CN110592460B - Steelmaking method of non-oriented silicon steel - Google Patents
Steelmaking method of non-oriented silicon steel Download PDFInfo
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- 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
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/064—Dephosphorising; Desulfurising
- C21C7/0645—Agents used for dephosphorising or desulfurising
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- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/10—Handling in a vacuum
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C33/04—Making ferrous alloys by melting
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/004—Very low carbon steels, i.e. having a carbon content of less than 0,01%
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/008—Ferrous alloys, e.g. steel alloys containing tin
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/02—Ferrous alloys, e.g. steel alloys containing silicon
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/04—Ferrous alloys, e.g. steel alloys containing manganese
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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Abstract
The invention discloses a steelmaking method of non-oriented silicon steel, which comprises the following steps: drying waste electrotinning mud generated by an electrotinning production line to prepare tin mud powder; the molten iron desulphurization station adopts the combined blowing and stirring of the tin sludge powder and the desulfurizer to carry out desulphurization operation; after molten iron is desulfurized, smelting the non-oriented silicon steel through the working procedures of converter steelmaking, RH vacuum refining, continuous casting and the like; the main components of the tin mud powder prepared by drying the electroplated tin mud are as follows: c: 0% -2%, S: 0% -1.5% of SiO2：0％‑0.2％，SnO2：93％‑97％，Fe2O3：0％‑3％，P2O5: 0% -0.2%; the finished product of the Sn-containing non-oriented silicon steel comprises the following chemical components: less than or equal to 0.005 percent of C, less than or equal to 3.5 percent of Si, less than or equal to 2.0 percent of Mn, less than or equal to 1.0 percent of Al, less than or equal to 0.05 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.01 percent of Sn, less than or equal to 0.05 percent of Sn, and the balance of Fe and inevitable impurity elements. The invention utilizes the tinned mud to dry and prepare the tinned mud powder for smelting the non-oriented silicon steel, thereby reducing goldBelongs to the consumption of tin ingots, simultaneously realizes the recovery and the effective utilization of the electrotinning mud, reduces the production cost and reduces the environmental pollution.
Description
Technical Field
The invention relates to the technical field of non-oriented silicon steel making, in particular to a method for smelting non-oriented silicon steel by using tinned mud instead of pure tin ingots.
Background
Melting point of Sn: 231.89 ℃, boiling point: 2260 ℃ is a low-melting-point metal with silvery white metallic luster, pure tin is soft, the ductility is good at normal temperature, the chemical property is stable, and the metal is not easy to oxidize. The metal Sn has wide application, the tin is plated on the surface of other products by using an electroplating process, and the main component of the electroplating solution is Sn (OH) in the production process of the electroplating tin4If the foreign matters are not filtered and removed, the foreign matters can be adhered to the electroplated tin plate to form 'tin ash' defects. Therefore, the filtering systems are arranged on the electrotinning wires for filtering the electroplating solution to obtain electrotinning mud. The recovery of the prior electrotinning sludge generally needs to be processed by professional institutions, the main recovery mode is to fully soak and filter the electrotinning sludge in an acid solution to obtain electrotinning sludge, separate the stanniferous sludge from the electrotinning sludge, adjust the pH value of the solution to precipitate a tin compound, separate and recover the precipitated tin compound, finally dissolve the tin compound obtained by separation in an alkaline solution, and obtain metallic tin after the alkaline solution is electrolyzed. The recovery process of the electrotinning sludge is complicated, the production flow is long, the pH value of the solution needs to be continuously adjusted in the recovery process, certain waste liquid is generated, the environmental pollution is caused, and the production cost is higher.
Sn is an interface active element and is easy to be segregated near the grain boundary. Due to the characteristic, when the non-oriented silicon steel is smelted, a small amount of Sn element is added, so that the recrystallization texture of the non-oriented silicon steel after final annealing can be obviously improved, the {100} favorable texture component is increased, the {111} unfavorable texture component is reduced, and the magnetic induction intensity is improved. The addition of Sn element can also inhibit the formation of an internal oxidation layer and a nitriding layer, thereby improving the magnetic performance of the non-oriented silicon steel. At present, Sn-containing non-oriented silicon steel is smelted by mainly adding pure tin ingots to meet the requirement of adding tin elements.
At present, the requirement of environmental protection in the steel industry is pressing day by day, and the problem of rationally recycling and utilizing the waste materials in the steel production process becomes urgent to be solved. For enterprises having electrotinning production lines and producing silicon steel at the same time, if electrotinning mud can be used for replacing a pure tin ingot to produce Sn-containing high-performance non-oriented silicon steel, the production cost can be reduced, and meanwhile, the problem of electrotinning production waste can be solved. However, no relevant research is published at present.
Disclosure of Invention
In view of the above, the present invention provides a method for smelting non-oriented silicon steel using tin sludge instead of pure tin ingots.
The technical scheme of the invention is as follows: drying the waste electroplating tin mud generated in the electroplating tin production line, wherein the main component is Sn (OH)4The electrolytic tinning mud undergoes a chemical decomposition reaction: sn (OH)4＝SnO2+2H2O, evaporating water to obtain SnO as main component2The tin paste powder of (1); calculating the addition of metallic tin according to the component requirements of the steel-making finished product, and then according to SnO in the tin sludge powder2Content of (C) and SnO2Calculating the addition amount of the tin sludge powder according to the yield of the converted metal tin; the molten iron desulphurization station carries out desulphurization operation by adopting quantitative tin sludge powder and desulfurizer to jointly blow and stir, and then most of tin oxide in the tin sludge powder reacts with carbon in the molten iron, SnO2+2C ═ Sn +2CO and 2SnO + C ═ 2Sn + CO2To form metallic tin, unreacted SnO2Floating together with other impurities and the desulfurized slag to the surface of the molten iron, and removing the impurities by skimming; after molten iron is desulfurized, the Sn-containing non-oriented silicon is finished through the working procedures of converter steelmaking, RH vacuum refining, continuous casting and the likeAnd smelting the steel, wherein pure tin ingots can be supplemented in a proper amount according to component detection results during vacuum refining.
The process comprises the following steps:
(1) and (3) drying the electroplated tin mud to prepare tin mud powder: taking the electroplated tin mud out of a tin mud filter of an electroplating production line, and drying and pulverizing the electroplated tin mud;
(2) molten iron desulphurization pretreatment: carrying out desulfurization operation by jointly blowing and stirring quantitative tin sludge powder and a desulfurizing agent, wherein S is less than or equal to 20ppm after molten iron is desulfurized, the slagging rate is more than or equal to 98 percent, and the temperature is more than or equal to 1320 ℃;
(3) smelting in a converter: carrying out top-bottom combined blowing of the converter, wherein the end point of the converter is controlled to be 0.03-0.045% of C, 0.05-0.08% of free oxygen of molten steel, less than or equal to 0.004% of S, and the tapping temperature of the converter is 1660-1700 ℃; opening a ladle bottom argon blowing control valve before converter tapping, controlling the ladle bottom argon blowing pressure to be 0.5-1.0 MPa, and adjusting the ladle bottom argon blowing pressure to be 0.4-0.8 MPa after the tapping amount reaches 3/4; adding lime according to the proportion of 1.1-1.2 kg/t when the converter steel output is about 1/6, and adding a slag surface deoxidizer after steel output; sampling and carrying out component detection;
(4) RH vacuum refining: a decarburization treatment mode is adopted, after vacuum decarburization is carried out for 15-25 min, alloying is carried out according to the component requirements in the sequence of aluminum block → ultra-low titanium ferrosilicon → low titanium ferrophosphorus → metal manganese → tin ingot; after alloying is completed for 3-6 min, taking the steel sample for component inspection, and continuously adjusting chemical components according to component inspection results; after the chemical components are adjusted, carrying out net circulation for 5-10 min;
(5) and (4) continuous casting.
Preferably, the tin mud powder added in the molten iron desulphurization process is prepared by drying the electroplated tin mud, the drying temperature is 350-400 ℃, and the drying time is more than or equal to 60 min; the tin mud powder comprises the following main components: c: 0% -2%, S: 0% -1.5% of SiO2：0％-0.2％，SnO2：93％-97％，Fe2O3：0％-3％，P2O5：0％-0.2％。
Preferably, the molten iron comprises the following components: c: 4.0% -5.0%, S: 0% -0.07%, Si: 0% -0.7%, Ti: 0% -0.15%, Mn: 0% -0.2%, P: 0 to 0.2 percent of the total weight of the alloy, and the balance of Fe and inevitable impurity elements; the arrival temperature of the molten iron is more than or equal to 1350 ℃.
Preferably, the molten iron desulfurization station performs desulfurization operation by jointly blowing quantitative tin sludge powder and desulfurizer and stirring, and then part of SnO in C and tin sludge powder in molten iron2React at high temperature to form Sn, CO and CO metals2Unreacted SnO2Floating together with other impurities and the desulfurized slag to the surface of the molten iron, and removing the impurities by skimming; the yield of the metal Sn in the tin mud powder is more than or equal to 73 percent.
Preferably, the finished product of the non-oriented silicon steel comprises the following chemical components in percentage by weight: less than or equal to 0.005 percent of C, less than or equal to 3.5 percent of Si, less than or equal to 2.0 percent of Mn, less than or equal to 1.0 percent of Al, less than or equal to 0.05 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.01 percent of Sn, less than or equal to 0.05 percent of Sn, and the balance of Fe and inevitable impurity elements.
The invention has the following technical effects or advantages:
the invention treats the electrotinning sludge according to the process that the drying temperature is 350-2When molten iron containing Sn non-oriented silicon steel is desulfurized, molten iron conditions and process conditions during molten iron desulphurization are fully utilized, quantitative tin sludge powder and a desulfurizing agent are jointly blown and stirred, and SnO is realized while desulphurization operation is carried out2To obtain metal Sn; the method can realize the treatment of the waste electrotinning mud in the electrotinning workshop, reduce the environmental pollution caused in the traditional recovery process of the electrotinning mud, reduce the treatment cost of the electrotinning mud, change waste into valuable, save the consumption of pure tin ingots in the production of Sn-containing non-oriented silicon steel and reduce the steel-making cost of the silicon steel; meanwhile, the method is simple in process and easy to operate.
Detailed Description
The present invention is described in further detail below with reference to examples, which are only a part of the present invention.
Comparative example:
the smelting non-oriented silicon steel comprises the following target components: c is less than or equal to 0.005%, Si: 1.6%, Al: 0.30%, Mn: 0.25%, P: 0.04%, S is less than or equal to 0.005%, Sn: 0.025%, and the balance of Fe and inevitable impurity elements.
The process flow comprises molten iron desulphurization, 180-ton converter steelmaking, RH vacuum refining and continuous casting, and the specific process flow comprises the following steps:
(1) molten iron desulphurization: the molten iron comprises the following components: 4.73%, S: 0.038%, Si: 0.38%, Ti: 0.055%, Mn: 0.14%, P: 0.099%, the balance being Fe and unavoidable impurity elements; the arrival temperature of the molten iron is 1356 ℃; a desulfurization station with a good stirring head is selected, desulfurization is carried out by blowing a desulfurizing agent and stirring, the S content is less than or equal to 0.002 percent after molten iron desulfurization treatment, and the slagging rate is more than or equal to 98 percent; the molten iron outlet temperature is 1328 ℃;
(2) converter steelmaking: performing converter oxygen blowing smelting, wherein the end point of the converter is controlled to be 0.03-0.045% of C, less than or equal to 750ppm of O and less than or equal to 40ppm of S; opening a ladle bottom argon blowing control valve before converter tapping, wherein the ladle bottom argon blowing pressure is 0.8MPa, and after the tapping amount reaches 3/4, the ladle bottom argon blowing pressure is adjusted to 0.6 MPa; when the converter steel output is about 1/6, adding 200kg of lime, adding a slag surface deoxidant after steel output, and uniformly spreading a deoxidizer on the slag surface; the tapping temperature of the converter is 1686 ℃. After tapping is finished, sampling and carrying out component detection, wherein the components are as follows: 0.0325%, Si: 0.0030%, Mn: 0.045%, P: 0.0086%, S: 0.0032%, Al: 0.002%, Ti: 0.0005%;
(3) RH vacuum refining: and (3) adopting a decarburization treatment mode, starting to add alloy after vacuumizing for 20 minutes, then alloying according to the sequence of an aluminum block, ultra-low titanium silicon iron, low titanium ferrophosphorus, metal manganese and 45kg of pure tin ingot, wherein the vacuum degree is 1.9mBar, degassing is carried out for 12 minutes, and the net cycle time after alloying is 7 minutes. The RH tapping temperature is 1589 ℃.
(4) Continuous casting: casting into 220 x 1250mm continuous casting billet according to the size requirement of the finished product.
Through tests, the casting blank comprises the following chemical components: c: 0.0029%, Si: 1.58%, Al: 0.29%, Mn: 0.22 percent; p: 0.043%, S: 0.0036%, Sn: 0.024%, and the balance of Fe and inevitable impurity elements. The yield of metallic Sn was 96%.
Example 1:
the smelting non-oriented silicon steel comprises the following target components: c is less than or equal to 0.005%, Si: 1.6%, Al: 0.30%, Mn: 0.25%, P: 0.04%, S is less than or equal to 0.005%, Sn: 0.025%, and the balance of Fe and inevitable impurity elements.
The process flow comprises the following steps of preparing tin sludge powder, desulfurizing molten iron, steelmaking by a 180-ton converter, RH vacuum refining and continuous casting, and the specific process flow is as follows:
(1) and (3) drying the electroplated tin mud to prepare tin mud powder: taking the electroplated tin mud out of the tin mud filter of the electroplating production line, and drying at the drying temperature of 350-400 ℃ for more than or equal to 60 min; the obtained stannum mud powder comprises the following components: c: 1.52%, S: 0.51% of SiO2：0.0068％，SnO2：95.82％，Fe2O3：2.09％，P2O5：0.046％；
(2) Molten iron desulphurization pretreatment: 45kg of metallic tin is required, calculated as 0.025% of Sn target component in 180 tons of molten steel. The atomic weight of tin is 118.71, the atomic weight of oxygen is 15.99, and SnO is required by calculation2Total 57.1 kg. SnO2The yield of Sn is 80%, and SnO is required271.4kg in total, SnO in the tin mud powder2The content of the tin paste powder is 95.82 percent, so that 74.5kg of tin paste powder needs to be added. The molten iron comprises the following components: 4.30%, S: 0.023%, Si: 0.48%, Ti: 0.065%, Mn: 0.12%, P: 0.091%, the balance being Fe and unavoidable impurity elements; the arrival temperature of the molten iron is 1358 ℃; a desulfurization station with a good stirring head is selected, 74.5kg of tin mud powder and a desulfurizer are jointly blown and stirred for desulfurization operation, S is less than or equal to 20ppm after molten iron desulfurization, and the slagging rate is more than or equal to 98%; the molten iron outlet temperature is 1325 ℃;
(3) converter steelmaking: performing oxygen blowing smelting in a converter, wherein the end point of the converter is controlled to be 0.03-0.045% C, less than or equal to 750ppm O and less than or equal to 40ppm S: opening a ladle bottom argon blowing control valve before converter tapping, wherein the ladle bottom argon blowing pressure is 0.8MPa, and after the tapping amount reaches 3/4, the ladle bottom argon blowing pressure is adjusted to 0.6 MPa; when the converter steel output is about 1/6, adding 200kg of lime, adding a slag surface deoxidant after steel output, and uniformly spreading a deoxidizer on the slag surface; the tapping temperature of the converter is 1684 ℃. After tapping, sampling and detecting components, wherein the components comprise 0.036% of C, and Si: 0.001%, Mn: 0.049%, P: 0.0134%, S: 0.0026%, Al: 0.005%, Ti: 0.0005%, Sn: 0.027%;
(4) RH vacuum refining: and (3) adopting a decarburization treatment mode, starting to add alloy after vacuumizing for 20 minutes, alloying according to the sequence of aluminum blocks, ultra-low titanium silicon iron, low titanium ferrophosphorus and metal manganese without adding pure tin ingots according to the composition result of the converter, wherein the vacuum degree is 1.8mBar, degassing is carried out for 12 minutes, and the net cycle time after alloying is 7 minutes. The RH tapping temperature is 1586 ℃.
(5) Continuous casting: casting into 220 x 1250mm continuous casting billet according to the size requirement of the finished product.
Through tests, the casting blank comprises the following chemical components: c: 0.0025%, Si: 1.56%, Al: 0.28%, Mn: 0.24 percent; p: 0.040%, S: 0.0031%, Sn: 0.026%, and Fe and inevitable impurity elements as the rest. SnO when adding tin sludge powder2The yield of converted Sn is calculated by 80%, the target Sn is 0.025%, and the actual Sn is 0.026%, so SnO2The yield of converted Sn was 83.2%.
TABLE 1 comparison of chemical compositions
As can be seen from Table 1, compared with the Sn-containing non-oriented silicon steel smelting by vacuum refining and adding pure tin ingots, the non-oriented silicon steel obtained by smelting by the method of the invention has approximate components and obtains expected effects.
The method has the advantages that the non-oriented silicon steel is smelted by using the electrotinning sludge, compared with the traditional process, the recovery and the effective utilization of the electrotinning sludge are realized, the process is simple and easy to operate, the purchasing cost of tin ingots required in the process of converter steelmaking production is reduced, and the environmental pollution caused in the traditional electrotinning sludge recovery process is also reduced.
While embodiments of the present invention have been described, variations and modifications of those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, modifications, adaptations, variations, and the like based on the principles and spirit of the present invention should be included in the scope of the present invention.
Claims (3)
1. A method of making steel from non-oriented silicon steel, the method comprising: drying waste electrotinning mud generated by an electrotinning production line to prepare stannum mud powder; the molten iron desulphurization station adopts the combined blowing and stirring of the tin sludge powder and the desulfurizer to carry out desulphurization operation; after molten iron is desulfurized, smelting of the non-oriented silicon steel is completed through the working procedures of converter steelmaking, RH vacuum refining and continuous casting, and the process flow is as follows:
(1) and (3) drying the electroplated tin mud to prepare tin mud powder: taking the electrotinning sludge out of a tin sludge filter of an electrotinning production line, and drying and pulverizing the electrotinning sludge;
(2) molten iron desulphurization pretreatment: carrying out desulfurization operation by adopting combined blowing and stirring of the tin sludge powder and the desulfurizer, wherein S is less than or equal to 20ppm after molten iron is desulfurized, the slagging rate is more than or equal to 98 percent, and the temperature is more than or equal to 1320 ℃; the molten iron before desulfurization comprises the following components: c: 4.0% -5.0%, S: 0% -0.07%, Si: 0% -0.7%, Ti: 0% -0.15%, Mn: 0% -0.2%, P: 0 to 0.2 percent of the total weight of the alloy, and the balance of Fe and inevitable impurity elements; the arrival temperature of the molten iron is equal to or more than 1350 ℃;
(3) smelting in a converter: carrying out top-bottom combined blowing of the converter, wherein the end point of the converter is controlled to be 0.030-0.045% of C, 0.05-0.08% of free oxygen of molten steel, less than or equal to 0.004% of S, and the tapping temperature of the converter is 1660-1700 ℃; opening a ladle bottom argon blowing control valve before converter tapping, controlling the ladle bottom argon blowing pressure to be 0.5-1.0 MPa, and adjusting the ladle bottom argon blowing pressure to be 0.4-0.8 MPa after the tapping amount reaches 3/4; adding lime according to the proportion of 1.1-1.2 kg/t when the converter steel output is 1/6, and adding a slag surface deoxidizer after steel output; sampling and carrying out component detection;
(4) RH vacuum refining: a decarburization treatment mode is adopted, after vacuum decarburization is carried out for 15-25 min, alloying is carried out according to the component requirements in the sequence of aluminum block → ultra-low titanium ferrosilicon → low titanium ferrophosphorus → metal manganese → tin ingot; after alloying is completed for 3-6 min, taking the steel sample for component inspection, and continuously adjusting chemical components according to component inspection results; after the chemical components are adjusted, carrying out net circulation for 5-10 min;
(5) continuous casting;
the finished product of the non-oriented silicon steel comprises the following chemical components: less than or equal to 0.005 percent of C, less than or equal to 3.5 percent of Si, less than or equal to 2.0 percent of Mn, less than or equal to 1.0 percent of Al, less than or equal to 0.05 percent of P, less than or equal to 0.005 percent of S, less than or equal to 0.01 percent of Sn, less than or equal to 0.05 percent of Sn, and the balance of Fe and inevitable impurity elements.
2. As set forth in claim 1The steelmaking method of the non-oriented silicon steel is characterized by comprising the following steps: the tin mud powder added in the molten iron desulphurization process is prepared by drying the electroplated tin mud, the drying temperature is 350-400 ℃, and the drying time is more than or equal to 60 min; the tin mud powder comprises the following main components: c: 0% -2%, S: 0% -1.5% of SiO2：0％-0.2％，SnO2：93％-97％，Fe2O3：0％-3％，P2O5：0％-0.2％。
3. A method of making steel from non-oriented silicon steel as claimed in claim 1, wherein: the molten iron desulphurization station carries out desulphurization operation by adopting combined blowing and stirring of the tin sludge powder and the desulfurizer, and the yield of metal Sn in the tin sludge powder is more than or equal to 73 percent.
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