, continuing converting, reducing carbon, heating and the like for other smelting and purification to obtain a second-stage manganese-removed iron liquid; and C, injecting the second-stage demanganizing iron liquid into a ladle of an LF refining furnace, adjusting the temperature of the iron liquid and the alkalinity of top slag in the ladle, and then performing strong-stirring and strong-oxidation demanganizing by utilizing a ladle bottom-blowing argon top-blowing oxygen facility (CAS-OB) to obtain a third-stage demanganizing iron liquid, wherein the third-stage demanganizing iron liquid reaches an ultralow manganese index with the manganese weight percent content of less than or equal to 0.0015.
And (C) the weight percent of manganese in the high-purity pig iron in the step A is less than or equal to 0.05.
The high-purity pig iron molten iron in the step A meets 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, 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 molten iron injection demanganization, the molten iron injection demanganization comprises a molten iron pretreatment oxygen lance and a powder injection stirring gun which are arranged at the top of the molten iron tank, and the molten iron pretreatment oxygen lance blows oxygen to the molten iron liquid level at a distance of 600-1200 mm from the molten iron 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 completed in a reaction mode, the nozzle end of the powder injection stirring gun is inserted into the high-purity pig iron and sprays fluidized lime powder to form demanganizing slag in the stirred molten iron, and the conditions of high demanganizing rate (more than 80 percent) are met as follows: the temperature of the molten iron is less than 1280 ℃, and the alkalinity R=0.45-0.65 of the demanganizing slag.
The manganese-removed molten iron in the first stage reaches the index of Mn% -0.010, and when the index is reached, the manganese-removed slag on the molten iron liquid level is scraped off, and the next working procedure is carried out.
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 part of the furnace body, a top blowing oxygen gun arranged at the top of the furnace body and a re-blowing gun, wherein the re-blowing 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, the Mn removal and P removal slag are poured out from the tapping liquid, the tapping liquid is then added into the top-bottom side combined blowing oxidation purification converter, the blowing is continued for 7-13 min, the carbon reduction and the temperature rise are carried out, and the like for other smelting purification, and the Mn percentage of the second-stage demanganization liquid reaches the index of less than or equal to 0.004.
The top-blown oxygen strength of the top-blown oxygen lance was 3.5Nm 3 And/t.min, wherein the bottom blowing air supply intensity of the bottom blowing gun is 0.15Nm 3 /t.min，Nm 3 Is a standard cubic meter, t is ton, and min is minute.
The ladle top of the LF refining furnace in the step C is provided with a heating electrode capable of being inserted into a top slag layer, the top slag layer is connected with a feed bin through a feeding device, the bottom of the ladle is provided with a bottom argon blowing interface, molten iron is blown with argon and stirred through the bottom argon blowing interface, fluorite and/or active lime is input into the top slag layer through the feed bin and the feeding device so that the slag forming 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 controlled to be 1570-1590 ℃ through electrode heating.
The ladle bottom-blowing argon top-blowing oxygen facility in the step C comprises an impregnating cover and an oxygen blowing gun which are arranged at the top of the ladle, wherein the impregnating cover and the oxygen blowing gun are coaxially arranged, and a bottom-blowing argon interface is arranged at the bottom of the ladle.
The strong stirring and strong oxidation demanganization in the step C comprises the following steps: step C1, hoisting the ladle subjected to temperature adjustment of the molten iron by the LF refining furnace to a CAS-OB processing position; step C2, starting bottom argon blowing through the bottom argon blowing interface, gradually increasing the argon blowing intensity until the slag-free area with the diameter of 800-1000 mm is formed on the surface of molten iron in the steel ladle, lowering the dipping cover, and lowering the oxygen blowing gun to blow oxygen to the surface of the molten iron when the oxygen blowing gun approaches to the surface of the molten iron; step C3, when the mass fraction of free oxygen in the molten iron reaches 600-900 ppm, lifting the dipping cover and the oxygen blowing gun, and increasing the flow of argon blowing of the ladle to 50-100 Nm 3 Stirring the molten iron strongly for 10-25 min; and C4, detecting the manganese content in the molten iron, returning to the step C2 if the Mn percentage in the molten iron is more than 0.0015, stopping demanganizing treatment if the Mn percentage in the molten iron is less than or equal to 0.0015, and removing slag after demanganizing the molten iron, and removing the demanganizing 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 4N-grade high-purity iron ultralow manganese by fire purification, the ultralow manganese is controlled to be divided into three stages, so that the first-stage demanganizing iron liquid, the second-stage demanganizing iron liquid and the third-stage demanganizing iron liquid are respectively obtained, and the demanganizing effect is convenient to implement in a segmented mode. And the pretreatment demanganization, top-bottom side composite blowing oxidation purification demanganization, temperature adjustment and top slag alkalinity adjustment based on an LF refining furnace and strong oxidation and strong stirring demanganization in a ladle based on a ladle bottom blowing argon top blowing oxygen facility are effectively combined, so that the ultralow manganese index control of Mn less than or equal to 0.0015 in the preparation of 4N-grade high-purity iron by the pyrogenic purification is realized.
The invention is characterized in that: (1) the purity of the high-purity iron is 99.97-99.99% (4N). Other impurity elements are removed by pyrometallurgy and 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, not more than 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 molten iron is deeply purified by adopting external refining, so that Mn element in the molten iron can be further removed, and the requirement of 4N-level high-purity iron is met. (3) The related refining equipment facilities are adopted for pyrometallurgy, the Mn removing facilities are reasonably combined according to thermodynamic and kinetic conditions favorable for manganese removal, the thermodynamic and kinetic conditions of molten iron manganese removal are fully exerted, mn element in molten iron is removed to the maximum extent, and the requirement of raw material pure iron on low manganese content products is met. (4) After Mn is removed from molten iron and purified by the method, mn in the molten iron is less than or equal to 0.0015%, and the requirements of high-purity iron and ultra-purity iron raw material products on low-manganese control can be met.
Drawings
FIG. 1 is a schematic diagram of the control method for purifying and preparing 4N-grade high-purity iron by using the fire method to perform oxygen blowing and stirring injection on molten iron to remove manganese. The arrow in fig. 1 indicates the main movement direction of lime powder in molten iron.
FIG. 2 is a schematic diagram of the top-bottom composite converting oxidation purification converter in the control method for preparing 4N-grade high-purity iron ultra-low manganese by fire purification according to the invention.
Fig. 3 is a schematic diagram of iron bath temperature adjustment and top slag alkalinity adjustment in an LF refining Furnace (LF, ladle Furnace, ladle refining Furnace) of a control method for fire purification preparation of 4N grade high purity iron according to the present invention. And (3) performing temperature adjustment and top slag alkalinity adjustment on the molten iron by the LF refining furnace.
FIG. 4 is a schematic diagram of the strong oxidation and strong stirring demanganization of a ladle bottom argon blowing top oxygen blowing facility in the control method for preparing 4N-grade high-purity iron ultralow manganese by performing fire purification. The strong oxidation, strong agitation demanganization in FIG. 4 uses CAS-OB (CAS-OB, composition Adjustment by Sealed Argon Bubbling-Oxygen bubbing), seal argon blowing and Oxygen blowing composition adjustment.
The reference numerals are listed below: 1-a hot-metal ladle; 2-molten iron; 3-liquid level; 4-an oxygen blowing gun for molten iron pretreatment; 5-spraying powder stirring gun; 6-a top and bottom side combined converting oxidation purification converter; 7-a bottom blowing gun; 8-side blowing gun; 9-top blowing gun; 10-compound gun (for temperature measurement, sampling, carbon fixation, oxygen fixation, etc.); 11-ladle; 12-molten iron; 13-air brick; 14-bottom blowing argon interface; 15-oxygen lance blowing; 16-dipping cover; 17-argon bubbling; 20-feeding devices; 21-a storage bin; 22-heating the electrode; 23-top slag.
Detailed Description
The present invention will be described below with reference to examples and drawings (fig. 1 to 4).
FIG. 1 is a schematic diagram of demanganization of molten iron by oxygen blowing and stirring blowing by a control method for preparing 4N-grade high-purity iron ultralow manganese by fire purification of the invention. FIG. 2 is a schematic diagram of the top-bottom composite converting oxidation purification converter in the control method for preparing 4N-grade high-purity iron ultra-low manganese by fire purification according to the invention. Fig. 3 is a schematic diagram of iron bath temperature adjustment and top slag alkalinity adjustment in an LF refining Furnace (LF, ladle Furnace, ladle refining Furnace) of a control method for fire purification preparation of 4N grade high purity iron according to the present invention. FIG. 4 is a schematic diagram of the strong oxidation and strong stirring demanganization of a ladle bottom-blowing argon top-blowing oxygen facility in the control method for preparing 4N-grade high-purity iron and ultra-low manganese by performing fire purification according to the invention. As shown in fig. 1 to 4, the fire purification preparationThe 4N-level high-purity iron ultralow manganese control method comprises the following steps: step A, demanganizing high-purity pig iron (molten iron 2) output from a blast furnace into a molten iron tank 1 by pretreatment of the molten iron in the molten iron tank 1 to obtain a first-stage demanganizing molten iron; b, adding the first-stage manganese-removed iron liquid into a top-bottom side composite converting oxidation purification converter 6 for oxidation purification and demanganization, pouring out Mn-removed and P-removed slag from the iron liquid, and adding the iron liquid into the top-bottom side composite converting oxidation purification converter for other smelting and purification such as carbon reduction, temperature rise and the like to obtain a second-stage manganese-removed iron liquid; and C, injecting the second-stage demanganizing iron liquid into a ladle 11 of an LF refining furnace, adjusting the temperature of the iron liquid and the top slag alkalinity in the ladle 11, and then performing strong stirring and strong oxidation demanganizing by utilizing a top-blowing facility (such as CAS-OB facility, CAS-OB, composition Adjustment by Sealed Argon Bubbling-Oxygen bubbing and sealing argon blowing Oxygen component adjustment) based on ladle bottom blowing argon to obtain a third-stage demanganizing iron liquid, wherein the third-stage demanganizing iron liquid reaches an ultralow manganese index with the manganese weight percent content less than or equal to 0.0015. And (C) the weight percent of manganese in the high-purity pig iron in the step A is less than or equal to 0.05. The high-purity pig iron molten iron in the step A meets 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, 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 molten iron injection demanganization, the molten iron injection demanganization comprises a molten iron pretreatment oxygen lance 4 and a powder injection stirring lance 5 which are arranged at the top of the molten iron tank 1, and the molten iron pretreatment oxygen lance 4 blows oxygen to the molten iron liquid level 3 at a distance of 600-1200 mm from the molten iron liquid level 3 to pass 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 injection stirring gun 5 is inserted into the high-purity pig iron molten iron and sprays fluidized lime powder to form demanganizing slag in the stirred molten iron, and the conditions of high demanganizing rate (more than 80 percent) are met as follows: the temperature of the molten iron is less than 1280 ℃, and the alkalinity R=0.45-0.65 of the demanganizing slag. The manganese-removed molten iron in the first stage reaches the index of Mn% -0.010, and when the index is reached, the manganese-removed slag on the molten iron liquid level is scraped off, and the next working procedure is carried out.
The top-bottom side combined 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 of the furnace body, a top blowing oxygen gun 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 is smelted by adopting a full iron method, the oxygen blowing purification smelting is finished for 8-12 min, the Mn and P removing slag are poured out from the tapping liquid, the tapping liquid is added into the top-bottom side combined blowing oxidation purification converter, the blowing is continued for 7-13 min, the carbon is reduced, the temperature is raised and the like for other smelting purification, and the Mn of the second-stage demanganization iron liquid reaches an index of less than or equal to 0.004%. The top-blown oxygen strength of the top-blown lance was 3.5 (Nm) 3 /t.min), the bottom blowing air supply intensity of the bottom blowing gun is 0.15 (Nm) 3 /t.min), wherein Nm 3 Is marked with cubic meters, and 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 positioned above the liquid level 3), the top slag layer 23 is connected with a feed bin 21 through a feeding device 20, the bottom of the ladle 11 is provided with a bottom argon blowing interface 14 (an air brick 13 can be adopted in the structure), the molten iron 12 is blown with argon through the bottom argon blowing interface 14 to be stirred (argon bubbles 17 are formed in the molten iron 12), fluorite and/or active lime is input into the top slag layer 23 through the feed bin 21 and the feeding device 20 so that the slag 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 22. The ladle bottom-blowing argon top-blowing oxygen facility in the step C comprises an impregnating cover 16 and an oxygen blowing gun 15 which are arranged at the top of the ladle 11, wherein the impregnating cover 16 is sleeved with the oxygen blowing gun 15, the impregnating cover 16 and the oxygen blowing gun 15 are coaxially arranged, and a bottom-blowing argon interface 14 is arranged at the bottom of the ladle 11. The strong stirring and strong oxidation demanganization in the step C comprises the following steps: step C1, hoisting a ladle 11 of the LF refining furnace to a ladle bottom blowing argon top blowing oxygen facility (CAS-OB facility); step C2, beginning to blow argon from the bottom through the bottom argon blowing interface 14, gradually increasing argon blowing intensity to a slag-free area with phi 800-1000 mm on the surface of molten iron in the ladle 11, lowering the dipping cover 16, and lowering the oxygen lance 15 to blow oxygen on the surface of molten iron when approaching to the surface of molten iron; step (a)C3, when the mass fraction of free oxygen in the molten iron 12 reaches 600-900 ppm, lifting the dipping cover 16 and the oxygen lance 15, and increasing the argon blowing flow of the ladle to 50-100 Nm 3 Stirring the molten iron 12 strongly for 10-25 min (argon bubbles 17 are formed in the molten iron 12); and C4, detecting the manganese content in the molten iron 12, returning to the step C2 if the Mn content in the molten iron is more than 0.0015%, stopping the manganese removal treatment if the Mn content in the molten iron 12 is less than or equal to 0.0015%, and completing the manganese removal of the molten iron and slag removal operation, and removing the molten iron demanganizing top slag in the ladle 11.
The deep demanganization method of molten iron comprises the following steps:
(1) the process route of deep demanganization of molten iron (preparation of 4N-grade high-purity iron by combined fire purification) comprises the following steps: the method comprises the steps of (1) blast Furnace high-purity pig iron-iron pretreatment desulfurization-iron pretreatment desilication demanganization-top and bottom side composite blowing oxidation purification converter desilication, manganese, phosphorus, carbon and the like-RH (Ruhrstahl-Heraeus-Vacuum degaussing), LF (Ladle Furnace, ladle refining Furnace) to CASOB (Composition Adjustment by Sealed Argon Bubbling-Oxygen bubbing), sealing argon blowing Oxygen component adjustment), ladle (refining Ladle) deslagging and completing preparation of ultralow manganese iron liquid.
(2) The blast furnace produces high purity pig iron. Raw fuel fed into the blast furnace is carefully selected, reasonably blended, and the manganese in the high-purity pig iron is strictly controlled, wherein the Mn content in the molten iron is less than or equal to 0.05. The high-purity pig iron 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, 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) Mn is removed by pretreatment of molten iron. In a ladle (also called a ladle), top-blown oxygen and blowing flow slaked lime powder are adopted for stirring, mn slag is scraped off after the stirring is finished, and preliminary removal of Mn in molten iron is completed: mn+o2=mno2. The Mn in molten iron (also called as molten iron) can be controlled to be less than or equal to 0.010 percent, and the conditions of high demanganization rate (more than 80 percent) are as follows: the temperature of molten iron is less than 1280 ℃, and the alkalinity is controlled to be R=0.45-0.65.
(4) Adding the pretreated molten iron into a top-bottom side composite blowing oxidation purification converter for purification smelting, wherein the top-bottom side composite blowing oxidation purification converter is a multifunctional multipoint oxygen blowing furnace, and the top-blowing oxygen supply strength is 3.5Nm 3 T.min, bottom blowing air supply strengthDegree of 0.15Nm 3 And/t.min. Adding iron by a full iron method, purifying and smelting for 8-12 min, pouring out Mn-removed and P-removed slag from the tapping liquid, and adding the tapping liquid into a top-bottom side composite blowing oxidation purification converter for other smelting and purification. The process can purify the manganese in the molten iron to Mn less than or equal to 0.004 percent.
(5) LF furnace+CAS-OB deep Mn removal. And the LF furnace carries out temperature adjustment and slag tapping degree reduction adjustment on molten iron. After the molten iron subjected to the manganese removal by the top-bottom side composite blowing oxidation purification converter through a duplex method enters a refining ladle (namely a ladle), temperature adjustment and top slag alkalinity adjustment are carried out at an LF furnace working site, 300-1000 kg of active lime and 50-300 kg of fluorite (according to the usual ladle molten iron capacity) are added, the slag thickness is 150-200 mm, the molten iron is properly heated by using electrode slag, when slag melting is completed, the alkalinity R of top slag is 1.6-2.5, and the molten iron temperature is 1570-1590 ℃, the working procedure is considered to be completed.
CAS-OB deep demanganization. The refining package is lifted to CAS-OB deep demanganization position. The manganese oxide of the manganese oxide is alkaline, the alkalinity of top slag is moderate in the process of removing the manganese by oxidation, low alkalinity and good fluidity are required, and in addition, the equilibrium constant k of the reaction of Mn element and ferric oxide is reduced along with the rise of temperature, so that the proper reduction of the temperature is beneficial to the oxidation removal of the manganese. In the CAS-OB station treatment process, the strength of bottom blowing argon is properly increased, when the slag-free area with the diameter of 800-1000 mm is formed on the surface of the refining ladle iron liquid, the dipping cover is lowered, the oxygen blowing gun is lowered to blow oxygen to the iron liquid, when the free oxygen amount in the iron liquid reaches 600-900 ppm, the dipping cover and the oxygen blowing gun are lifted, the flow of the bottom blowing argon of the refining ladle is increased, the iron liquid is strongly stirred for 10-25 min, and the flow of the bottom blowing argon is 50-100 Nm 3 /h。
When the Mn content in the molten iron is removed to be less than or equal to 0.0015 percent, the manganese removal requirement is met, the treatment is stopped, and the manganese removal of the molten iron is completed. Otherwise, repeating the above operation until the demanganization reaches the required target component.
After the demanganization and purification of the molten iron are completed, slag removal operation is carried out on the molten iron, namely, the base liquid demanganization top slag in the refining ladle is removed.
(6) The method is used for removing manganese from the molten iron, and the manganese removal effect reaches Mn less than or equal to 0.0015 percent.
The invention discloses a method for deeply removing and purifying manganese from molten iron, which comprises the following steps: the device comprises a molten iron pretreatment blowing Mn and P removing facility, a top and bottom side combined blowing oxidation and purification converter, an LF refining facility and a CAS-OB oxygen blowing argon blowing refining facility. Wherein, the Mn and P removing facilities (shown in figure 1) of the molten iron pretreatment injection have desilication, mn and P removing functions; the top and bottom side combined converting oxidation purification converter (shown in figure 2) has the characteristic of multi-point strong oxidation, and can oxidize and remove all various impurity elements easy to oxidize; the LF refining facility (or LF refining furnace as shown in figure 3) adjusts the temperature of molten iron to 1570-1590 ℃ and the top slag alkalinity to R=1.6-2.5; the primary effect of CAS-OB oxygen blowing argon blowing refining facilities (as in fig. 4) on demanganization is oxygen blowing strong oxidation and strong agitation.
The invention relates to a new method for continuously demanganizing molten iron by a single-furnace duplex method through a top-bottom side composite converting oxidation purification converter after molten iron pretreatment demanganizing and slag skimming, and then deeply demanganizing through an LF refining furnace and a CAS-OB refining facility, which can be characterized by comprising the following steps:
(1) the refining process carries out deep demanganization operation in the refining ladle, can fully realize thermodynamic and kinetic conditions of demanganization, and achieves the aim of demanganization and purification of molten iron to the maximum extent.
(2) The demanganization treatment time is sufficient, and the demanganization purification time of the molten iron is 10-40 min, so that the demanganization oxidation reaction tends to be balanced.
(3) And (3) adopting an LF refining furnace to remove slag, so as 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 molten iron, so that the molten iron temperature is ensured to carry out demanganization and purification operation at a lower temperature, and Mn is easily oxidized and removed.
(4) The introduction of CAS-OB is one of the most effective refining facilities for removing manganese, is very flexible in the process of removing manganese, can realize large-volume stirring, increases the dynamic condition of removing manganese, can also perform oxygen blowing operation on molten iron, improves the oxidizing property of the molten iron and quickens the rapid progress of the manganese removal reaction. The CAS-OB is adopted to blow oxygen to the molten iron, so that the pollution to the molten iron caused by adding other oxides (such as ferric oxide and the like) is eliminated while the oxygen content in the molten iron is increased.
(5) The LF refining furnace and CAS-OB refining facilities are combined to perform deep demanganization refining treatment on the molten iron, so that the favorable conditions of demanganization can be fully developed: low alkalinity, low temperature, high oxidability, large slag amount and strong stirring. Realizes the deep demanganization and purification of the molten iron in the refining process.
(6) Realizes that Mn in the molten iron is less than or equal to 0.0015 percent.
What is not described in detail in this specification is prior art known to those skilled in the art. It is noted that the above description is helpful for a person skilled in the art to understand the present invention, but does not limit the scope of the present invention. Any and all such equivalent substitutions, modifications and/or deletions as may be made without departing from the spirit and scope of the invention.
Claims (1)
1. The control method for preparing 4N-grade high-purity iron ultralow manganese by fire purification is characterized by comprising the following steps of: step A, demanganizing high-purity pig iron molten iron output from a blast furnace into a molten iron tank by adopting molten iron pretreatment in the molten iron tank to obtain demanganizing molten iron in a first stage; b, adding the first-stage demanganized iron liquid into a top-bottom side composite converting oxidation purification converter for oxidation purification, pouring Mn-removing and P-removing slag out of the iron liquid, and adding the iron liquid into the top-bottom side composite converting oxidation purification converter for carbon reduction and heating smelting purification to obtain a second-stage demanganized iron liquid; c, injecting the second-stage demanganizing iron liquid into a ladle of an LF refining furnace, adjusting the temperature of the iron liquid and the alkalinity of top slag in the ladle, and then performing strong-stirring and strong-oxidation demanganizing by utilizing a ladle bottom-blowing argon top-blowing oxygen facility to obtain a third-stage demanganizing iron liquid, wherein the third-stage demanganizing iron liquid reaches an ultralow manganese index with Mn less than or equal to 0.0015 in weight percent;
the weight percent of manganese in the high-purity pig iron molten iron in the step A is less than or equal to 0.05;
the high-purity pig iron molten iron in the step A meets 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, 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 molten iron injection demanganization, the molten iron injection demanganization comprises a molten iron pretreatment oxygen lance and a powder injection stirring gun which are arranged at the top of the molten iron tank, and the molten iron pretreatment oxygen lance blows oxygen to the molten iron liquid level at a distance of 600-1200 mm from the molten iron pretreatment oxygen lance to the molten iron 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 completed in a reaction mode, the nozzle end of the powder spraying stirring gun is inserted into the high-purity pig iron, and fluidized lime powder is sprayed to form demanganizing slag in the stirred molten iron, so that the conditions of high demanganizing rate of more than 80% are met as follows: the temperature of the molten iron is less than 1280 ℃, and the alkalinity R of the demanganizing slag is between 0.45 and 0.65;
the first-stage demanganization molten iron reaches the index of Mn% -0.05, demanganization slag on the molten iron liquid surface is scraped off, and the next procedure is carried out;
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 part of the furnace body, a top blowing oxygen gun and a sublance arranged at the top of the furnace body, wherein the sublance 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, the Mn removal and P removal slag of the tapping liquid are poured out, the tapping liquid is added into the top-bottom side combined blowing oxidation purification converter for smelting and purifying with the temperature rise of the carbon reduction, and the Mn removal liquid in the second stage reaches the index of less than or equal to 0.004;
the top-blown oxygen strength of the top-blown oxygen lance was 3.5Nm 3 And/t.min, wherein the bottom blowing air supply intensity of the bottom blowing gun is 0.15Nm 3 T.min, where Nm 3 The standard cubic meter is represented, t is represented by ton, and min is min;
the top of a ladle of the LF refining furnace in the step C is provided with a heating electrode inserted into a top slag layer, the top slag layer is connected with a feed bin through a feeding device, the bottom of the ladle is provided with a bottom argon blowing interface, argon is blown to molten iron through the bottom argon blowing interface for stirring, fluorite and/or active lime is input into the top slag layer through the feed bin and the feeding device so that the slag forming 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;
the ladle bottom argon blowing top oxygen blowing facility in the step C comprises an immersion cover and an oxygen blowing gun which are arranged at the top of the ladle, wherein the immersion cover is sleeved with the oxygen blowing gun, the immersion cover and the oxygen blowing gun are coaxially arranged, and a bottom argon blowing interface is arranged at the bottom of the ladle;
the strong stirring and strong oxidation demanganization in the step C comprises the following steps: step C1, hoisting the ladle of the LF refining furnace to a ladle bottom-blowing argon top-blowing oxygen facility; step C2, starting bottom argon blowing through the bottom argon blowing interface, gradually increasing argon blowing intensity until the slag-free area with phi of 800-1000 mm is formed on the surface of molten iron in the steel ladle, lowering the dipping cover, and lowering the oxygen blowing gun to blow oxygen to the surface of the molten iron when the oxygen blowing gun approaches to the surface of the molten iron; step C3, when the mass fraction of free oxygen in the molten iron reaches 600-900 ppm, lifting the dipping cover and the oxygen blowing gun, and increasing the argon blowing flow of the ladle to 50-100 Nm 3 Stirring the molten iron strongly for 10-25 min; and C4, detecting the manganese content in the molten iron, returning to the step C2 if the Mn percentage in the molten iron is more than 0.0015, stopping the manganese removal treatment if the Mn percentage 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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