CN110184476B - Method for eliminating accretions in electric settling furnace - Google Patents

Method for eliminating accretions in electric settling furnace Download PDF

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CN110184476B
CN110184476B CN201910404495.7A CN201910404495A CN110184476B CN 110184476 B CN110184476 B CN 110184476B CN 201910404495 A CN201910404495 A CN 201910404495A CN 110184476 B CN110184476 B CN 110184476B
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iron
furnace
matte
slag
alloy
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CN110184476A (en
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李东波
沈强华
欧阳飞
陈雯
杨鹏
李超航
赵双红
姚培福
张新宇
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Yunnan Copper Co ltd Southwest Copper Branch
Kunming University of Science and Technology
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Yunnan Copper Co ltd Southwest Copper Branch
Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0026—Pyrometallurgy
    • C22B15/0028—Smelting or converting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0026—Pyrometallurgy
    • C22B15/0054—Slag, slime, speiss, or dross treating
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B15/00—Obtaining copper
    • C22B15/0026—Pyrometallurgy
    • C22B15/006—Pyrometallurgy working up of molten copper, e.g. refining

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Abstract

The invention relates to a method for eliminating accretions in a settling electric furnace, belonging to the technical field of nonferrous metallurgy. The mixed melting of the smelting slag and the matte produced in the copper smelting processThe body is sent into a settling electric furnace to carry out clarification and separation of slag matte, when the temperature of a melt in the electric furnace is controlled within a set range to carry out settling of matte, an iron-sulfur alloy is put into a molten pool, the iron-sulfur alloy is an alloy consisting of simple substance iron and ferrous sulfide, wherein the iron in the iron-sulfur alloy is 61-70 percent, and the sulfur in the iron-sulfur alloy is 25-35 percent; the specific gravity of the iron-sulfur alloy is 5.3 to 7.0 g/cm3The melting point is 900-1300 ℃, and the granularity is 1-40 mm. The method can ensure that the furnace bottom accretion thickness of the electric settling furnace is controlled below 300mm, and the slag discharge port and the matte discharge port are unblocked and not blocked; the furnace accretion is melted quickly and eliminated integrally. The use of pig iron to eliminate accretions can produce a pit in the accretion layer, which is not favorable for eliminating accretions as a whole.

Description

Method for eliminating accretions in electric settling furnace
Technical Field
The invention relates to a method for eliminating accretions in a settling electric furnace, belonging to the technical field of nonferrous metallurgy.
Background
The chemical essence of copper smelting by taking copper sulfide ore as a raw material is the gathering of desulfurization and iron removal and oxide gangue. The traditional smelting method such as electric furnace, blast furnace and reverberatory furnace smelting has low smelting intensity, low oxygen potential of the system and no obvious harm of magnetic iron oxide. The development trend of modern copper metallurgy is strong oxidation smelting, and because the oxygen potential of a system is high, the smelting strength is high, the copper matte grade is high, and the increase of the content of magnetic iron oxide in smelting slag is an important reason for the increase of copper content in slag and the formation of accretion. After oxidation reaction, part of iron in the furnace charge is formed into Fe3O4，Fe3O4Has a high melting point (1597 ℃) and exists in a Fe-O complex ion state in the slag, when the amount of the Fe-O complex ion existsWhen the amount 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 melt3O4Part of the iron oxide precipitates on the bottom of the furnace to form a furnace knot, and the composition of the furnace knot contains magnesium aluminate spinel and copper nickel cobalt oxide besides the magnetic iron oxide.
The thickening of the furnace bottom and the furnace accretion can harm the normal operation of the electric settling furnace, and the furnace accretion thickness is maintained between 200mm and 300mm, which is beneficial to protecting the furnace bottom. How to efficiently and safely eliminate the over-thick accretion formed at the bottom of the electric settling furnace is the focus of modern copper metallurgy and the technical problem.
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 melted slowly at the operating temperature of the electric settling furnace, and have low reaction rate.
The silicon carbide, coke and coal can react with Fe in the accretion without the participation of flux3O4The reduction is carried out, but the specific gravity of the three substances is small, the three substances can float on the upper layer in the melt and are difficult to contact with a furnace accretion, and in order to obtain good reaction kinetic conditions, the three substances need to be stirred by gas or sent to the furnace bottom by a plug-in spray gun, but the melt is inevitably splashed on the furnace wall and the furnace top to generate serious accretion, and the environment of slag matte standing, settling and separating is also disturbed, so that the waste slag of the electric furnace contains high-value metal.
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, and the problems in production are that slag splashing causes accretion on the top of the furnace wall, the burning loss of the spray gun is serious, the gun position is not accurately controlled, and the reduction rate of Fe3O4 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.
Disclosure of Invention
In order to solve the problems and the defects, the invention provides a method for eliminating accretions in a settling electric furnace. The invention is realized by the following technical scheme.
A method for eliminating accretions in a settling electric furnace, comprising the steps of:
feeding mixed melt of smelting slag and matte produced in the copper smelting process into a settling electric furnace for clarifying and separating slag matte, and when the temperature of the melt in the electric furnace is controlled within a set range for settling the matte, feeding an iron-sulfur alloy into a molten pool, wherein the iron-sulfur alloy is an alloy consisting of simple substance iron and ferrous sulfide, and the iron and sulfur alloy contains 61-70% of iron and 25-35% of sulfur; the specific gravity of the iron-sulfur alloy is 5.3 to 7.0 g/cm3The melting point is 900-1300 ℃, and the granularity is 1-40 mm.
The method specifically comprises the following steps:
an iron-sulfur alloy Fe-FeS alloy (specific gravity 5.3-7.0 g/cm)3) The alloy is put into a molten pool from a slag inlet at the top of the electric furnace and feed holes at two sides, and the alloy passes throughSlag layer (specific gravity 3.3-3.7 g/cm)3) A sulfonium layer (specific gravity 4.7-5.2 g/cm)3) Reaching the surface of a bottom furnace junction, heating and melting the alloy at the temperature of a molten pool of a settling electric furnace (1150-1300 ℃), spreading the alloy along the surface of the furnace junction, and enabling the Fe simple substance in the alloy and the Fe in the furnace junction3O4Carrying out a reaction:
Figure BDA0002060779240000021
carrying out sulfonium making reaction on FeS in the alloy and copper nickel cobalt oxide in a furnace junction:
Cu2O+FeS＝Cu2S+FeO (2)
3NiO+3FeS＝Ni3S2+3FeO+1/2S2 (3)
CoO+FeS＝CoS+FeO (4)
FeO generated by the reaction floats upwards and SiO in the melt2Combining to generate iron olive stone which is merged into slag:
Figure BDA0002060779240000022
cu produced by sulfonium-making reaction2S、Ni3S2The CoS and the FeS are mutually dissolved to form the matte.
The method can lead the magnetic iron oxide in the furnace accretion to be successfully reduced and slagged, lead the copper nickel cobalt oxide in the furnace accretion to be formed into matte, lead the furnace accretion to be melted and converted into slag and matte with low melting point and low specific gravity.
When the mixed melt of the smelting slag and the matte is subjected to matte sedimentation in the sedimentation electric furnace, the iron-sulfur alloy is added once every day, the iron-sulfur alloy addition is completed within 15 minutes, the matte discharge is avoided during the iron-sulfur alloy addition, and the smelting slag and the matte discharge can be carried out according to the normal operation system of the sedimentation electric furnace after the delay of the iron-sulfur alloy addition for 10 minutes.
The electric settling furnace is discharged every day, and copper matte and slag are discharged respectively. Because the temperature field distribution of each area of the molten pool is different, the accretion thickness of each area of the furnace bottom is different, when the copper matte surface and the slag surface are lowered to low positions, the accretion thickness distribution is actually measured by the probe rod for the electric settling furnace, the alloy input amount of the corresponding area is adjusted, and then the measured iron-sulfur alloy fragments are freely dropped from each feed hole of the furnace top.
The above Fe-containing3O4After the smelting slag and the flux are added into a settling electric furnace, part of Fe is under the action of a carbon electrode3O4The slag-making furnace can perform reduction slagging reaction, and the rest of slag-making furnace is distributed in molten slag, molten matte and separated out to form furnace knots. The thickening speed of the accretion is influenced by the slag type, the furnace temperature, the electrode operating system and the melt discharge system. The total alloy consumption for treating the accretion once a day is calculated by calculating the iron content of each material entering the electric furnace and the iron content of each material discharged from the electric furnace every day, wherein the difference value of the iron content and the iron content can be regarded as the amount of iron entering the accretion, and the total alloy consumption for treating the accretion once a day is calculated by combining the reaction formula (1) and the content of simple substance iron in the Fe-FeS alloy of the iron-sulfur alloy.
The preparation method of the iron-sulfur alloy comprises the following steps:
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:
Figure BDA0002060779240000031
Figure BDA0002060779240000032
Figure BDA0002060779240000033
Figure BDA0002060779240000034
Figure BDA0002060779240000035
reactant S in chemical reaction (5)2From the thermal decomposition of pyrite:
Figure BDA0002060779240000041
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 (9) 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:
Figure BDA0002060779240000042
Figure BDA0002060779240000043
Figure BDA0002060779240000044
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:
Figure BDA0002060779240000045
Figure BDA0002060779240000046
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 method can eliminate accretion and reduce the magnetic iron oxide in the waste slag to below 6.5 wt%, and the copper content of the electric furnace waste slag is controlled to below 0.55 wt%.
The invention has the beneficial effects that:
(1) the method can ensure that the furnace bottom accretion thickness of the electric settling furnace is controlled below 300mm, and the slag discharge port and the matte discharge port are unblocked and not blocked; the furnace accretion is melted quickly and eliminated integrally. The use of pig iron to eliminate accretions can produce a pit in the accretion layer, which is not favorable for eliminating accretions as a whole.
(2) The ferrous sulfide brought by the Fe-FeS alloy carries out the matte making reaction on the copper nickel cobalt oxide in the furnace junction, thereby being beneficial to improving the recovery rate of the copper nickel cobalt.
(3) The Fe-FeS alloy has low price, and the operation cost for treating the accretion by the alloy is lower than that of the current various methods.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The cupronickel production flow matching settlement electric furnace (also called depletion electric furnace in the industry) for producing 20 ten thousand tons of copper annually by oxygen-enriched top blowing has the hearth size of 22.28 multiplied by 5.81 multiplied by 4.5 meters and 6 electrodes. The traditional process is that an electric furnace receives 110 tons of slag-matte mixed melt (the mixed melt contains 23.52 percent of copper and 26.73 percent of iron, wherein the smelting slag contains 7.8 percent of magnetic iron oxide) sent by a top-blowing furnace every hour, the furnace temperature is kept between 1180 and 1220 ℃, the power of the electric furnace is maintained at 4870 kilowatts per hour, the slag-matte mixed melt is inserted into an oil gun from the top of the electric furnace for reduction during the heat preservation, clarification and separation of the electric furnace, the oil gun is inserted for reduction twice every day, and 9 am: 00 start first reduction, 13 pm: 00 the second reduction was started, each for 50 minutes, with a diesel consumption of 10 litres/minute. 45.5 tons of copper matte (the copper grade is 56 weight percent, and the total iron content is 18.6 weight percent) and 63 tons of waste slag are obtained every hour, and the waste slag contains Cu0.568weight percent, and the total iron content is 32.3 weight percent, and the waste slag contains Fe3O47.0 wt%. The furnace accretion layer at the bottom of the electric furnace is thickened at the area near the matte discharging port according to the thickness of 3-5mm every day, the maximum thickness of the furnace accretion can reach about 500mm, and the maximum thickness of the furnace accretion at the slag discharging port area can reach about 800 mm.
Example 1
The method for eliminating accretions in the electric settling furnace comprises the following steps:
the electric settling furnace receives a mixed melt (the mixed melt contains 23.47 wt% of copper and 27.10 wt% of iron, wherein the smelting slag contains 7.8 wt% of magnetic iron oxide) of smelting slag and matte produced in a copper smelting process, which is conveyed from the top-blowing furnace, and the mixed melt is conveyed into the electric settling furnace for slag and matte clarification and separation, the furnace temperature is kept between 1180 ℃ and 1220 ℃, the electric furnace power is maintained at 4850 kilowatts per hour, and the electric settling furnace power is 13: 00-14:after the procedure of charging the matte mixed melt into the electric precipitation furnace is finished in the time period of 00, 3 tons of iron-sulfur alloy (containing 67 wt% of iron, 28 wt% of sulfur, melting point 1100 ℃ and specific gravity of 6.4 g/cm) is added in 15 minutes3And the granularity is 5 mm-40 mm). Clarifying and separating by an electric furnace to obtain 45.1 tons of matte (the copper grade is 56.4wt percent, and the total iron content is 17.83wt percent) and 65 tons of waste slag per hour, wherein the waste slag contains Cu0.548wt percent, and the total iron content is 35.8wt percent, and the waste slag contains Fe3O46.2 wt%. The elimination condition of the furnace accretion at the bottom of the electric furnace is detected after 96 hours of production, the thickness of the furnace accretion in the area near the matte discharge port is about 250mm, and the thickness of the furnace accretion in the area of the slag discharge port is about 350mm, so that the smooth condition of the furnace bottom and the furnace is favorably protected.
Example 2
The method for eliminating accretions in the electric settling furnace comprises the following steps:
the electric settling furnace receives a mixed melt (the mixed melt contains 24.55 wt% of copper and 26.27 wt% of iron, wherein the smelting slag contains 8.5 wt% of magnetic iron oxide) of smelting slag and matte produced in a copper smelting process, which is conveyed from the top-blowing furnace, and the mixed melt is conveyed into the electric settling furnace for clarifying and separating the slag and the matte, the furnace temperature is kept between 1180 ℃ and 1220 ℃, the electric furnace power is maintained at 4850 kilowatts per hour, and the ratio of the molten slag to the matte is 13: 00-14: after the procedure of feeding the matte mixed melt into the electric precipitation furnace is finished in the time period of 00 hours, 3.5 tons of iron-sulfur alloy (containing 61 wt% of iron and 35 wt% of sulfur, melting point 1150 ℃ and specific gravity of 5.8 g/cm) is added in 15 minutes3And the granularity is 1 mm-20 mm). Clarifying and separating by an electric furnace to obtain 39.5 tons of matte (copper grade 67wt percent, total iron content 10.1wt percent) and 72.6 tons of waste slag per hour, wherein the waste slag contains Cu0.546wt percent, total iron content 36.97wt percent and Fe content3O46.4 wt%. After 7 days of production, the elimination condition of the furnace bottom accretion of the electric furnace is detected, the thickness of the accretion in the area near the matte discharge port is about 250mm, the thickness of the accretion in the area of the slag discharge port is about 300mm, and the thickness of the accretion is reasonably controlled.
Example 3
The method for eliminating accretions in the electric settling furnace comprises the following steps:
the precipitation electric furnace receives a mixed melt of the slag and matte (the mixed melt contains 24.10 wt.% copper and 26.72 wt.% iron) produced in a copper smelting process of 110 tons per hour from the top-blowing furnace, wherein the slag contains magnetic oxygen7.2 wt%) of iron, feeding the iron melt into a settling electric furnace to perform clarification and separation of slag matte, keeping the furnace temperature at 1180-1220 ℃, and maintaining the electric furnace power at 4860 kilowatts per hour, wherein the ratio of the iron melt to the sulfur melt is 13: 00-14: after the procedure of feeding the matte mixed melt into the electric precipitation furnace is finished in the time period of 00, 2.5 tons of iron-sulfur alloy (containing 70 wt% of iron, 25 wt% of sulfur, melting point of 1200 ℃ and specific gravity of 6.7 g/cm) is added in 15 minutes3And the granularity is 5 mm-20 mm). Clarifying and separating by an electric furnace to obtain 49 tons of matte (the copper grade is 53.3wt percent, and the total iron content is 20.7wt percent) and 62.8 tons of waste slag per hour, wherein the waste slag contains 0.53wt percent of Cu0.3 wt percent, and the total iron content is 32.3wt percent3O45.7 wt%. After 7 days of production, the elimination condition of the furnace bottom accretion of the electric furnace is detected, the thickness of the accretion in the area near the matte discharge port is about 250mm, the thickness of the accretion in the area of the slag discharge port is about 300mm, and the thickness of the accretion is reasonably controlled.
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 (3)

1. A method for eliminating accretions in a settling electric furnace is characterized by comprising the following steps:
feeding mixed melt of smelting slag and matte produced in the copper smelting process into a settling electric furnace for clarifying and separating slag matte, and when the temperature of the melt in the electric furnace is controlled within a set range for settling the matte, feeding an iron-sulfur alloy into a molten pool, wherein the iron-sulfur alloy is an alloy consisting of simple substance iron and ferrous sulfide, and the iron and sulfur alloy contains 61-70% of iron and 25-35% of sulfur; the specific gravity of the iron-sulfur alloy is 5.3 to 7.0 g/cm3The melting point is 900-1300 ℃, and the granularity is 1-40 mm;
the preparation method of the iron-sulfur alloy comprises the following steps:
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;
and 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 the iron-sulfur alloy.
2. The method for eliminating accretions in a settling electric furnace as claimed in claim 1, wherein: when the mixed melt of the smelting slag and the matte is subjected to matte sedimentation in the sedimentation electric furnace, the iron-sulfur alloy is added once every day, the iron-sulfur alloy addition is completed within 15 minutes, the matte discharge is avoided during the iron-sulfur alloy addition, and the smelting slag and the matte discharge can be carried out according to the normal operation system of the sedimentation electric furnace after the delay of the iron-sulfur alloy addition for 10 minutes.
3. The method for eliminating accretions in a settling electric furnace as claimed in claim 1, wherein: and the probe rod for the settlement electric furnace actually measures the thickness distribution of furnace accretions, adjusts the alloy input amount of a corresponding area, and then freely drops the measured iron-sulfur alloy fragments from each feeding hole on the furnace top.
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