CN110205432B - Method for producing iron-sulfur alloy - Google Patents
Method for producing iron-sulfur alloy Download PDFInfo
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- CN110205432B CN110205432B CN201910404491.9A CN201910404491A CN110205432B CN 110205432 B CN110205432 B CN 110205432B CN 201910404491 A CN201910404491 A CN 201910404491A CN 110205432 B CN110205432 B CN 110205432B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/0006—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
- C21B13/14—Multi-stage processes processes carried out in different vessels or furnaces
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/002—Ferrous alloys, e.g. steel alloys containing In, Mg, or other elements not provided for in one single group C22C38/001 - C22C38/60
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/16—Ferrous alloys, e.g. steel alloys containing copper
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Abstract
The invention relates to a method for producing iron-sulfur alloy, belonging to the technical field of nonferrous metallurgy. Blowing slag, pyrite and a coal-based reducing agent produced in the copper matte blowing process are sent into a side-blown depletion converter, and a section of weak reduction smelting is carried out at the temperature of 1150-1300 ℃, and after the weak reduction smelting is finished, slag is discharged to obtain a Fe-S-O melt in which the copper matte is dissolved; and carrying out two-stage strong reduction smelting on the obtained Fe-S-O melt dissolved with the copper matte at the temperature of 1150-1300 ℃ to prepare the iron-sulfur alloy. The iron-sulfur alloy prepared by the invention is Fe-FeS alloy, the blowing hot slag is used as a main raw material to produce the iron-sulfur alloy, nonferrous metals and ferrous metals in the blowing slag are comprehensively recovered, the energy consumption is low, and the processing cost of the alloy is low.
Description
Technical Field
The invention relates to a method for producing iron-sulfur alloy, belonging to the technical field of nonferrous metallurgy.
Background
(1) Accretion formation and elimination
The essence of the copper smelting process using copper sulfide ore as raw material is to raise the oxygen potential step by step and lower the sulfur potential to remove gangue, iron and sulfur, and to prepare blister copper. The development trend of modern copper metallurgy is oxygen-enriched intensified smelting, and because the oxygen potential of the system is high, the smelting strength is high, and the copper matte grade is high, in the process of separating the iron element in the furnace burden in the form of iron-making olivine slag, FeO is oxidized into Fe3O4The reaction of (A) inevitably occurs, Fe3O4The melting point of (1597 ℃) is high, and the slag exists in a Fe-O complex ion state, and when the amount of the Fe-O complex ion is large, the melting point of the slag is increased, the specific gravity is increased, and the settling separation of the slag and the matte is deteriorated. When the smelting slag is sent into a settling electric furnace, Fe in the melt3O4Partial precipitates are precipitated at the bottom of the furnace to form a furnace knot, the composition of the furnace knot contains magnesia-chromite spinel and oxides of copper nickel cobalt, and the nickel cobalt is dissolved in the magnetic iron oxide in an atom substitution mode.
The thickness of the furnace junction of the electric settling furnace is maintained between 200mm and 300mm, which is beneficial to protecting the furnace bottom. If the accretion of the furnace is thickened, the effective volume of the electric furnace can be reduced, and a matte discharging port can be blocked, so that the normal operation of the settling electric furnace is damaged. The traditional method for eliminating accretion by using reduction-vulcanization technology is to add one or more of pyrite, high-quality copper concentrate, pig iron, ferrosilicon, silicon carbide, coke, coal, oil reducing agent, natural gas and acidic or alkaline flux into the molten pool, and the adding mode includes top scattering, chute carrying along with smelting slag and spray gun inserting into the molten pool to spray. These methods have obvious drawbacks, limited by the structure of the precipitation furnace and by the physico-chemical properties of the additions:
the pig iron and the ferrosilicon with high specific gravity can pass through the slag layer and the molten matte layer to sink to the bottom furnace knot for Fe3O4Reducing the copper nickel cobalt oxide, but not carrying out the matte making capability on the copper nickel cobalt oxide in the furnace junction. The pig iron and the ferrosilicon have high melting points, are slowly melted at the operating temperature of the electric settling furnace, have low reaction rate, and in addition, the pig iron is used for eliminating accretions, can generate deep pits on accretion layers and are not favorable for integrally eliminating accretions.
The silicon carbide, coke and coal can react with Fe in the accretion without the participation of flux3O4The reduction is carried out, but the three substances have small specific gravity, float on the upper layer in the melt and are difficult to contact with the accretion, and in order to obtain good reaction kinetic conditions, the three substances need to be conveyed to the furnace bottom by using a gas stirring molten pool or using a plug-in spray gun, but the serious accretion is inevitably generated by splashing the melt on the furnace wall top, and simultaneously, the ring for separating the slag matte by settling still is interferedAnd the electric furnace waste slag contains high valuable metals.
Ferrous sulfide in pyrite and high-quality copper concentrate needs to participate in a silica flux to react with Fe in accretions3O4And (4) carrying out reduction. Since the specific gravity of silica is smaller than that of slag, pyrite and copper concentrate can not sink to the bottom of the furnace, so that the molten pool is well stirred by compressed air to eliminate accretions by using pyrite and copper concentrate.
Diesel oil and natural gas are used as reducing agents to eliminate accretions, a spray gun is needed to send the diesel oil or the natural gas to the bottom of the furnace, slag splashing causes furnace wall and furnace top accretion, the spray gun is seriously burnt, the gun position is inaccurately controlled, and Fe3O4The reduction rate of (2) is low.
In production, the surface of the molten slag is reduced to make the molten slag contact with the accretion as much as possible, and the electrode is moved downwards to increase the power of the electric furnace and raise the temperature of the electric furnace, and the accretion is melted by overheating the molten slag. This measure only eliminates accretions in a limited area below the electrode area, which is energy intensive and makes the discharge of melt difficult.
The practice proves that the method is more reliable by periodically stopping the furnace and emptying the melt, and manually entering the furnace to clean the accretion, but the method has long stopping time, is difficult to utilize mechanized facilities, has high manual labor intensity, and damages the lining of the furnace by cleaning the accretion.
If the iron-sulfur alloy with high specific gravity, low melting point and reduction and vulcanization functions is adopted to efficiently and safely eliminate the over-thick accretion formed at the bottom of the settling electric furnace, the method has practical significance.
(2) Properties of iron-sulfur alloys
The melting point of pure iron is 1535 ℃ and the specific gravity of pure iron is 7.8, the melting point of FeS is 1193 ℃ and the specific gravity of FeS is 4.8. When the sulfur content of the pure iron is increased, the melting point is reduced, and the pure iron and FeS form eutectic at the sulfur content of 31 percent, the melting point is 988 ℃, and the eutectic composition is gamma Fe + FeS. Controlling the sulfur content in the process of preparing the iron-sulfur alloy can obtain alloys with different melting points and specific gravities.
The iron-sulfur alloy can not be used as a structural material and can be used as a reduction vulcanizing agent for the reverse sulfonium making reaction of slag and accretions in the nonferrous smelting industry.
(3) Difficulty in handling blowing slag
The slag produced in the process of converting matte into blister copper is called converting slag, and the main component of the converting slag is fayalite (Fe)2SiO4) Phase and magnetite (Fe)3O4) Phase, containing a certain amount of copper, nickel and cobalt. The copper in the converting slag exists mainly in the form of sulfide and then in the form of oxide; the existing forms of nickel and cobalt are mainly oxides and combinations, and are distributed in silicate and magnetite. The copper content in the blowing slag is usually 2% -5%, and the recycling process of the blowing slag comprises three processes:
and (3) slow cooling grinding floating process. Only the copper nickel cobalt existing in sulfide or simple substance form can be recovered, and if the copper nickel cobalt exists in oxidation state and combination state and is dissolved in slag, the mineral separation recovery rate is very low.
A pyrogenic process depletion process. The traditional dilution process is to carry out reduction vulcanization on the blowing slag, magnetic iron oxide carries out reduction slagging reaction under the action of supplemented flux to generate fayalite slag, copper nickel cobalt is vulcanized into sulfonium, the sulfonium is separated from the slag by convergence and sedimentation, the copper content in the slag can only be reduced to the slag-sulfonium balance level, and sulfonium drops smaller than 40 mu m are difficult to recover and are lost in the slag.
And returning to smelting and batching processes. The process is simple, but in the oxygen-enriched intensified smelting system, the Fe in the slag is blown and smelted3O4To be reacted with O2Competing for FeS, is at a disadvantage and requires SiO2Participating in the reduction slagging reaction of the magnetic iron oxide (3 Fe)3O4+FeS+5SiO2＝5Fe2SiO4+SO2) Can be done. Practice proves that the blowing slag returns a small amount to the smelting ingredients, the influence on the smelting operation is small, if the slag return amount is large, the content of magnetic iron oxide in the smelting slag can be increased, the discharge is difficult, and even the operation of a subsequent electric settling furnace is influenced.
The three processes have advantages and disadvantages respectively, and have the common point that copper is recycled, and iron in slag is not utilized.
Disclosure of Invention
In view of the problems and deficiencies of the prior art, the present invention provides a method for producing an iron-sulfur alloy. The iron-sulfur alloy prepared by the invention is Fe-FeS alloy. The invention is realized by the following technical scheme.
A method of producing an iron-sulfur alloy, comprising the steps of:
step 1, conveying converting slag, pyrite and a coal-based reducing agent produced in a matte converting process into a side-blown depletion converter, carrying out first-stage weak reduction smelting at the temperature of 1150-1300 ℃, and obtaining a Fe-S-O melt in which matte is dissolved after the weak reduction smelting finishes slag discharge; the specific process is as follows:
the method comprises the following steps of loading molten blowing slag into a furnace from a furnace mouth of a side-blowing depletion converter by using a slag ladle, feeding pyrite into the furnace from the furnace mouth by using a hopper, injecting a mixture of air and fuel into the furnace by using a combustion spray gun arranged on the end wall of the side-blowing depletion converter to adjust the furnace temperature, injecting a coal-based reducing agent into the deep part of a molten pool by using compressed air or nitrogen from a wind port of the side-blowing depletion converter, controlling a reducing atmosphere to perform a section of weak reduction on magnetic iron oxide in the blowing slag, wherein the reduction reaction is as follows:
reactant S in chemical reaction (5)2From the thermal decomposition of pyrite:
the atmosphere of the system is controlled to be weak reducing atmosphere, namely the adding amount of the reducing agent coal is controlled, the reaction (4) is difficult to occur, and the fayalite slag is not decomposed in a section of weak reducing operation. Controlling the charging amount of the pyrite, enabling the sulfur in the melt to be in a proper range, ensuring that a proper amount of FeO exists in the melt, and enabling FeS and FeO to form a completely-miscible Fe-S-O melt. And (3) carrying out copper nickel cobalt oxide sulfonium making in the blowing slag:
the matte is dissolved in the Fe-S-O melt. After the first stage of weak reduction, two layers of melts are formed in the molten pool, wherein the upper layer is the silicate-based slag with small specific gravity, and the lower layer is the Fe-S-O melt with large specific gravity and used for trapping the matte, and the two layers of melts are layered due to mutual insolubility and specific gravity difference. And after the weak reduction smelting is finished, slag is discharged to obtain Fe-S-O melt in which matte (matte) is dissolved.
Step 2, carrying out two-stage strong reduction smelting on the Fe-S-O melt dissolved with the copper matte obtained in the step 1 at the temperature of 1150-1300 ℃ to prepare iron-sulfur alloy; the method specifically comprises the following steps:
and discharging the upper-layer silicate slag by rotating the furnace, and leaving Fe-S-O melt to enter a two-stage strong reduction operation. Controlling the furnace temperature and the strong reducing atmosphere to reduce FeO in the Fe-S-O melt:
FeS cannot be reduced by carbon. Elemental iron generated by strong reduction is mutually soluble with FeS to form Fe-FeS alloy, and the matte containing copper, nickel and cobalt is also dissolved in the alloy. And after the second-stage strong reduction is finished, discharging the iron-sulfur alloy melt out of the furnace for water quenching to obtain granular iron-sulfur alloy.
The step 1 of controlling CO/CO by one-stage weak reduction smelting2The volume percentage is 0.1-0.2: 1.
controlling CO/CO by two-stage strong reduction smelting in the step 22The volume percentage is 1.5-2.0: 1.
the specific gravity of the iron-sulfur alloy is 5.3-7.0 g/cm3The sulfur content is 25-35%, the melting point is 900-1300 ℃, and the granularity is 1-40 mm.
The invention has the beneficial effects that:
(1) the iron-sulfur alloy is produced by using the converting hot slag as a main raw material, nonferrous metals and ferrous metals in the converting slag are comprehensively recovered, the energy consumption is low, and the processing cost of the alloy is low.
(2) The first-stage weak reduction produces a low-melting-point (the lowest melting point is 906 ℃) Fe-S-O melt, collects sulfonium, and discharges low-melting-point fayalite slag, so that the problem that high-melting-point calcium silicate slag needs to be produced in the traditional iron-making process is solved, the first-stage weak reduction is operated in the dilution converter design temperature range of 1150-1250 ℃, and the improvement of the furnace life of the dilution converter is facilitated.
(3) The Fe-FeS alloy of the two-stage strong reduction product has low melting point (the lowest melting point is 988 ℃), and the operating temperature is controlled within the range of 1100-1250 ℃. The two-stage strong reduction belongs to slag-free smelting, and the product recovery rate is high.
(4) The water quenching granulation of the Fe-FeS alloy melt avoids the problem of component segregation caused by slow cooling of the iron-sulfur alloy melt, and in addition, the granular alloy is convenient to use.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The method for producing the iron-sulfur alloy comprises the following steps:
step 1, blowing slag (containing Cu3.2wt% and Fe) produced in 50 tons of matte blowing process3O446wt percent of iron olivine slag, 49.2wt percent of iron olivine slag), pyrite (25.8 tons of pyrite containing 48wt percent of sulfur and 43wt percent of iron) are fed in batches into a 60-ton side-blown depletion converter, diesel oil is injected from a heat-preserving spray gun arranged on an end wall to keep the temperature of the converter at about 1220 ℃, a coal-based reducing agent (82 wt percent of fixed carbon, 8wt percent of volatile matter, 10wt percent of ash and granularity less than 5mm) is injected into a molten pool by nitrogen from a tuyere, the two guns are used for injecting, the injection rate of the reducing agent is controlled to be 69kg/min per gun, and the quantity of compressed nitrogen for conveying the reducing agent is 300 Nm/3Control of CO/h2The volume percentage is 0.1-0.2: 1; reducing for 30 minutes to a weak reduction smelting end point, consuming 650 liters of diesel oil and 4140kg of coal-based reducing agent; pouring a section of reducing slag, namely fayalite slag, into a slag bag from a furnace mouth by rotating a furnace body, and carrying out water quenching, wherein 29 tons of slag are discharged, the copper content in the slag is 0.36 wt%, and after the weak reduction smelting is finished, slag is discharged to obtain a Fe-S-O melt in which the copper matte is dissolved;
step 2, injecting the Fe-S-O melt dissolved with the copper matte obtained in the step 1 into a molten pool from an air port by using a coal-based reducing agent (fixed carbon 82%, volatile matter 8%, ash content 10% and granularity less than 5mm), injecting diesel oil from a heat-insulating spray gun arranged on a headwall to keep the temperature of the furnace at about 1180 ℃ for two-stage strong reduction smelting, controlling the injection rate of the reducing agent at 15kg/min for each gun, and conveying the reducing agent by using compressed air with the amount of 200Nm for each gun3Control of CO/h2The volume percentage is 1.5-2.0: 1; and (3) strongly reducing for 25 minutes to the end point of the second stage, and consuming 400 liters of the heat-preservation diesel oil and 750kg of reducing agent. And after the second-stage strong reduction is finished, the furnace body is rotated to pour the second-stage reduced iron-sulfur alloy melt into the copper matte bag and send the copper matte bag to carry out water quenching, 40 tons of alloy melt is generated altogether, and the water quenched iron-sulfur alloy contains 29.3 percent of sulfur, 65.58 percent of iron, 3.74 percent of copper, 1-20 mm of granularity, 1080 melting point and 6.1 specific gravity.
Example 2
The method for producing the iron-sulfur alloy comprises the following steps:
step 1, blowing 50 tons of matte into the blowing processProduced blowing slag (containing Cu2.6wt% and Fe)3O442 wt% of fayalite slag and 50 wt% of fayalite slag), pyrite (25.8 tons of pyrite containing 48 wt% of sulfur and 43 wt% of iron is fed in batches) is fed into a 60-ton side-blown depletion converter, diesel oil is injected from a heat-insulating spray gun arranged on a headwall to keep the temperature of the converter about 1200 ℃, a coal-based reducing agent (82 wt% of fixed carbon, 8 wt% of volatile matters, 10 wt% of ash and granularity less than 5mm) is injected into a molten pool by nitrogen from a tuyere, the two guns are used for injecting, the injection rate of the reducing agent is controlled to be 60kg/min for each gun, and the amount of compressed nitrogen for conveying the reducing agent is 300N3Control of CO/h2The volume percentage is 0.1-0.2: 1; reducing for 30 minutes to a weak reduction smelting end point, consuming 630 liters of diesel oil and 3600kg of coal-based reducing agent; pouring a section of reducing slag, namely fayalite slag, into a slag bag from a furnace mouth by rotating a furnace body, and carrying out water quenching, wherein 30 tons of slag are discharged, the copper content in the slag is 0.32 wt%, and after the weak reduction smelting is finished, slag is discharged to obtain a Fe-S-O melt in which the copper matte is dissolved;
step 2, injecting the Fe-S-O melt dissolved with the copper matte obtained in the step 1 into a molten pool from an air port by using a coal-based reducing agent (fixed carbon 82%, volatile matter 8%, ash content 10% and granularity less than 5mm), injecting diesel oil from a heat-insulating spray gun arranged on a headwall to keep the temperature of the furnace at about 1180 ℃ for two-stage strong reduction smelting, controlling the injection rate of the reducing agent to be 16kg/min for each gun, and conveying the reducing agent by using compressed air with the amount of 200Nm for each gun3Control of CO/h2The volume percentage is 1.5-2.0: 1; after strong reduction is carried out for 25 minutes to the end point of the second stage, 380 liters of heat-preservation diesel oil and 800kg of reducing agent are consumed. And after the second-stage strong reduction is finished, the furnace body is rotated to pour the second-stage reduced iron-sulfur alloy melt into the copper matte bag, and water quenching is carried out to produce 35.15 tons of alloy melt, wherein the water quenched iron-sulfur alloy contains 29.3 wt% of sulfur, 65.58 wt% of iron, 3.74 wt% of copper, 5-40 mm of granularity, 1130 ℃ of melting point and 6.4 of specific gravity.
While the present invention has been described in detail with reference to the specific embodiments thereof, the present invention is not limited to the embodiments described above, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Claims (2)
1. A method of producing an iron-sulfur alloy, characterized by the steps comprising:
step 1, conveying converting slag, pyrite and a coal-based reducing agent produced in a matte converting process into a side-blown depletion converter, carrying out first-stage weak reduction smelting at the temperature of 1150-1300 ℃, and obtaining a Fe-S-O melt in which matte is dissolved after the weak reduction smelting finishes slag discharge;
step 2, carrying out second-stage strong reduction smelting on the Fe-S-O melt dissolved with the copper matte obtained in the step 1 at the temperature of 1150-1300 ℃, discharging the iron-sulfur alloy melt out of the furnace to carry out water quenching after the second-stage strong reduction is finished, and preparing to obtain the iron-sulfur alloy;
the step 1 of controlling CO/CO by one-stage weak reduction smelting2The volume percentage is 0.1-0.2: 1;
controlling CO/CO by two-stage strong reduction smelting in the step 22The volume percentage is 1.5-2.0: 1.
2. the method of producing an iron-sulfur alloy according to claim 1, characterized in that: the specific gravity of the iron-sulfur alloy is 5.3-7.0 g/cm3The sulfur content is 25-35%, the melting point is 900-1300 ℃, and the granularity is 1-40 mm.
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| WO1979000058A1 (en) * | 1977-07-22 | 1979-02-08 | Boliden Ab | A method of manufacturing crude iron from sulphidic ironcontaining material |
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