CN108342585B - A kind of method of comprehensive utilization of magnesium-smelting reduction slag - Google Patents
A kind of method of comprehensive utilization of magnesium-smelting reduction slag Download PDFInfo
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- CN108342585B CN108342585B CN201810203208.1A CN201810203208A CN108342585B CN 108342585 B CN108342585 B CN 108342585B CN 201810203208 A CN201810203208 A CN 201810203208A CN 108342585 B CN108342585 B CN 108342585B
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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
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/14—Agglomerating; Briquetting; Binding; Granulating
- C22B1/24—Binding; Briquetting ; Granulating
- C22B1/242—Binding; Briquetting ; Granulating with binders
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
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- 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
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- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/04—Refining by applying a vacuum
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Abstract
A kind of method of comprehensive utilization of magnesium-smelting reduction slag, comprising the following steps: (1) mix powdered magnesium-smelting reduction slag, Cab-O-sil, carbonaceous reductant and binder；(2) it is dried after pelletizing is made；(3) melting is carried out using electric arc furnaces, the Silcaz that liquid is formed after melting is deposited on electric arc furnace bottom；(4) it after the Silcaz of liquid being discharged, pours into pig moulding machine and pours into Silcaz block；Silcaz block is directly as finished product or carries out step (5)；(5) broken be put into of Silcaz block is evaporated in vacuo in tank, is evaporated in vacuo, calcium is distilled off, and surplus material is Antaciron.Technique of the invention can realize the comprehensive utilization of reducing slag, be a kind for the treatment of process of green.
Description
Technical field
The invention belongs to metallurgical technology field, in particular to a kind of method of comprehensive utilization of magnesium-smelting reduction slag.
Background technique
85% or more magnesium metal is produced using ferrosilicon process in the world at present, now worldwide, the silicon of application
Thermal method is mainly Pidgeon process and interior electrical resistance heating.Either still interior electrical resistance heating, reducing agent used are Pidgeon process
Ferrosilicon, raw material are dolomite, and the two differs only in heating method difference.It is the magnesium-smelting silicothermic process of reducing agent using ferrosilicon
Technology, one ton of magnesium of every production will consume 10 tons or more of dolomite and one ton or more of ferrosilicon, while generate 5 tons or more of refining magnesium
Reducing slag.
The main ingredient of magnesium-smelting reduction slag is calcium orthosilicate, is in addition to this also had neither part nor lot in containing 4~7% MgO and part
The ferrosilicon of reduction reaction and some other impurity.In magnesium-smelting reduction slag in the form of ferrosilicon existing for silicon be about 3-5%, iron about exists
5% or so；Magnesium-smelting reduction slag contains calcium oxide about 50~60%, and silica about 28~35% (contains unreacted silicon)；Magnesium smelting reducing
Slag is mainly used for making cement raw material or for producing various bricks, but due to higher containing magnesium amount is aoxidized in reducing slag, cement plant addition
Measure limited, and brickmaking profit is lower, and dosage is also limited, therefore most magnesium-smelting reduction slag is simply discarded or fills,
This undoubtedly will cause environmental problem；Therefore, the processing problem of magnesium-smelting reduction slag, which has become, restricts Smelting magnesium industry value chain
A main problem.
Summary of the invention
The above problem existing for the magnesium-smelting reduction slag processing technique formed for existing ferrosilicon process production magnesium metal, the present invention
A kind of method of comprehensive utilization of magnesium-smelting reduction slag is provided, this method is using magnesium-smelting reduction slag as raw material, using carbonaceous material as reducing agent,
It first carries out melting and produces Silcaz, Silcaz is used to return to reduction magnesium process as magnesium smelting reducing agent, or carries out true
Sky distillation obtains calcium metal and Antaciron, and Antaciron is used to return to refining magnesium process as reducing agent, is not generating secondary dirt
While dye, reducing slag waste material is efficiently utilized.
The method of the present invention includes the following steps:
1, powdered magnesium-smelting reduction slag, Cab-O-sil, carbonaceous reductant and binder are uniformly mixed, mixture is made
Material；Wherein the dosage of Cab-O-sil is 0.4~2.0 times of magnesium-smelting reduction slag quality；The dosage of carbonaceous reductant presses fixation therein
Carbon and calcium oxide, silica and the complete Response calculation of magnesia, based on reaction equation are as follows:
CaO+C=CO+Ca (1),
SiO2+ C=Si+CO (2)
With MgO+C=Mg+CO (3)；
The dosage of binder is the 90~100% of carbonaceous reductant gross mass；
2, pelletizing is made in mixed material, then dried；
3, the pelletizing after drying is subjected to melting using electric arc furnaces, the Silcaz that liquid is formed after melting is deposited on electricity
Arc furnace bottom；
4, it after the Silcaz of liquid being discharged, pours into pig moulding machine and pours into Silcaz block；The silico-calcium of acquisition
Iron alloy block is directly as finished product or carries out step 5；
5, Silcaz block is broken into granularity≤10cm fragment, be put into vacuum distillation tank in, vacuum degree be 0.1~
It is heated to 900~1250 DEG C under conditions of 50Pa to be evaporated in vacuo, the time is 2~12h；Vacuum is kept in vacuum distillation process
Degree is 0.1~50Pa；After the completion of vacuum distillation, calcium is distilled off and becomes solid metallic calcium in condensation, and surplus material is silicon
Ferroalloy.
The ingredient of above-mentioned magnesium-smelting reduction slag contains MgO 4~7%, SiO by mass percentage225~32%, CaO 60~
66%, Fe2O33~5%.
In the above method, scrap iron is added in step 3 before melting into electric arc furnaces, control the Silcaz finally obtained
In, the mass percent of calcium is 29~50%, and the mass percent of silicon is 40~70%, and the mass percent of iron is 1~15%.
Partial size≤0.15mm of above-mentioned Cab-O-sil, partial size≤0.15mm of the carbonaceous reductant.
Above-mentioned carbonaceous reductant select coal, coke, semi-coke, forge after without coal-fired, petroleum coke and/or metallurgical coke.
Above-mentioned binder selects sulfite cellulose binder, bentonite, waterglass or other organic binders.
Briquetting pressure is 50~150MPa, the temperature 50~250 when drying when pelletizing being made in the above method, in step 2
DEG C, 2~8h of drying time.
In the above method, every the Silcaz of 2~10h discharge liquid when melting in step 3.
Part CaO, SiO in the above method, in step 3 when melting, in raw material2After being reduced into metal with MgO, due to
Vapour pressure is higher to be evaporated, and is reoxidized as corresponding oxide, and deposit in dust arrester installation, and oxidation is formed
The mixture of object；It is reused in the hopcalite return step 1 as magnesium-smelting reduction slag.
In the above method, Silcaz block is as magnesium smelting reducing agent for restoring refining magnesium process.
In the above method, Antaciron is as magnesium smelting reducing agent for restoring refining magnesium process.
In method fusion process of the invention in addition to generating portion gas, solid slag is not generated；It is all valuable in raw material
Ingredient enters in alloy；Calcium in Silcaz is distilled off condensation, and ferrosilicon stays in thermal region, to realize calcium
With the separation of ferrosilicon；The calcium of acquisition is sold after remelting refining ingot casting as metal calcium product, and remaining ferrosilicon is as refining magnesium
Reducing agent returns to refining magnesium process；The vacuum distillation tank of use is divided into heating zone and condensing zone, and heating zone is located in heating furnace and adds
Heat, condensing zone are located at the outside of heating furnace, and heating furnace is resistance furnace or gas burner, and reductive jar can take out out of reduction furnace, with
Convenient for fast cooling.
Process smelting silicothermic process magnesium reduction slag through the invention can realize the comprehensive utilization of reducing slag, refine after processing
Oxide in magnesium reduction slag is changed into Silcaz, and Silcaz can be used as reducing agent and return to refining magnesium process, can also be with
Silcaz is further distilled and obtains calcium and two kinds of products of ferrosilicon, and calcium is sold as product, Antaciron is as reduction
Agent returns to refining magnesium process.No matter which kind of method, any waste water in treatment process, the secondary pollutions such as waste residue are a kind of places of green
Science and engineering skill, while can get certain economic benefit.
Detailed description of the invention
Fig. 1 is the method for comprehensive utilization process flow chart of the magnesium-smelting reduction slag of the embodiment of the present invention 1；
Fig. 2 is the method for comprehensive utilization process flow chart of the magnesium-smelting reduction slag of the embodiment of the present invention 2；
Fig. 3 is the X-ray diffraction material phase analysis XRD diagram for the Silcaz that the embodiment of the present invention 1 obtains.
Specific embodiment
The vacuum distillation tank used in the embodiment of the present invention is equipped with heating zone and condensing zone, and heating zone is placed in heating furnace,
Condensing zone is located at outside heating furnace；The heating furnace is resistance furnace or gas burner.
The ingredient of the magnesium-smelting reduction slag used in the embodiment of the present invention contains MgO 4~7%, SiO by mass percentage2 25
~32%, CaO 60~66%, Fe2O33~5%.
Antaciron by mass percentage siliceous 65~80%, iron 35~20% in the embodiment of the present invention.
Cab-O-sil, carbonaceous reductant and the binder used in the embodiment of the present invention is commercial products.
The scrap iron used in the embodiment of the present invention is commercial products, main component Fe, FeO and Fe3O4, wherein iron content
It should be greater than 98%.
The model X Pert Pro MPDDY2094 of X-ray diffraction equipment in the embodiment of the present invention.
The equipment that pelletizing uses is made in the embodiment of the present invention as briquetting machine.
The Silcaz discharge of state is to go out the discharge of alloy mouth by electric arc furnace bottom in liquid embodiment of the present invention.
Temperature is subject to whole material melts when melting in the embodiment of the present invention.
Magnesium step is refined in vacuum-thermal reduction in the embodiment of the present invention are as follows: magnesium-Crystalline Magnesium-refining-ingot casting is refined in vacuum reduction, obtains
Obtain magnesium ingot.
The small agglomerate size produced with production of magnesium by pidgeonprocess process of the agglomerate size produced in the embodiment of the present invention is identical.
The briquetting machine used in the embodiment of the present invention is industrial production of magnesium by pidgeonprocess briquetting machine.
Embodiment 1
Powdered magnesium-smelting reduction slag, Cab-O-sil, carbonaceous reductant and binder are uniformly mixed, mixed material is made；
Wherein the dosage of Cab-O-sil is 0.4 times of magnesium-smelting reduction slag quality；The dosage of carbonaceous reductant is by fixed carbon therein and oxidation
Calcium, silica and the complete Response calculation of magnesia；The dosage of binder is the 90% of carbonaceous reductant gross mass；The grain of Cab-O-sil
Diameter≤0.15mm, carbonaceous reductant are coal, partial size≤0.15mm；Binder is sulfite cellulose binder；
Pelletizing is made in mixed material, is then dried；Briquetting pressure is 50MPa, the temperature 50 when drying when pelletizing is made
DEG C, drying time 8h；
Pelletizing after drying is subjected to melting using electric arc furnaces, the Silcaz that liquid is formed after melting is deposited on electric arc
Furnace bottom；Scrap iron is added before melting into electric arc furnaces, is controlled in the Silcaz finally obtained, the mass percent of calcium is
45%, the mass percent of silicon is 40%, and the mass percent of iron is 15%；Every the Silcaz of 10h discharge liquid；It is former
Part CaO, SiO in material2After being reduced into metal with MgO, evaporates, be reoxidized as phase since vapour pressure is higher
The oxide answered, and deposited in dust arrester installation, form hopcalite；The hopcalite is as refining magnesium
Reducing slag is reused；
After the Silcaz of liquid is discharged, pours into pig moulding machine and pour into Silcaz block；The silico-calcium iron of acquisition
The X-ray diffraction material phase analysis result of alloy block is as shown in figure 3, as magnesium smelting reducing agent for restoring refining magnesium process, by true
Sky reduction refining magnesium-Crystalline Magnesium-refining-ingot casting, obtains magnesium ingot, and the magnesium-smelting reduction slag that wherein vacuum reduction refining magnesium generates is as synthesis
Using the raw material of method, process is as shown in Figure 1.
Embodiment 2
Powdered magnesium-smelting reduction slag, Cab-O-sil, carbonaceous reductant and binder are uniformly mixed, mixed material is made；
Wherein the dosage of Cab-O-sil is 0.6 times of magnesium-smelting reduction slag quality；The dosage of carbonaceous reductant is by fixed carbon therein and oxidation
Calcium, silica and the complete Response calculation of magnesia；The dosage of binder is the 90% of carbonaceous reductant gross mass；The grain of Cab-O-sil
Diameter≤0.15mm, carbonaceous reductant are coke, partial size≤0.15mm；Binder is sulfite cellulose binder；
Pelletizing is made in mixed material, is then dried；Briquetting pressure is 50MPa, the temperature 100 when drying when pelletizing is made
DEG C, drying time 6h；
Pelletizing after drying is subjected to melting using electric arc furnaces, the Silcaz that liquid is formed after melting is deposited on electric arc
Furnace bottom；Scrap iron is added before melting into electric arc furnaces, is controlled in the Silcaz finally obtained, the mass percent of calcium is
26%, the mass percent of silicon is 62%, and the mass percent of iron is 12%；Every the Silcaz of 8h discharge liquid；It is former
Part CaO, SiO in material2After being reduced into metal with MgO, evaporates, be reoxidized as phase since vapour pressure is higher
The oxide answered, and deposited in dust arrester installation, form hopcalite；The hopcalite is as refining magnesium
Reducing slag is reused；
After the Silcaz of liquid is discharged, pours into pig moulding machine and pour into Silcaz block；
Silcaz block is broken into granularity≤10cm fragment, is put into vacuum distillation tank, is 0.1Pa's in vacuum degree
Under the conditions of be heated to 900 DEG C and be evaporated in vacuo, time 12h；It is 0.1Pa that vacuum degree is kept in vacuum distillation process；Vacuum
After the completion of distillation, calcium is distilled off and becomes solid metallic calcium in condensation, and surplus material is Antaciron, as magnesium smelting reducing
Agent refines magnesium-Crystalline Magnesium-refining-ingot casting for restoring refining magnesium process, by vacuum reduction, obtains magnesium ingot, and wherein vacuum reduction is refined
Raw material of the magnesium-smelting reduction slag that magnesium generates as method of comprehensive utilization, process are as shown in Figure 2.
Embodiment 3
With embodiment 1, difference is method:
(1) dosage of Cab-O-sil is 0.8 times of magnesium-smelting reduction slag quality；The dosage of binder is carbonaceous reductant gross mass
95%；Carbonaceous reductant is semi-coke；Binder is bentonite；
(2) briquetting pressure is 100MPa, 150 DEG C of temperature when drying, drying time 5h；
(3) scrap iron is added before melting into electric arc furnaces, is controlled in the Silcaz finally obtained, the mass percent of calcium
It is 50%, the mass percent of silicon is 40%, and the mass percent of iron is 10%；Every the Silcaz of 6h discharge liquid.
Embodiment 4
With embodiment 1, difference is method:
(1) dosage of Cab-O-sil is 1.0 times of magnesium-smelting reduction slag quality；The dosage of binder is carbonaceous reductant gross mass
95%；Carbonaceous reductant is after forging without fire coal；Binder is waterglass；
(2) briquetting pressure is 100MPa, 200 DEG C of temperature when drying, drying time 4h；
(3) scrap iron is added before melting into electric arc furnaces, is controlled in the Silcaz finally obtained, the mass percent of calcium
It is 33%, the mass percent of silicon is 59%, and the mass percent of iron is 8%；Every the Silcaz of 5h discharge liquid.
Embodiment 5
With embodiment 2, difference is method:
(1) dosage of Cab-O-sil is 1.5 times of magnesium-smelting reduction slag quality；The dosage of binder is carbonaceous reductant gross mass
100%；Carbonaceous reductant is petroleum coke；Binder is bentonite；
(2) briquetting pressure is 150MPa, 220 DEG C of temperature when drying, drying time 3h；
(3) scrap iron not to be added when melting, is controlled in the Silcaz finally obtained, the mass percent of calcium is 22%,
The mass percent of silicon is 75%, and the mass percent of iron is 3%；Every the Silcaz of 3h discharge liquid；
(4) be evaporated in vacuo vacuum degree be 5Pa, 1000 DEG C of temperature, time 6h；Holding vacuum degree is in vacuum distillation process
5Pa。
Embodiment 6
With embodiment 2, difference is method:
(1) dosage of Cab-O-sil is 2.0 times of magnesium-smelting reduction slag quality；The dosage of binder is carbonaceous reductant gross mass
100%；Carbonaceous reductant is metallurgical coke；Binder is waterglass；
(2) briquetting pressure is 150MPa, 250 DEG C of temperature when drying, drying time 2h；
(3) scrap iron not to be added when melting, is controlled in the Silcaz finally obtained, the mass percent of calcium is 19%,
The mass percent of silicon is 80%, and the mass percent of iron is 1%；Every the Silcaz of 2h discharge liquid；
(4) be evaporated in vacuo vacuum degree be 50Pa, 1250 DEG C of temperature, time 2h；Vacuum degree is kept in vacuum distillation process
For 50Pa.
Claims (4)
1. a kind of method of comprehensive utilization of magnesium-smelting reduction slag, it is characterised in that the following steps are included:
(1) powdered magnesium-smelting reduction slag, Cab-O-sil, carbonaceous reductant and binder are uniformly mixed, mixed material is made；Its
The dosage of middle Cab-O-sil is 0.4 ~ 2.0 times of magnesium-smelting reduction slag quality；The dosage of carbonaceous reductant presses fixed carbon therein and oxygen
Change calcium, silica and the complete Response calculation of magnesia, based on reaction equation are as follows:
CaO+C=CO+Ca (1),
SiO2+ C=Si+CO (2)
With MgO+C=Mg+CO (3)；
The dosage of binder is the 90 ~ 100% of carbonaceous reductant gross mass；The ingredient of the magnesium-smelting reduction slag presses quality percentage
Than containing MgO 4 ~ 7%, SiO225 ~ 32%, CaO 60 ~ 66%, Fe2O33~5%；Partial size≤0.15mm of the Cab-O-sil, it is described
Carbonaceous reductant partial size≤0.15mm；The carbonaceous reductant select coal, coke, semi-coke, forge after without coal-fired, petroleum coke
And/or metallurgical coke；The binder selects sulfite cellulose binder, bentonite or waterglass；
(2) pelletizing is made in mixed material, then dried；Briquetting pressure is 50 ~ 150MPa, the temperature when drying when pelletizing is made
50 ~ 250 DEG C, 2 ~ 8h of drying time；
(3) pelletizing after drying is subjected to melting using electric arc furnaces, the Silcaz that liquid is formed after melting is deposited on electric arc
Furnace bottom；
(4) it after the Silcaz of liquid being discharged, pours into pig moulding machine and pours into Silcaz block；The silico-calcium iron of acquisition closes
Gold bullion is directly as finished product or carries out step (5)；
(5) Silcaz block is broken into granularity≤10cm fragment, be put into vacuum distillation tank, be 0.1 ~ 50Pa in vacuum degree
Under conditions of be heated to 900 ~ 1250 DEG C and be evaporated in vacuo, the time is 2 ~ 12h；Holding vacuum degree is in vacuum distillation process
0.1~50Pa；After the completion of vacuum distillation, calcium is distilled off and becomes solid metallic calcium in condensation, and surplus material is ferrosilicon conjunction
Gold.
2. a kind of method of comprehensive utilization of magnesium-smelting reduction slag according to claim 1, it is characterised in that melting in step (3)
Scrap iron is added in forward direction electric arc furnaces, is controlled in the Silcaz finally obtained, and the mass percent of calcium is 29 ~ 50%, the matter of silicon
Measuring percentage is 40 ~ 70%, and the mass percent of iron is 1 ~ 15%.
3. a kind of method of comprehensive utilization of magnesium-smelting reduction slag according to claim 1, it is characterised in that melting in step (3)
When every 2 ~ 10h discharge liquid Silcaz.
4. a kind of method of comprehensive utilization of magnesium-smelting reduction slag according to claim 1, it is characterised in that melting in step (3)
When, part CaO, SiO in raw material2After being reduced into metal with MgO, evaporates, be reoxidized since vapour pressure is higher
It is deposited as corresponding oxide, and in dust arrester installation, forms hopcalite；The hopcalite returns
It returns in step 1 and is reused as magnesium-smelting reduction slag.
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| CN102560149B (en) * | 2012-03-08 | 2014-03-05 | 东北大学 | Method for refining magnesium by taking silico-calcium alloy as reducing agent under vacuum |
| CN104245974A (en) * | 2012-04-27 | 2014-12-24 | 姜远燮 | Method for preparing ferro-silicon and magnesium using ferro-nickel slag, preparation apparatus used therefor, and smelting reduction furnace |
| CN103361448B (en) * | 2013-07-29 | 2014-11-26 | 东北大学 | Method of preparing Fe-Ca-Si alloy from melt metallurgical slag |
| CN104120284B (en) * | 2014-08-12 | 2015-09-09 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of magnesium is reclaimed from magnesium eletrolysis residue |
| CN105039744A (en) * | 2015-07-28 | 2015-11-11 | 宋开泉 | Method for preparing solid carbon dioxide and calcium metal through calcite |
| CN106467936B (en) * | 2016-09-08 | 2018-01-02 | 江苏省冶金设计院有限公司 | A kind of preparation method of Silcaz |
| CN107090547A (en) * | 2017-05-17 | 2017-08-25 | 西安建筑科技大学 | It is a kind of to reduce the method that magnesium process prepares AL-Si-Fe alloy and reduces magnesium in Pidgeon process |
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