CN105568004B - A kind of method of the aluminium chromium slag melting crome metal in electric arc furnaces - Google Patents

A kind of method of the aluminium chromium slag melting crome metal in electric arc furnaces Download PDF

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CN105568004B
CN105568004B CN201610121427.6A CN201610121427A CN105568004B CN 105568004 B CN105568004 B CN 105568004B CN 201610121427 A CN201610121427 A CN 201610121427A CN 105568004 B CN105568004 B CN 105568004B
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chromium
crome metal
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aluminium
aluminium chromium
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CN105568004A (en
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高红军
宋建义
曹杨
寇志远
朱逾倩
刘帅
杨晓辉
黄博
田刚
高辉
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JINZHOU JIXIN HIGH-TEMPERATURE MATERIAL Co Ltd
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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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • 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
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/32—Obtaining chromium
    • 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
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Refinement Of Pig-Iron, Manufacture Of Cast Iron, And Steel Manufacture Other Than In Revolving Furnaces (AREA)
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Abstract

A kind of method of the aluminium chromium slag melting crome metal in electric arc furnaces, the petroleum coke of granularity 10mm aluminium chromium slags and granularity 10mm is well mixed, it is sent to and dries kiln drying to moisture≤0.5%, it is added to smelting in three-phawse arc furnace, pyrolytic semlting, the liquid chromium carbide in arc furnace cylinder bottom portion is transferred in plasma arc furnace, to being passed through oxygen in the cupola well of plasma arc furnace, and add calcium oxide and slag former calcirm-fluoride, argon gas is passed through as protection gas to plasma arc furnace after high melt, aluminum shot is added to continue to smelt, obtain qualified liquid metal chromium, it is poured in arenaceous shell mould, natural cooling, remove the impurity on surface, it is broken, obtain crome metal.With aluminium chromium slag be raw material production crome metal, by first reducing, rear oxidation remove carbon two-step method metal smelting chromium, it is with low cost, solve aluminium chromium slag emission problem, realize resource reutilization, rational technology, product purity is high, and performance is good, be adapted to industrialized production.

Description

A kind of method of the aluminium chromium slag melting crome metal in electric arc furnaces
Technical field
The invention belongs to metal material field of smelting, the side of more particularly to a kind of aluminium chromium slag melting crome metal in electric arc furnaces Method.
Background technology
As the emission request of the attention of Environmental, the particularly three wastes is stricter.Enterprise is to the solid that is discharged Discarded object can not only bring huge economic benefit through treatment, recycling, more meet friendly environment production.
Crome metal product is national strategy product, and the product is applied to smelts high temperature alloy, electric resistance alloy and accurate conjunction Gold.
At present, the production method of crome metal only has three kinds, and one is with chromium oxide and metal aluminum reduction method, industrial referred to as gold Category thermal reduction；It is for second to reduce generation chromium carbide under vacuum conditions with chromium oxide and carbon, with chromium carbide and chromium oxide Mixing generates granulated metal chromium under vacuum conditions；The third is to produce crome metal with chromic salts (chromic salts of sexavalence) electrolysis.
Aluminothermic process production crome metal produces substantial amounts of solid waste aluminium chromium slag, aluminium chromium slag to contain Al2O3And Cr2O3Consolidate Melt, wherein Al2O3+Cr2O3Weight/mass percentage composition is generally higher than 97%, wherein, the oxygen containing mass percent 8%~16% Change chromium and a small amount of Na2CrO4、CaO、Fe2O3、Na2O、K2O and SiO2Impurity.Wherein Na2CrO4It is soluble chromic salts, contains Cr (VI) be country prohibit row a class hazardous waste.
The content of the invention
Carbon two-step method metal smelting is removed by first reduction, rear oxidation in electric furnace using aluminium chromium slag the invention provides one kind The method of chromium, crome metal is produced by raw material of aluminium chromium slag, with low cost, solves aluminium chromium slag emission problem, realizes resource again Utilize, rational technology, product purity is high, and performance is good, be adapted to industrialized production.
The technical scheme is that：
A kind of method of the aluminium chromium slag melting crome metal in electric arc furnaces, it is comprised the following steps that：
A. raw material and processing
Aluminium chromium clinker material is taken, aluminium chromium clinker material be crushed to granularity for below 10mm；It is below 10mm's to take granularity Aluminum shot；Taking reducing agent petroleum coke be crushed to granularity for below 10mm；Take oxygen purity >=99.5%；Take smelting solvent oxidation Calcium, gross mass content≤0.3% of iron oxide and silica in calcium oxide；Slag former calcirm-fluoride is taken, iron oxide in calcirm-fluoride With gross mass content≤0.3% of silica, mass content≤0.02% of phosphorus；
B. mixing is homogenized
By the petroleum coke after the aluminium chromium slag after crushing and smashing according to mass ratio 100:3~100:6 are well mixed, and are sent to dry Dry kiln drying obtains mixed dry material to moisture≤0.5%；
C. pyrolytic semlting
Mixed dry material is added in three-phawse arc furnace and is smelted, temperature control is 2000 DEG C~2200 DEG C, duration of heat control After 8h~12h, pyrolytic semlting, the aluminum oxide in aluminium chromium slag is through high-temperature oxydation into α-Al for system2O3Corundum is on electric arc furnaces cupola well Portion, the Cr in aluminium chromium slag2O3Chromium carbide is reduced to by petroleum coke and is settled down to arc furnace cylinder bottom portion；
D. oxidation is except carbon and removes impurity
The liquid chromium carbide in arc furnace cylinder bottom portion is transferred in plasma arc furnace, to the cupola well of plasma arc furnace Oxygen is inside passed through, and adds calcium oxide and slag former calcirm-fluoride, at 1800 DEG C~2200 DEG C, high melt 40min~70min, Wherein, the quality of carbon and the mass ratio for being passed through oxygen are 3 in chromium carbide:4, chromium carbide is 100 with calcium oxide mass ratio:3~ 100:5, chromium carbide is 100 with calcirm-fluoride mass ratio:1~100:3, it is passed through argon gas conduct to plasma arc furnace after high melt Protection gas, while carbon content in the crome metal obtained after sampling analysis melting；When carbon content≤0.5%, sampling analysis again Oxygen content in crome metal, during crome metal oxygen content≤0.5%, obtains qualified liquid metal chromium, comes out of the stove；Crome metal oxygen content During ＞ 0.5%, according to chromium carbide and aluminum shot mass ratio 100:0.3~100:0.5 adds aluminum shot to continue at 2000 DEG C~2200 DEG C 1min~2min is smelted, qualified liquid metal chromium is obtained；
E. qualified liquid metal chromium will be smelted to be poured in arenaceous shell mould, natural cooling 24h, by the crome metal in grinding tool Stick together out, removed the impurity on surface, be crushed to 10mm~100mm, obtained crome metal.
Al in the aluminium chromium slag2O3Mass percentage content for 70%~84%, Cr2O3Mass percentage content be 8%~16%, Na2The mass percentage content of O is 1.5%~3%；The mass percentage content of CaO is 0.6%~1.1%.
The mass percentage content containing C is 98%~99%, ash content mass percent≤0.5% in the petroleum coke.
Mass percentage content >=99% of Al in the aluminum shot.
The activity degree of the calcium oxide is CaO >=300；CaF in the calcirm-fluoride2Mass percentage content >=90%.
The purity of the crome metal is 96%~99%.
When being passed through argon gas and doing protection gas, argon gas intake is 400L/min~500L/min, wherein, the purity of argon gas >= 99.9%.
Beneficial effects of the present invention：
(1), Cr is contained in aluminium chromium slag2O3, crome metal is produced by raw material of aluminium chromium slag, it is with low cost, solve the discharge of chromium slag Problem, realizes resource reutilization.
(2) crome metal, is produced using two-step method, first, with petroleum coke also primary aluminum chromium slag, the oxidation in aluminium chromium slag can be made Aluminium is through high-temperature oxydation into α-Al2O3Corundum is on electric furnace cupola well top, the Cr in chromium slag2O3Agent reduction and carbonization chromium is reduced, is carbonized Chromium obtains final products crome metal, with traditional metallothermic reduction by being passed through oxygen, calcium oxide and calcirm-fluoride except carbon, purification Method, carbon reduction method are compared with electrolysis, it is possible to use containing chromium oxide very low raw material aluminium chromium slag production crome metal, rational technology, Aluminium chromium slag produces crome metal product and corundum phase material is completely separated, and realizes zero-emission, and chromium content can reach after smelting 96wt%~99wt%, product purity is high, and performance is good, and about 20,000 tons of chromium ore resource can be saved every year, is adapted to industrialized production.
Specific embodiment
Embodiment 1
A. raw material and processing
Take containing Cr2O3The aluminium chromium clinker material of mass percent 10%, by aluminium chromium clinker material be crushed to granularity for 10mm with Under；
The aluminum shot of mass percentage content >=99% of Al is taken, granularity is below 10mm；
The mass percentage content for taking C is 98% petroleum coke, ash content mass percent≤0.5%, and being crushed to granularity is Below 10mm；
Take oxygen, argon gas, oxygen purity >=99.5%, purity >=99.9% of argon gas；
Smelting solvent oxidation calcium is taken, the activity degree of calcium oxide is CaO >=300, iron oxide and silica in calcium oxide Gross mass content≤0.3%；
Slag former calcirm-fluoride is taken, CaF in calcirm-fluoride2Mass percentage content >=90%, iron oxide and silica Gross mass content≤0.3%, mass content≤0.02% of phosphorus；
B. mixing is homogenized
18 tons of aluminium chromium slag charge for being crushed to -10mm (below 10mm) is taken, is mixed with the petroleum coke 540kg for being crushed to -10mm Homogenizing, is sent to and dries kiln drying to moisture≤0.5%, obtains mixed dry material；
C. pyrolytic semlting
By 4000KVA three-phawse arc furnaces open cooling water, feeding temperature-raising, by smelting with mixed dry material add electric arc furnaces in, Three-phase graphite electrode mixed dry material submerged-arc smelting to molten condition, smelting temperature are controlled at 2000 DEG C~2200 DEG C, is smelted After 8h, pyrolytic semlting, the aluminum oxide in aluminium chromium slag is through high-temperature oxydation into α-Al for time control2O3Corundum is in electric arc furnaces cupola well Top, the Cr in aluminium chromium slag2O3Chromium carbide (Cr is reduced to by petroleum coke7C3And Cr23C6) it is settled down to arc furnace cylinder bottom portion；
D. oxidation is except carbon and removes impurity
After smelting is finished, the liquid oxidatively aluminium on stove top is poured in bull ladle and is removed, remaining 1.5 tons of chromium carbides are poured on In another bull ladle, it is transported in 1000KVA plasma arc furnaces, oxygen is passed through in the cupola well of plasma arc furnace, wherein, The quality of carbon and the mass ratio for being passed through oxygen are 3 in chromium carbide:4, feeding temperature-raising；60kg calcium oxide and 15kg fluorinations are added simultaneously Calcium, is passed through argon gas in cupola well when smelting 40min at 1800 DEG C~2000 DEG C, argon gas intake is 400L/min, while Carbon content in the crome metal obtained after sampling analysis melting, during carbon content≤0.5%, the oxygen in sampling analysis crome metal contains again During amount ＞ 0.5%, add 6kg aluminum shots to continue to smelt 1min at 2000 DEG C~2200 DEG C, obtain qualified liquid metal chromium；
E. qualified liquid metal chromium will be smelted to be poured in arenaceous shell mould, natural cooling 24h, by the crome metal in grinding tool Stick together out, removed the impurity on surface, be crushed to 10mm~100mm, obtained the crome metal of 1.133t, realized 92% receipts Rate, sampling detection physical and chemical composition, physical and chemical composition is shown in Table 1；Then it is classified, is put in storage by the product packaging of the different trades mark.
Embodiment 2
A. raw material and processing
Take containing Cr2O3The aluminium chromium clinker material of mass percent 10%, by aluminium chromium clinker material be crushed to granularity for 10mm with Under；
The aluminum shot of mass percentage content >=99% of Al is taken, granularity is below 10mm；
The mass percentage content for taking C is 98% petroleum coke, ash content mass percent≤0.5%, and being crushed to granularity is Below 10mm；
Take oxygen, argon gas, oxygen purity >=99.5%, purity >=99.9% of argon gas；
Smelting solvent oxidation calcium is taken, the activity degree of calcium oxide is CaO >=300, iron oxide and silica in calcium oxide Gross mass content≤0.3%；
Slag former calcirm-fluoride is taken, CaF in calcirm-fluoride2Mass percentage content >=90%, iron oxide and silica Gross mass content≤0.3%, mass content≤0.02% of phosphorus；
B. mixing is homogenized
20 tons of aluminium chromium slag charge for being crushed to -10mm is taken, homogenizing is mixed with the petroleum coke 800kg for being crushed to -10mm, be sent to dry Dry kiln drying obtains mixed dry material to moisture≤0.5%；
C. pyrolytic semlting
By 4000KVA three-phawse arc furnaces open cooling water, feeding temperature-raising, by smelting with mixed dry material add electric arc furnaces in, Three-phase graphite electrode mixed dry material submerged-arc smelting to molten condition, smelting temperature are controlled at 2000 DEG C~2200 DEG C, is smelted After 9h, pyrolytic semlting, the aluminum oxide in aluminium chromium slag is through high-temperature oxydation into α-Al for time control2O3Corundum is in electric arc furnaces cupola well Top, the Cr in aluminium chromium slag2O3Chromium carbide (Cr is reduced to by petroleum coke7C3And Cr23C6) it is settled down to arc furnace cylinder bottom portion；
D. oxidation is except carbon and removes impurity
The liquid oxidatively aluminium on stove top is poured in bull ladle and is removed, be finally poured on remaining 2 tons carbon containing liquid metal chromium In another bull ladle, it is transported in 1000KVA plasma arc furnaces, oxygen is passed through in the cupola well of plasma arc furnace, wherein, The quality of carbon and the mass ratio for being passed through oxygen are 3 in chromium carbide:4, feeding temperature-raising；100kg calcium oxide and 60kg fluorine are added simultaneously Change calcium, be passed through argon gas when smelting to 70min in cupola well, argon gas intake is 500L/min, while after sampling analysis melting To crome metal in carbon content, during carbon content≤0.5%, the oxygen content ＞ 0.5% in sampling analysis crome metal again is added 10kg aluminum shots continue to smelt 2min at 1900 DEG C~2100 DEG C, and remaining chromium oxide, obtains qualified liquid in the chromium of reducing metal Crome metal；
E. qualified liquid metal chromium will be smelted to be poured in arenaceous shell mould, natural cooling 24h, by the crome metal in grinding tool Stick together out, removed the impurity on surface, be crushed to 10mm~100mm, obtained the crome metal of 1.645t, realized 92.5% receipts Rate, sampling detection physical and chemical composition, physical and chemical composition is shown in Table 1；Then it is classified, is put in storage by the product packaging of the different trades mark.
Embodiment 3
A. raw material and processing
Take containing Cr2O3The aluminium chromium clinker material of mass percent 10%, by aluminium chromium clinker material be crushed to granularity for 10mm with Under；
The aluminum shot of mass percentage content >=99% of Al is taken, granularity is below 10mm；
The mass percentage content for taking C is 98% petroleum coke, ash content mass percent≤0.5%, and being crushed to granularity is Below 10mm；
Take oxygen, argon gas, oxygen purity >=99.5%, purity >=99.9% of argon gas；
Smelting solvent oxidation calcium is taken, the activity degree of calcium oxide is CaO >=300, iron oxide and silica in calcium oxide Gross mass content≤0.3%；
Slag former calcirm-fluoride is taken, CaF in calcirm-fluoride2Mass percentage content >=90%, iron oxide and silica Gross mass content≤0.3%, mass content≤0.02% of phosphorus；
B. mixing is homogenized
21 tons of aluminium chromium slag charge for being crushed to -10mm (below 10mm) is taken, is mixed with the petroleum coke 1050kg for being crushed to -10mm Homogenizing, is sent to and dries kiln drying to moisture≤0.5%, obtains mixed dry material；
C. pyrolytic semlting
By 4000KVA three-phawse arc furnaces open cooling water, feeding temperature-raising, by smelting with mixed dry material add electric arc furnaces in, Three-phase graphite electrode mixed dry material submerged-arc smelting to molten condition, smelting temperature are controlled at 2000 DEG C~2200 DEG C, is smelted After 12h, pyrolytic semlting, the aluminum oxide in aluminium chromium slag is through high-temperature oxydation into α-Al for time control2O3Corundum is in electric arc furnaces cupola well Top, the Cr in aluminium chromium slag2O3Chromium carbide (Cr is reduced to by petroleum coke7C3And Cr23C6) it is settled down to arc furnace cylinder bottom portion；
D. oxidation is except carbon and removes impurity
The liquid oxidatively aluminium on stove top is poured in bull ladle and is removed, finally fall remaining 2.3 tons carbon containing liquid metal chromium In another bull ladle, it is transported in 1000KVA plasma arc furnaces, oxygen is passed through in the cupola well of plasma arc furnace, its In, the quality of carbon and the mass ratio for being passed through oxygen are 3 in chromium carbide:4, feeding temperature-raising；92kg calcium oxide and 46kg are added simultaneously Calcirm-fluoride, is passed through argon gas in cupola well when smelting to 50min, argon gas intake is 400L/min, while after sampling analysis melting Carbon content in the crome metal for obtaining, when carbon content≤0.5%, sampling analysis, oxygen content≤0.5% in crome metal, obtain again To qualified liquid metal chromium；
E. qualified liquid metal chromium will be smelted to be poured in arenaceous shell mould, natural cooling 24h, by the crome metal in grinding tool Stick together out, removed the impurity on surface, be crushed to 10mm~100mm, obtained the crome metal of 2t, realized 92.8% yield, Sampling detection physical and chemical composition, physical and chemical composition is shown in Table 1；Then it is classified, is put in storage by the product packaging of the different trades mark.
Physical and chemical composition testing result (the unit of 1 1~embodiment of the embodiment of the present invention of table 3：Wt%)
Cr Al Fe Si C S Cu P O+H+N Pb+Sn+Sb+Bi+As
Embodiment 1 96.05 1.05 0.98 0.33 0.06 0.03 0.05 0.01 0.5 0.005
Embodiment 2 98.21 0.45 0.60 0.20 0.05 0.03 0.04 0.01 0.3 0.005
Embodiment 3 98.99 0.25 0.3 0.15 0.04 0.02 0.04 0.01 0.15 0.005

Claims (7)

1. a kind of method of the aluminium chromium slag melting crome metal in electric arc furnaces, it is characterized in that：
Comprise the following steps that：
A. raw material and processing
Aluminium chromium clinker material is taken, aluminium chromium clinker material be crushed to granularity for below 10mm；Take the aluminum shot that granularity is below 10mm； Taking reducing agent petroleum coke be crushed to granularity for below 10mm；Take oxygen purity >=99.5%；Take smelting solvent oxidation calcium, oxygen Change gross mass content≤0.3% of iron oxide and silica in calcium；Slag former calcirm-fluoride is taken, iron oxide and dioxy in calcirm-fluoride Gross mass content≤0.3% of SiClx, mass content≤0.02% of phosphorus；
B. mixing is homogenized
By the petroleum coke after the aluminium chromium slag after crushing and smashing according to mass ratio 100:3~100:6 are well mixed, and are sent to dry kiln Middle drying obtains mixed dry material to moisture≤0.5%；
C. pyrolytic semlting
Mixed dry material is added in three-phawse arc furnace and is smelted, temperature control is 2000 DEG C~2200 DEG C, duration of heat control exists 8h~12h, after pyrolytic semlting, the aluminum oxide in aluminium chromium slag is through high-temperature oxydation into α-Al2O3Corundum on electric arc furnaces cupola well top, Cr in aluminium chromium slag2O3Chromium carbide is reduced to by petroleum coke and is settled down to arc furnace cylinder bottom portion；
D. oxidation is except carbon and removes impurity
The liquid chromium carbide in arc furnace cylinder bottom portion is transferred in plasma arc furnace, is led to in the cupola well of plasma arc furnace Enter oxygen, and add calcium oxide and slag former calcirm-fluoride, at 1800 DEG C~2200 DEG C, high melt 40min~70min, wherein, The quality of carbon and the mass ratio for being passed through oxygen are 3 in chromium carbide:4, chromium carbide is 100 with calcium oxide mass ratio:3~100:5, carbon It is 100 to change chromium with calcirm-fluoride mass ratio:1~100:3, argon gas is passed through as protection gas to plasma arc furnace after high melt, Carbon content in the crome metal obtained after sampling analysis melting simultaneously；When carbon content≤0.5%, again in sampling analysis crome metal Oxygen content, during crome metal oxygen content≤0.5%, obtain qualified liquid metal chromium, come out of the stove；Crome metal oxygen content ＞ 0.5% When, according to chromium carbide and aluminum shot mass ratio 100:0.3~100:0.5 adds aluminum shot to continue to smelt 1min at 2000 DEG C~2200 DEG C ~2min, obtains qualified liquid metal chromium；
E. qualified liquid metal chromium will be smelted to be poured in arenaceous shell mould, natural cooling 24h has sticked together the crome metal in grinding tool Go out, remove the impurity on surface, be crushed to 10mm~100mm, obtain the crome metal that purity is 96%~99%.
2. the method for the aluminium chromium slag melting crome metal in electric arc furnaces according to claim 1, it is characterized in that：The aluminium chromium slag Middle Al2O3Mass percentage content for 70%~84%, Cr2O3Mass percentage content for 8%~16%, Na2The quality of O Degree is 1.5%~3%；The mass percentage content of CaO is 0.6%~1.1%.
3. the method for the aluminium chromium slag melting crome metal in electric arc furnaces according to claim 1, it is characterized in that：The petroleum coke In containing C mass percentage content be 98%~99%, ash content mass percent≤0.5%.
4. the method for the aluminium chromium slag melting crome metal in electric arc furnaces according to claim 1, it is characterized in that：In the aluminum shot Mass percentage content >=99% of Al.
5. the method for the aluminium chromium slag melting crome metal in electric arc furnaces according to claim 1, it is characterized in that：The calcium oxide Activity degree be CaO >=300.
6. the method for the aluminium chromium slag melting crome metal in electric arc furnaces according to claim 1, it is characterized in that：The calcirm-fluoride Middle CaF2Mass percentage content >=90%.
7. the method for the aluminium chromium slag melting crome metal in electric arc furnaces according to claim 1, it is characterized in that：Argon gas is passed through to do During protection gas, argon gas intake is 400L/min~500L/min, wherein, purity >=99.9% of argon gas.
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