CN111809061A - Method for smelting titanium-silicon-aluminum intermediate alloy by reducing titanium-containing blast furnace slag with atmosphere protection aluminum - Google Patents
Method for smelting titanium-silicon-aluminum intermediate alloy by reducing titanium-containing blast furnace slag with atmosphere protection aluminum Download PDFInfo
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- CN111809061A CN111809061A CN202010710778.7A CN202010710778A CN111809061A CN 111809061 A CN111809061 A CN 111809061A CN 202010710778 A CN202010710778 A CN 202010710778A CN 111809061 A CN111809061 A CN 111809061A
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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
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B3/00—General features in the manufacture of pig-iron
- C21B3/04—Recovery of by-products, e.g. slag
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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
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1263—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction
- C22B34/1277—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining metallic titanium from titanium compounds, e.g. by reduction using other metals, e.g. Al, Si, Mn
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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
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- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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Abstract
The invention relates to a method for smelting a titanium-silicon-aluminum intermediate alloy by reducing titanium-containing blast furnace slag with atmosphere protective aluminum, belonging to the technical field of metallurgy. The method for smelting the titanium-silicon-aluminum intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protective aluminum comprises the following steps: A. mixing titanium-containing blast furnace slag, aluminum powder, lime and a fluxing agent according to a mass ratio of 100: 30-50: 20-28: 0-10, and reacting under the condition of blowing Ar protection or protection of vacuum degree of 1-1000 Pa and at the temperature of 1500-1700 ℃; B. after the reaction is finished, the reaction product is isolated from air and cooled to room temperature, and then crushing and deslagging are carried out, so as to obtain the titanium-containing intermediate alloy of titanium, silicon and aluminum. The alloy phase prepared by the method has high titanium content and low silicon and iron content, and can realize economic titanium extraction, thereby greatly reducing the waste of titanium resources.
Description
Technical Field
The invention relates to a method for smelting a titanium-silicon-aluminum intermediate alloy by reducing titanium-containing blast furnace slag with atmosphere protective aluminum, belonging to the technical field of metallurgy.
Background
The high titanium blast furnace slag is rich in a large amount of titanium dioxide resources besides calcium oxide, magnesium oxide, silicon dioxide, aluminum oxide, iron oxide, metallic iron, physical sensible heat and other resources, and is a valuable strategic resource and a secondary resource. The Panzhihua titanium resource accounts for 90 percent of the national titanium resource, and the titanium resource in the Panzhihua high-titanium blast furnace slag accounts for about 50 percent of the Panzhihua titanium resource. Therefore, it is necessary to use Panzhihua high titanium type blast furnace slag as comprehensively as possible. The main chemical components of the Panzhihua high titanium type blast furnace slag are shown in Table 1.
TABLE 1 Panzhihua high-titanium blast furnace slag composition
The application numbers are: the patent application CN2013101343150 discloses a titanium extraction process of a titanium-containing blast furnace slag by an aluminothermic method, which comprises the following steps: the main component is TiO2、SiO2、CaO、Al2O3Crushing and grinding the MgO titanium-containing blast furnace slag to 180 meshes; mixing the slag, the aluminum powder and the CaO according to a certain mass ratio; aluminothermic reduction: under the protection atmosphere of argon, the temperature of the tubular electric furnace is raised to a given temperature, the mixed ingredients are put into an alumina crucible, and the tubular electric furnace is put into the tubular electric furnace at a high temperature and is kept for a certain time; water cooling: taking out at high temperature, and cooling in water; the slag and the alloy are mechanically separated. The invention reduces the pretreated titanium-containing blast furnace slag by using aluminum powder, and separates slag and metal by water cooling after the reduction is finished. Finally, the slag mainly comprises CaO, MgO and Al2O3(ii) a The metal components are Si and Ti, and a small amount of Al is also included. In fact, this method has no practical operation guide meaning, and repeating the operation does not produce a metal-like aggregate in the form of a lump, a granule, a sphere or the like after cooling.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for smelting a titanium-silicon-aluminum intermediate alloy by reducing titanium-containing blast furnace slag with atmosphere protective aluminum, wherein the titanium-silicon-aluminum alloy obtained by the method has high titanium content.
In order to solve the technical problem, the method for smelting the titanium-silicon-aluminum intermediate alloy by reducing the titanium-containing blast furnace slag by the atmosphere protective aluminum comprises the following steps:
A. mixing titanium-containing blast furnace slag, aluminum, lime and a fluxing agent according to a mass ratio of 100: 30-50: 20-28: 0-10, and reacting under the conditions of Ar blowing protection or vacuum degree protection of 1-1000 Pa and temperature of 1500-1700 ℃;
B. after the reaction is finished, the reaction product is isolated from air and cooled to room temperature, and then crushing and deslagging are carried out, so as to obtain the titanium-containing intermediate alloy of titanium, silicon and aluminum.
Preferably, the mass ratio of the titanium-containing blast furnace slag to the aluminum to the lime to the fluxing agent is 100: 30-50: 20-24: 0-10.
Preferably, the mass ratio of the titanium-containing blast furnace slag to the aluminum to the lime to the fluxing agent is 100: 30-50: 22-24: 5-10.
Preferably, the fluxing agent is fluorite, KCl, BaO and Li2At least one of O.
Further, when the titanium-containing blast furnace slag is in a solid state, the titanium-containing blast furnace slag, aluminum, lime and a fluxing agent are uniformly mixed, and the ball is pressed to obtain a ball with the diameter of less than or equal to 40mm, and then the reaction is carried out.
Preferably, when the titanium-containing blast furnace slag is in a liquid state, aluminum, lime and a fluxing agent are sprayed into the liquid titanium-containing blast furnace slag for reaction, and preferably, the spraying is Ar or mechanical spraying.
Preferably, in the step A, the granularity of the titanium-containing blast furnace slag, the aluminum, the lime and the fluxing agent is less than or equal to 0.5 mm.
Preferably, the mixing degree is more than or equal to 98.5%.
Preferably, the reaction time is 0.1-1 h.
Preferably, the reaction time is 10-60 min.
Has the advantages that:
the method adopts vacuum decompression protection or Ar blowing protection aluminum reduction reaction to extract titanium from the titanium-containing blast furnace slag, and the titanium-silicon-aluminum alloy prepared by the method has high titanium content and less impurities. Preferably, the titanium-silicon-aluminum containing 41.97% of Ti, 30.13% of Si, 3.8% of Al and 21.38% of Fe can be obtained. Compared with the prior art, the titanium content in the alloy is improved by 7.97 percent, the silicon content in the alloy is reduced by 7.27 percent, the iron content is reduced by 4.3 percent, the economic titanium extraction can be realized, and the waste of titanium resources is greatly reduced.
Drawings
FIG. 1: schematic diagram of experimental reaction device;
FIG. 2: example 5 reaction alloy product and slag, alloy separation effect diagram;
FIG. 3: example 5 scanning electron micrographs of the reaction alloy product.
Detailed Description
In order to solve the technical problem, the method for smelting the titanium-silicon-aluminum intermediate alloy by reducing the titanium-containing blast furnace slag by the atmosphere protective aluminum comprises the following steps:
A. mixing titanium-containing blast furnace slag, aluminum, lime and a fluxing agent according to a mass ratio of 100: 30-50: 20-28: 0-10, and reacting under the conditions of Ar blowing protection or vacuum degree protection of 1-1000 Pa and temperature of 1500-1700 ℃;
B. after the reaction is finished, the reaction product is isolated from air and cooled to room temperature, and then crushing and deslagging are carried out, so as to obtain the titanium-containing intermediate alloy of titanium, silicon and aluminum.
Preferably, the mass ratio of the titanium-containing blast furnace slag to the aluminum to the lime to the fluxing agent is 100: 30-50: 20-24: 0-10.
Preferably, the mass ratio of the titanium-containing blast furnace slag to the aluminum to the lime to the fluxing agent is 100: 30-50: 22-24: 5-10.
Preferably, the fluxing agent is fluorite, KCl, BaO and Li2At least one of O.
Further, when the titanium-containing blast furnace slag is in a solid state, the titanium-containing blast furnace slag, aluminum, lime and a fluxing agent are uniformly mixed, and the ball is pressed to obtain a ball with the diameter of less than or equal to 40mm, and then the reaction is carried out.
Preferably, when the titanium-containing blast furnace slag is in a liquid state, aluminum, lime and a fluxing agent are sprayed into the liquid titanium-containing blast furnace slag for reaction, and preferably, the spraying is Ar or mechanical spraying.
Preferably, in the step A, the granularity of the titanium-containing blast furnace slag, the aluminum, the lime and the fluxing agent is less than or equal to 0.5 mm.
Preferably, the mixing degree is more than or equal to 98.5%.
Preferably, the reaction time is 0.1-1 h.
Preferably, the reaction time is 10-60 min.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Examples 1 to 6
The method for extracting titanium from the titanium-containing blast furnace slag through vacuum decompression protection and aluminothermic reduction for smelting titanium-silicon-aluminum alloy comprises the following steps:
A. respectively crushing the solid titanium-containing blast furnace slag, the aluminum powder, the lime and the fluorite to the particle size of 0.5 mm; uniformly mixing 100g of solid titanium-containing blast furnace slag, 30-50 g of aluminum powder, 20-28 g of lime and 0-10 g of fluorite until the mixing degree is more than or equal to 98.5%, pelletizing and drying to obtain a pellet material; putting the pellet material into a vacuum reduction reaction device shown in figure 1, and performing vacuum reduced atmosphere protection aluminum reduction metallurgical reaction for 0.5h under the conditions that the temperature is 1550 ℃ and the vacuum degree is 100 Pa;
B. after the reaction is finished, the reaction product is isolated from air and cooled to room temperature, and then the titanium-silicon-aluminum alloy is obtained after slag and alloy are mechanically separated. The experimental results data are shown in table 2 below.
Table 2 example results data
Example 5 reaction alloy product and slag, alloy separation effect figure details 2. Example 5 scanning electron micrographs of the reaction alloy product are detailed in figure 3. As can be seen from figure 2, the alloy product of the invention is easy to separate from slag, the automatic separation effect of the slag and the alloy is good, and the boundary line of the slag and the alloy is obvious. As can be seen from FIG. 3, the alloy of the present invention has uniform structure and clear structure.
Comparative example 1
According to the formula of 201310134315.0, 100g of blast furnace slag, 25.98g of aluminum powder and 5g of lime are weighed according to the proportion of 100:25.98:5 Al: CaO, and are reduced at 1550 ℃ for 30min under the protection of argon blowing, and metallic aggregates which are obviously in the shapes of blocks, particles, spheres and the like are not seen in the cooled product.
Claims (10)
1. The method for smelting the titanium-silicon-aluminum intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protective aluminum is characterized by comprising the following steps of:
A. mixing titanium-containing blast furnace slag, aluminum, lime and a fluxing agent according to a mass ratio of 100: 30-50: 20-28: 0-10, and reacting under the conditions of Ar blowing protection or vacuum degree protection of 1-1000 Pa and temperature of 1500-1700 ℃;
B. after the reaction is finished, the reaction product is isolated from air and cooled to room temperature, and then crushing and deslagging are carried out, so as to obtain the titanium-containing intermediate alloy of titanium, silicon and aluminum.
2. The method for smelting the titanium-silicon-aluminum intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protecting aluminum according to claim 1, wherein the titanium-containing blast furnace slag, the aluminum, the lime and the fluxing agent are in a mass ratio of 100: 30-50: 20-24: 0-10.
3. The method for smelting the TiSi-Al intermediate alloy by atmosphere protection aluminum reduction of the titanium-containing blast furnace slag according to claim 1 or 2, wherein the titanium-containing blast furnace slag, the aluminum, the lime and the fluxing agent are in a mass ratio of 100: 30-50: 22-24: 5-10.
4. The method for smelting the SiAl intermediate alloy by atmosphere protection aluminum reduction titanium-containing blast furnace slag according to any one of claims 1 to 3, wherein the fluxing agent is fluorite, KCl, BaO, Li2At least one of O.
5. The method for smelting the SiAl intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protective aluminum according to any one of claims 1 to 4, wherein when the titanium-containing blast furnace slag is in a solid state, the titanium-containing blast furnace slag, the aluminum, the lime and the fluxing agent are uniformly mixed, and the mixture is pressed into balls with the diameter of less than or equal to 40mm for reaction.
6. The method for smelting the TiSi-Al intermediate alloy by atmosphere protecting aluminum reduction of the titanium-containing blast furnace slag according to any one of claims 1 to 5, wherein when the titanium-containing blast furnace slag is in a liquid state, aluminum, lime and a fluxing agent are sprayed into the liquid titanium-containing blast furnace slag for reaction, preferably, the spraying is Ar or mechanical spraying.
7. The method for smelting the SiAl intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protecting aluminum according to any one of claims 1 to 5, wherein in the step A, the granularity of the titanium-containing blast furnace slag, the aluminum, the lime and the fluxing agent is less than or equal to 0.5 mm.
8. The method for smelting the TiSi-Al intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protecting aluminum according to any one of claims 1 to 5, wherein the mixing degree is more than or equal to 98.5%.
9. The method for smelting the TiSi-Al intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protecting aluminum according to any one of claims 1 to 8, wherein the reaction time is 0.1 to 1 hour.
10. The method for smelting the titanium-silicon-aluminum intermediate alloy by reducing the titanium-containing blast furnace slag with the atmosphere protecting aluminum according to claim 9, wherein the reaction time is 10-60 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115896494A (en) * | 2022-11-11 | 2023-04-04 | 攀枝花学院 | Method for smelting titanium-silicon alloy by reducing titanium-containing blast furnace slag with silicon |
| TWI823758B (en) * | 2023-01-19 | 2023-11-21 | 中國鋼鐵股份有限公司 | Composition of blast furnace mud containing silicon-aluminum oxide mineral powder and method of manufacture |
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| CN101067171A (en) * | 2007-06-08 | 2007-11-07 | 东北大学 | Vacuum induction smelting producing high-quality high-titanium iron method based on aluminothermic reduction |
| CN103173628A (en) * | 2013-04-18 | 2013-06-26 | 北京科技大学 | Process for extracting titanium from titanium-containing blast furnace slag through aluminothermic method |
| CN107400741A (en) * | 2016-05-18 | 2017-11-28 | 鞍钢股份有限公司 | One kind melting titanium-containing blast furnace slag smelting low-silicon ferrotianium technique |
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2020
- 2020-07-22 CN CN202010710778.7A patent/CN111809061A/en active Pending
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| CN101067171A (en) * | 2007-06-08 | 2007-11-07 | 东北大学 | Vacuum induction smelting producing high-quality high-titanium iron method based on aluminothermic reduction |
| CN103173628A (en) * | 2013-04-18 | 2013-06-26 | 北京科技大学 | Process for extracting titanium from titanium-containing blast furnace slag through aluminothermic method |
| CN107400741A (en) * | 2016-05-18 | 2017-11-28 | 鞍钢股份有限公司 | One kind melting titanium-containing blast furnace slag smelting low-silicon ferrotianium technique |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115896494A (en) * | 2022-11-11 | 2023-04-04 | 攀枝花学院 | Method for smelting titanium-silicon alloy by reducing titanium-containing blast furnace slag with silicon |
| TWI823758B (en) * | 2023-01-19 | 2023-11-21 | 中國鋼鐵股份有限公司 | Composition of blast furnace mud containing silicon-aluminum oxide mineral powder and method of manufacture |
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