CN110904347B - Method for reducing content of iron oxide in vanadium slag - Google Patents
Method for reducing content of iron oxide in vanadium slag Download PDFInfo
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- CN110904347B CN110904347B CN201911311436.1A CN201911311436A CN110904347B CN 110904347 B CN110904347 B CN 110904347B CN 201911311436 A CN201911311436 A CN 201911311436A CN 110904347 B CN110904347 B CN 110904347B
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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
- C22B34/00—Obtaining refractory metals
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
- C21C5/28—Manufacture of steel in the converter
- C21C5/30—Regulating or controlling the blowing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C5/00—Manufacture of carbon-steel, e.g. plain mild steel, medium carbon steel or cast steel or stainless steel
- C21C5/28—Manufacture of steel in the converter
- C21C5/36—Processes yielding slags of special composition
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Abstract
The invention relates to a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: and after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag. By the method, iron oxide in the vanadium slag is reduced to generate an iron simple substance and carbon monoxide, wherein the iron simple substance enters the semisteel, and the carbon monoxide is discharged along with furnace gas. By adopting the protective gas blowing and lance pulling operations, the stable state of the vanadium slag in the furnace is destroyed, the discharge of carbon monoxide is accelerated, and the reduction reaction is promoted. Finally, the purpose of reducing the content of ferric oxide in the vanadium slag is achieved.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for reducing the content of iron oxide in vanadium slag.
Background
Vanadium resources are important scarce resources in the country and even in the world, are called monosodium glutamate in modern industry, the capacity is mainly distributed in China (44.8%), south Africa (20.8%), Russia (13.8%), America (7.6%), Australia (4.6%) and other countries (8.4%), vanadium is widely applied to the fields of steel, chemical industry, aerospace, military industry and the like, more than 90% of vanadium is used in the steel industry, and is mainly applied to high-quality steel, low-alloy steel and part of plain carbon steel products. The global development and utilization of vanadium resources are characterized in that the development of vanadium Qinzi magnetite is mainly used, other resources are used as auxiliaries, the vanadium produced from the vanadium Qinzi magnetite accounts for 85% of the total amount, and the reserve reaches 470 billion t. China has over 170 hundred million copies of vanadium Qinzhou magnetite, is located at the third position of the world and is mainly distributed in the climbing areas of Sichuan province and the Chengdu areas of Hebei province.
A method for recovering vanadium resources from vanadium titanomagnetite mainly comprises the steps of smelting the vanadium titanomagnetite in a blast furnace or an electric furnace, obtaining vanadium-containing molten iron through reduction reaction, oxidizing vanadium elements into furnace slag by utilizing selective oxidation of the vanadium elements in the molten iron to obtain furnace slag with high vanadium content, and extracting vanadium from the furnace slag.
The blast furnace reduction method is to make the vanadium-containing magnetite into sintered ore in a sintering machine, and then reduce the sintered ore in a blast furnace to obtain vanadium-containing molten iron, and the countries adopting the process have China and Russia. The electric furnace reduction method is to reduce the vanadium-containing magnetite into metallized pellets, and then smelting the metallized pellets in an electric furnace to obtain vanadium-containing molten iron, and the countries adopting the method have New Zealand and south Africa.
In the process of extracting vanadium by the converter, vanadium in molten iron is oxidized, simultaneously, elements such as silicon, titanium, manganese, iron, chromium and the like are oxidized, and the oxidation products and impurities in the coolant form vanadium slag. The residual vanadium in the semisteel can be reduced and the recovery rate of vanadium element can be improved by prolonging the oxygen supply time, but the molten iron loss is increased while the oxygen supply time is prolonged.
The vanadium extraction process is an oxidation reaction process of elements such as iron, vanadium, carbon, silicon, manganese, phosphorus, sulfur and the like in molten iron, and the oxidation reaction of the elements is carried out at a speed which depends on the chemical composition of the molten iron and thermodynamic and kinetic conditions during blowing.
At present, there are three main treatment methods for extracting vanadium from vanadium-containing molten iron:
(1) a sodium slagging method: the sodium carbonate is directly added into the vanadium-containing molten iron, so that vanadium in the molten iron is converted into sodium vanadate, and meanwhile, harmful elements S, P in the molten iron can be removed. The slag obtained by this method can be directly extracted by water leaching process2O5. If the content of the semi-steel S, P is low, steel making can be carried out by a less slag method or a non-slag method.
(2) The blowing vanadium slag method comprises the following steps: blowing air or oxygen into converter or other container to obtain V2O5Vanadium slag and semisteel. The method utilizes the V, C selective oxidation principle, V needs to be oxidized to the maximum degree in smelting, and C is prevented from being oxidized in a large amount, so that vanadium extraction and carbon protection are realized. The process is the main method for extracting vanadium from vanadium Qinzhou magnetite at present, and is more economical compared with the method for directly extracting vanadium from ore. Currently 66% of the world's vanadium is produced using this process.
(3) The vanadium-containing steel slag method comprises the following steps: directly blowing vanadium-containing molten iron into steel, oxidizing vanadium into steel slag, and extracting vanadium from the steel slag. Compared with the method for converting vanadium slag, the method saves equipment for converting vanadium slag, saves investment, reduces iron loss during converting vanadium slag, and is a novel vanadium extraction method.
The converter vanadium extraction method is to mix vanadium-containing molten iron into a converter for blowing, so that vanadium is oxidized into slag to realize the separation of vanadium and iron. At present, the method for extracting vanadium by a converter comprises the following steps: top blowing, bottom blowing, or combined blowing. The key technology of vanadium extraction in the converter is to add a coolant to control the temperature of a molten pool, realize the purpose of vanadium extraction and carbon preservation and simultaneously remove Si.
When blown in a converter, vanadium is oxidized while part of carbon and other elements are oxidized, and a large amount of chemical heat is generated, which causes the temperature of the molten pool to rise. According to the selective oxidation of carbon and vanadium in molten iron, when the temperature of a molten pool is too high, a large amount of carbon is oxidized, and the oxidation of vanadium is inhibited, so that the condition that the carbon content in semi-steel is too low to be beneficial to subsequent steelmaking is caused, and the recovery rate of vanadium is reduced because vanadium cannot be sufficiently oxidized. Common coolants include iron ore, iron scale, pig iron block, scrap steel, water, and the like. The highest content of iron in the vanadium slag is about 35-40%. Reducing the iron content is an effective measure to increase the vanadium content. The total iron content in the slag depends on the oxygen supply intensity and the position of the oxygen lance. The reduction of the total iron content in the slag by 5 percent is beneficial to improving the vanadium content in the slag.
The vanadium production enterprises in China and Russia mainly adopt the process, and the process flow is as follows: and (3) extracting vanadium and vanadium slag from the vanadium-Qinzhou magnetite-iron ore concentrate-blast furnace molten iron rotary converter. Compared with the atomization vanadium extraction method, the converter vanadium extraction method has the obvious advantages that the heat loss of the converter vanadium extraction process is less than that of the atomization vanadium extraction process; in the smelting process, pig iron blocks and cold bonded pellets are required to be added as cooling agents, so that the production cost is reduced and the yield of semisteel is improved; the period of vanadium extraction in the converter is shorter than that of vanadium extraction by atomization.
But the vanadium content in the river steel bearing molten iron is lower at present, generally between 0.21 and 0.23 percent. In order to improve the recovery rate of vanadium elements, the oxygen supply time in the vanadium extraction process is prolonged, and the iron oxide content in the vanadium slag is increased while the residual vanadium in the semisteel is reduced.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a method for reducing the content of iron oxide in vanadium slag, and the method can remarkably reduce the content of iron oxide in the vanadium slag and further improve the metal yield.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: and after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag.
By the method, iron oxide in the vanadium slag is reduced to generate an iron simple substance and carbon monoxide, wherein the iron simple substance enters the semisteel, and the carbon monoxide is discharged along with furnace gas. By adopting the protective gas blowing and gun pulling operations, the stable state of the vanadium slag in the furnace is destroyed, the discharge of carbon monoxide is accelerated, the reduction reaction is promoted, and the purpose of reducing the content of iron oxide in the vanadium slag is finally achieved.
In a preferred embodiment of the present invention, the additive is added in an amount of 2 to 3 kg/ton of iron, for example, 2 kg/ton of iron, 2.1 kg/ton of iron, 2.2 kg/ton of iron, 2.3 kg/ton of iron, 2.4 kg/ton of iron, 2.5 kg/ton of iron, 2.6 kg/ton of iron, 2.7 kg/ton of iron, 2.8 kg/ton of iron, 2.9 kg/ton of iron, or 3 kg/ton of iron, but not limited to the values listed, and other values not listed in this range are also applicable.
As a preferred embodiment of the present invention, the additive includes 1 or at least 2 of coke powder, aluminum chips, charcoal, petroleum coke, semicoke, bituminous coke, or bituminous coal, and may be, for example, a combination of coke powder and aluminum chips, a combination of aluminum chips and charcoal, a combination of charcoal and petroleum coke, a combination of petroleum coke and semicoke, a combination of semicoke and bituminous coke, a combination of bituminous coke and bituminous coal, or a combination of bituminous coal and coke powder, but is not limited to the above-mentioned combinations, and other combinations not listed in this range are also applicable.
In a preferred embodiment of the present invention, the particle size of the additive is 1 to 5mm, and may be, for example, 1mm, 1.2mm, 1.4mm, 1.6mm, 1.8mm, 2mm, 2.2mm, 2.4mm, 2.6mm, 2.8mm, 3mm, 3.2mm, 3.4mm, 3.6mm, 3.8mm, 4mm, 4.2mm, 4.4mm, 4.6mm, 4.8mm or 5mm, but is not limited to the values listed, and other values not listed in this range are also applicable.
As a preferred embodiment of the present invention, the protective atmosphere comprises nitrogen and/or argon.
In a preferred embodiment of the present invention, the reaction time is 60 to 100 seconds, and may be, for example, 60s, 62s, 64s, 66s, 68s, 70s, 72s, 74s, 76s, 78s, 80s, 82s, 84s, 86s, 88s, 90s, 92s, 94s, 96s, 98s, or 100s, but is not limited to the listed values, and other values not listed in the range are also applicable.
As a preferred embodiment of the present invention, the protective atmosphere is provided by a spray gun.
As a preferred technical scheme of the invention, the spray gun is pulled for 3-5 times in a reciprocating way between 1m and 1.5 m.
In a preferred embodiment of the present invention, the pressure of the protective atmosphere is 1 to 3MPa, and may be, for example, 1MPa, 1.2MPa, 1.4MPa, 1.6MPa, 1.8MPa, 2MPa, 2.2MPa, 2.4MPa, 2.6MPa, 2.8MPa or 3MPa, but is not limited to the values listed, and other values not listed in the range are also applicable.
As a preferred technical solution of the present invention, the method comprises: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2-3 kg/ton iron; the additive comprises 1 or at least 2 of coke powder, aluminum scraps, charcoal, petroleum coke, semicoke, pitch coke or bituminous coal; the particle size of the additive is 1-5 mm; the protective atmosphere comprises nitrogen and/or argon; the reaction time is 60-100 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled in a reciprocating manner for 3-5 times between 1m and 1.5 m; the pressure of the protective atmosphere is 1-3 MPa.
Compared with the prior art, the invention has the following beneficial effects:
by the method, iron oxide in the vanadium slag is reduced to generate an iron simple substance and carbon monoxide, wherein the iron simple substance enters the semisteel, and the carbon monoxide is discharged along with furnace gas. By adopting the protective gas blowing and lance pulling operations, the stable state of the vanadium slag in the furnace is destroyed, the discharge of carbon monoxide is accelerated, and the reduction reaction is promoted. Finally, the purpose of reducing the content of ferric oxide in the vanadium slag is achieved, and the maximum reduction amplitude of the content of ferric oxide can reach 5%. Furthermore, the iron oxide content in the vanadium slag is reduced, so that the grade of the vanadium slag is improved, and the loss of iron elements in the vanadium extraction process is reduced.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2 kg/ton iron; the additive is coke powder; the particle size of the additive is 2 mm; the protective atmosphere is nitrogen; the reaction time is 60 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled in a reciprocating manner for 3 times between 1m and 1.5 m; the pressure of the protective atmosphere is 1.2 MPa.
The content of ferric oxide in the obtained vanadium slag is 34.15%, and the grade of vanadium in the vanadium slag is 12.34%.
Example 2
The embodiment provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2.5 kg/ton iron; the additive is charcoal; the particle size of the additive is 5 mm; the protective atmosphere is nitrogen; the reaction time is 72 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled for 4 times in a reciprocating way between 1m and 1.5 m; the pressure of the protective atmosphere is 2 MPa.
The content of iron oxide in the obtained vanadium slag is 33.59%, and the grade of vanadium in the vanadium slag is 12.72%.
Example 3
The embodiment provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 3 kg/ton iron; the additive is petroleum coke; the particle size of the additive is 3.8 mm; the protective atmosphere is nitrogen; the reaction time is 100 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled in a reciprocating manner for 5 times between 1m and 1.5 m; the pressure of the protective atmosphere is 3 MPa.
The content of ferric oxide in the obtained vanadium slag is 32.27%, and the grade of vanadium in the vanadium slag is 13.31%.
Example 4
The embodiment provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2.7 kg/ton iron; the additive is aluminum scraps; the particle size of the additive is 2.6 mm; the protective atmosphere is nitrogen; the reaction time is 94 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled in a reciprocating manner for 3 times between 1m and 1.5 m; the pressure of the protective atmosphere is 1.6 MPa.
The content of ferric oxide in the obtained vanadium slag is 32.61%, and the grade of vanadium in the vanadium slag is 12.87%.
Example 5
The embodiment provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2.2 kg/ton of iron; the additive is charcoal; the particle size of the additive is 1.2 mm; the protective atmosphere is nitrogen; the reaction time was 68 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled for 4 times in a reciprocating way between 1m and 1.5 m; the pressure of the protective atmosphere is 2.6 MPa.
The content of ferric oxide in the obtained vanadium slag is 33.04%, and the grade of vanadium in the vanadium slag is 12.76%.
Example 6
The embodiment provides a method for reducing the content of iron oxide in vanadium slag, which comprises the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2.4 kg/ton iron; the additive is coke powder; the particle size of the additive is 3 mm; the protective atmosphere is nitrogen; the reaction time is 88 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled for 4 times in a reciprocating way between 1m and 1.5 m; the pressure of the protective atmosphere is 1 MPa.
The content of ferric oxide in the obtained vanadium slag is 32.84%, and the grade of vanadium in the vanadium slag is 13.66%.
Comparative example 1
The only difference from example 2 is that no charcoal was added, no nitrogen lance was operated, the iron oxide content in the vanadium slag after the end of the converting was 38.45%, and the vanadium grade in the vanadium slag was 11.73%.
In the above-mentioned embodiment 1-2, the vanadium extraction and blowing in the converter is carried out by adding 135 tons of vanadium-containing molten iron into the converter, adding 45kg of coolant per ton of iron, with a blowing lance position of 1.0m and an oxygen flow of 11000m3H, oxygen supply time 402 s; and then the above-mentioned processing is performed. The elemental composition in the molten iron is shown in the following table 1:
TABLE 1
| Composition (I) | C | Si | Mn | P | S | V | Ti | Cr |
| Content (%) | 4.15 | 0.18 | 0.25 | 0.161 | 0.058 | 0.227 | 0.269 | 0.10 |
Example 3-4 vanadium extraction from converter blowing is carried out by charging vanadium-containing molten iron into converter 136 tons, adding coolant 45 kg/ton iron, blowing lance position 1.0m, and oxygen flow 11000m3H, oxygen supply time 422 s; and then the above-mentioned processing is performed. The elemental composition in the molten iron is shown in the following table 2:
TABLE 2
| Composition (I) | C | Si | Mn | P | S | V | Ti | Cr |
| Content (%) | 4.27 | 0.16 | 0.24 | 0.162 | 0.068 | 0.219 | 0.258 | 0.10 |
Example 5-6 vanadium extraction from converter and blowing, 135 tons of vanadium-containing molten iron were added into the converter, 45 kg/ton of iron was added as a coolant, the blowing lance was 1.0m, and the oxygen flow was 11000m3H, oxygen supply time 435 s. And then the above-mentioned processing is performed. The elemental composition in the molten iron is shown in the following table 3:
TABLE 3
| Composition (I) | C | Si | Mn | P | S | V | Ti | Cr |
| Content (%) | 4.21 | 0.16 | 0.24 | 0.169 | 0.072 | 0.224 | 0.266 | 0.11 |
By comparing the results of the above examples and comparative examples, it can be seen that the method provided by the present invention can significantly reduce the content of iron oxide in the vanadium slag, the content of iron oxide is reduced by 5.37%, and further the grade of vanadium in the vanadium slag is also improved by 1.21%.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (7)
1. A method for reducing the content of iron oxide in vanadium slag is characterized by comprising the following steps: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; the protective atmosphere is provided by a spray gun; the spray gun is pulled in a reciprocating manner for 3-5 times between 1m and 1.5 m; the protective atmosphere comprises nitrogen and/or argon.
2. The method of claim 1, wherein the additive is added in an amount of 2 to 3kg per ton of iron.
3. The method of claim 1, wherein the additive comprises 1 or a combination of at least 2 of coke breeze, aluminum chips, charcoal, petroleum coke, semicoke, pitch coke, or bituminous coal.
4. The method of claim 1, wherein the particle size of the additive is 1-5 mm.
5. The method of claim 1, wherein the reaction time is 60 to 100 s.
6. The method of claim 1, wherein the pressure of the protective atmosphere is 1 to 3 MPa.
7. The method of any one of claims 1-6, wherein the method comprises: after the converter vanadium extraction blowing is finished, adding an additive into the converter and reacting under a protective atmosphere to obtain vanadium slag; wherein the additive is added in an amount of 2-3 kg/ton iron; the additive comprises 1 or at least 2 of coke powder, aluminum scraps, charcoal, petroleum coke, semicoke, pitch coke or bituminous coal; the particle size of the additive is 1-5 mm; the protective atmosphere comprises nitrogen and/or argon; the reaction time is 60-100 s; the protective atmosphere is provided by a spray gun; the spray gun is pulled in a reciprocating manner for 3-5 times between 1m and 1.5 m; the pressure of the protective atmosphere is 1-3 MPa.
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|---|---|---|---|---|
| FR875418A (en) * | 1940-09-06 | 1942-09-21 | Dortmund Hoerder Hu Ttenver A | Process for obtaining a slag rich in vanadium during the refining of a vanaded iron in a basic converter |
| WO1998004750A1 (en) * | 1996-07-24 | 1998-02-05 | 'holderbank' Financiere Glarus Ag | Method for separating titanium and/or vanadium from pig iron |
| CN101407852A (en) * | 2008-11-11 | 2009-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium slag from ultra-low vanadium-containing molten iron by using converter |
| CN105349728A (en) * | 2015-11-26 | 2016-02-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for simultaneously conducting dephosphorization and vanadium extraction on vanadium-contained molten iron through converter |
| CN107312905A (en) * | 2017-07-03 | 2017-11-03 | 攀枝花学院 | A kind of high-grade vanadium slag and preparation method thereof |
-
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- 2019-12-18 CN CN201911311436.1A patent/CN110904347B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR875418A (en) * | 1940-09-06 | 1942-09-21 | Dortmund Hoerder Hu Ttenver A | Process for obtaining a slag rich in vanadium during the refining of a vanaded iron in a basic converter |
| WO1998004750A1 (en) * | 1996-07-24 | 1998-02-05 | 'holderbank' Financiere Glarus Ag | Method for separating titanium and/or vanadium from pig iron |
| CN101407852A (en) * | 2008-11-11 | 2009-04-15 | 攀钢集团研究院有限公司 | Method for extracting vanadium slag from ultra-low vanadium-containing molten iron by using converter |
| CN105349728A (en) * | 2015-11-26 | 2016-02-24 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for simultaneously conducting dephosphorization and vanadium extraction on vanadium-contained molten iron through converter |
| CN107312905A (en) * | 2017-07-03 | 2017-11-03 | 攀枝花学院 | A kind of high-grade vanadium slag and preparation method thereof |
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