CN111647759B - Process for producing metallic chromium by taking aluminum-chromium slag as main material and performing vacuum decarburization in vacuum sintering furnace - Google Patents
Process for producing metallic chromium by taking aluminum-chromium slag as main material and performing vacuum decarburization in vacuum sintering furnace Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- 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
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/06—Dry methods smelting of sulfides or formation of mattes by carbides or the like
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22B5/02—Dry methods smelting of sulfides or formation of mattes
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- 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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Abstract
A process for producing metallic chromium by using aluminum chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace comprises the steps of mixing the aluminum chromium slag with a carbonaceous raw material, putting the mixture into a three-phase arc furnace for smelting, naturally cooling, and separating out lower-layer chromium carbide; grinding chromium carbide, uniformly mixing with chromium oxide, explosion-proof fiber, carbonaceous raw material, methyl cellulose and water, pressing into a cylindrical mixed material rod, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat for 2-3 hours at 25-70 ℃, and reducing the vacuum degree to 10‑1And (4) continuously heating to 1300-1500 ℃ below Pa, carrying out vacuum sintering for 10-30 hours, and cooling along with the furnace to obtain the metal chromium. The advantages are that: the raw material cost is low, special production equipment and treatment means are not needed, the labor resource is saved, the process flow is simple, and the product extraction rate is high.
Description
Technical Field
The invention relates to a process for producing metal chromium by using aluminum chromium slag, in particular to a process for producing metal chromium by using aluminum chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace.
Background
The smelting of metal chromium uses chromite and the like as main raw materials, and comprises the steps of oxidizing roasting, leaching sodium chromate, preparing chromium hydroxide from the sodium chromate, precipitating, washing and filtering to obtain solid chromium hydroxide, calcining the chromium hydroxide in a rotary kiln to obtain chromium oxide, and finally preparing the metal chromium from the obtained chromium oxide by an aluminothermic reduction method.
CN 105568004A discloses a method for smelting metal chromium from aluminum chromium slag, which comprises the following steps: uniformly mixing aluminum-chromium slag with the particle size of less than or equal to 10mm and petroleum coke with the particle size of less than or equal to 10mm, drying the mixture in a drying kiln until the water content is less than or equal to 0.5%, adding the mixture into a three-phase electric arc furnace for smelting, carrying out high-temperature smelting, transferring liquid chromium carbide at the bottom of an electric arc furnace hearth into a plasma electric arc furnace, introducing oxygen into the hearth of the plasma electric arc furnace, adding calcium oxide and calcium fluoride serving as a slagging agent, introducing argon serving as protective gas into the plasma electric arc furnace after the high-temperature smelting, adding aluminum particles for continuous smelting to obtain qualified liquid metal chromium, pouring the liquid metal chromium into a sand shell mold, naturally cooling, removing impurities on the surface, and crushing to obtain the metal chromium. The method can obtain the metallic chromium with the purity of 96 wt% -99 wt%. However, the method needs to transfer the high-temperature molten chromium carbide into the plasma arc furnace in the three-phase arc furnace, and meanwhile, the operations of introducing protective gas, adding aluminum particles in the smelting process, introducing oxygen and the like are needed, the process is complex, and the three-phase arc furnace and the plasma arc furnace are high-power thermal equipment, so that the process cost is high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a process for producing metal chromium by taking aluminum chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace, which has low cost, simple process and high product extraction rate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a process for producing metallic chromium by using aluminum-chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace comprises the following steps:
(1) mixing the aluminum chromium slag and the carbonaceous raw material, putting the mixture into a three-phase electric arc furnace for smelting, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding the chromium carbide obtained in the step (1) into particles with the particle size of 80-150 meshes, and uniformly mixing the chromium carbide, chromium oxide, explosion-proof fiber, a carbonaceous raw material, methyl cellulose and water according to a mass ratio of 70: (20-40), 70: (0-2) and 70: (0-4) and 70: (0-2) and 70: (0-2), pressing into a cylindrical mixed material rod, placing the cylindrical mixed material rod in a vacuum sintering furnace, preserving the heat for 2-3 hours at the temperature of 25-70 ℃, and reducing the vacuum degree to 10- 1And (4) continuously heating to 1300-1500 ℃ below Pa, carrying out vacuum sintering for 10-30 hours, and cooling along with the furnace to obtain the metal chromium.
More preferably, the mass ratio of the chromium carbide to the chromium oxide to the explosion-proof fiber to the carbonaceous raw material to the methylcellulose to the water is 70: (35-40), 70: (1.5-2) and 70: (3-4) and 70: (1.5-2) and 70: (1.5-2).
Preferably, the aluminum chromium slag particles are slag generated by smelting ferrochrome, and the main phases are corundum phase and aluminum chromium solid solution phase; the main chemical components of the aluminum chromium slag particles are as follows: al (Al)2O375 to 85 weight percent of Cr2O310 to 15 weight percent of CaO, less than or equal to 3 weight percent of CaO, Fe2O3Less than or equal to 2 weight percent, and less than or equal to 2 weight percent of MgO; wherein the grain diameter of the aluminum chromium slag is 0.1 mm-5 mm.
Further preferably, the chromium oxide contains Cr as a main chemical component2O3Not less than 99 wt%; the grain diameter of the chromium oxide is less than or equal to 200 meshes.
More preferably, the mixing bar has a diameter of 10mm to 50mm and a height of 10mm to 50 mm.
Preferably, the diameter of the explosion-proof fiber is less than or equal to 0.5mm, and the length of the explosion-proof fiber is 10-15 mm; the softening and shrinking temperature of the explosion-proof fiber is 100-130 ℃.
As a further preference, the carbonaceous feedstock in step (1) and step (2) comprises at least one of petroleum coke, graphite, carbon black.
Further preferably, when the temperature is further raised in the step (2), the temperature raising rate is 10 to 20 ℃/min.
Preferably, the mass ratio of the aluminum chromium slag to the carbonaceous raw material in the step (1) is 100: (3-4).
More preferably, in the step (1), when the three-phase arc furnace is used for smelting, the smelting temperature is 1900 to 2000 ℃, and the smelting time is 4 to 8 hours.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the raw materials used in the invention are low in price, and the aluminum chromium slag belongs to industrial solid waste and has environmental hazard.
2. The invention does not need special production equipment and treatment means, saves labor resources and has simple process flow.
3. The invention utilizes the carbonization reaction between the aluminum chromium slag and the carbon element and the difference of the specific gravity of the reaction product to realize the high-efficiency separation of the chromium element and the aluminum element in the aluminum chromium slag.
4. The present invention utilizes chromium carbide and Cr2O3The decarburization-deoxidation reaction is carried out to realize the preparation of the metal chromium.
5. The invention presses the material into a cylinder, which is beneficial to the discharge of gas, and utilizes the high-temperature loss of the explosion-proof fiber to generate a gas channel, thereby being beneficial to the implementation of decarburization-deoxidation reaction, and the prepared chromium metal has no unreacted area and high product extraction rate.
The chromium metal prepared by the invention is determined as follows: the Cr content of the metal chromium is 91-95 wt%.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
In order to avoid repetition, the raw materials related to this specific embodiment are uniformly described as follows, and are not described in detail in the embodiments:
a. the aluminum chromium slag particles are slag generated by smelting ferrochrome, and the main phases are corundum phase and aluminum chromium solid solution phase; wherein, the main chemical components of the aluminum chromium slag particles are as follows: al (Al)2O375 to 85 weight percent of Cr2O310 to 15 weight percent of CaO, less than or equal to 3 weight percent of CaO, Fe2O3Less than or equal to 2 weight percent, and less than or equal to 2 weight percent of MgO; the grain size of the aluminum-chromium slag is 0.1 mm-5 mm;
b. main chemical component Cr of chromium oxide2O3Not less than 99 wt%; the grain size of the chromium oxide is not more than 200 meshes;
c. the diameter of the explosion-proof fiber is less than or equal to 0.5mm, and the length is 10 mm-15 mm; the softening and shrinking temperature of the explosion-proof fiber is 100-130 ℃;
d. the carbonaceous raw material comprises at least one of petroleum coke, graphite and carbon black.
Example 1
(1) Mixing the aluminum-chromium slag and the coke according to the mass ratio of 100:3.5, putting the mixture into a three-phase arc furnace at the temperature of 1900-2000 ℃, smelting for 6 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding chromium carbide into particles with the particle size of 80-150 meshes, uniformly mixing the chromium carbide and chromium oxide according to the mass ratio of 70:20, pressing into a cylindrical mixed material rod with the diameter of 10mm and the height of 10mm, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat at 50 ℃ for 2.5 hours and reducing the vacuum degree to 10-1And (3) continuously raising the temperature to 1400 ℃ at the speed of 15 ℃/min below Pa, carrying out vacuum sintering at the temperature of 1400-1450 ℃ for 20 hours, and cooling along with the furnace to obtain the metal chromium.
The chromium metal prepared by the invention is determined as follows: the Cr content in the metallic chromium is 91.00 wt%.
Example 2
(1) Mixing the aluminum-chromium slag and the coke according to the mass ratio of 100:3.5, putting the mixture into a three-phase arc furnace at the temperature of 1900-2000 ℃, smelting for 6 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding chromium carbide into particles with the particle size of 80-150 meshes, uniformly mixing the chromium carbide, chromium oxide, explosion-proof fiber, coke, methyl cellulose and water according to the mass ratio of 70:25:0.5:1:0.5:0.5, pressing into a cylindrical mixed material rod with the diameter of 20mm and the height of 20mm, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat at 50 ℃ for 2.5 hours, and reducing the vacuum degree to 10-1And (3) Pa below, raising the temperature to 1400 ℃ at the speed of 15 ℃/min, sintering for 20 hours in vacuum at the temperature of 1400-1450 ℃, and cooling along with the furnace to obtain the metal chromium.
The chromium metal prepared by the invention is determined as follows: the Cr content of the metallic chromium is 92.52 wt%.
Example 3
(1) Mixing the aluminum-chromium slag and the coke according to the mass ratio of 100:3.5, putting the mixture into a three-phase arc furnace at the temperature of 1900-2000 ℃, smelting for 6 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) mixing carbonGrinding chromium into powder with the granularity of 80-150 meshes, and then mixing chromium carbide, chromium oxide, explosion-proof fiber and coke: uniformly mixing methyl cellulose and water according to the mass ratio of 70:30:1:2:1:1, pressing into a cylindrical mixture rod with the diameter of 20mm and the height of 20mm, placing the cylindrical mixture rod in a vacuum sintering furnace, preserving the heat at 50 ℃ for 2.5 hours and reducing the vacuum degree to 10-1And (3) Pa below, raising the temperature to 1400 ℃ at the speed of 15 ℃/min, sintering for 20 hours in vacuum at the temperature of 1400-1450 ℃, and cooling along with the furnace to obtain the metal chromium.
The chromium metal prepared by the invention is determined as follows: the Cr content of the metallic chromium is 94.09 wt%.
Example 4
(1) Mixing the aluminum-chromium slag and the coke according to the mass ratio of 100:3.5, putting the mixture into a three-phase arc furnace at the temperature of 1900-2000 ℃, smelting for 6 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding chromium carbide into particles with the particle size of 80-150 meshes, uniformly mixing the chromium carbide, chromium oxide, explosion-proof fiber, coke, methyl cellulose and water according to the mass ratio of 70:40:2:4:2:2, pressing into a cylindrical mixed material rod with the diameter of 20mm and the height of 20mm, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat at 50 ℃ for 2.5 hours, and reducing the vacuum degree to 10-1And (3) Pa below, raising the temperature to 1400 ℃ at the speed of 15 ℃/min, sintering for 20 hours in vacuum at the temperature of 1400-1450 ℃, and cooling along with the furnace to obtain the metal chromium.
The chromium metal prepared by the invention is determined as follows: the Cr content of the metallic chromium is 95.00 wt%.
Example 5
(1) Mixing the aluminum-chromium slag and the coke according to the mass ratio of 100:3.5, putting the mixture into a three-phase arc furnace at the temperature of 1900-2000 ℃, smelting for 6 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding chromium carbide into particles with the particle size of 80-150 meshes, uniformly mixing the chromium carbide, chromium oxide, explosion-proof fiber, coke, methyl cellulose and water according to the mass ratio of 70:35:1.5:3:1.5:1.5, pressing into a cylindrical mixed material rod with the diameter of 20mm and the height of 20mm, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat for 2.5 hours at 50 ℃, and reducing the vacuum degree to 10-1Heating to 1400 deg.C at a rate of 15 deg.C/min under Pa, vacuum sintering at 1400-1450 deg.C for 20 hr, and furnace cooling to obtain the final productTo metallic chromium.
The chromium metal prepared by the invention is determined as follows: the Cr content in the metallic chromium is 94.52 wt%.
The aluminum-chromium slag, the coke, the chromium oxide and the explosion-proof fiber in the embodiments 1 to 5 of the invention are produced by selecting the raw materials of the same batch.
TABLE 1 raw material proportioning Table for examples 1 to 5 of the present invention (unit: parts by mass)
Examples | Chromium carbide | Chromium oxide | Explosion-proof fiber | Coke | Methyl cellulose | Water (W) |
Example 1 | 70 | 20 | 0 | 0 | 0 | 0 |
Example 2 | 70 | 25 | 0.5 | 1 | 0.5 | 0.5 |
Example 3 | 70 | 30 | 1 | 2 | 1 | 1 |
Example 4 | 70 | 40 | 2 | 4 | 2 | 2 |
Example 5 | 70 | 35 | 1.5 | 3 | 1.5 | 1.5 |
TABLE 2 table (wt%) of results of physical and chemical component measurements of inventive examples 1 to 5
As can be seen from Table 1, the metallic chromium with different physicochemical compositions is obtained by the method of the invention, and with the increase of the addition of the chromium oxide, the explosion-proof fiber, the coke, the methylcellulose and the water, the content of Cr element in the obtained metallic chromium is increased, C, O, Al and Fe element are reduced, the content of P and S is basically unchanged, and the content of Cr element in example 4 is the highest.
Example 6
(1) Mixing the aluminum chromium slag and the petroleum coke according to the mass ratio of 100:3, putting the mixture into a three-phase arc furnace at the temperature of 1900-2000 ℃, smelting for 8 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding chromium carbide into particles with the particle size of 80-150 meshes, uniformly mixing the chromium carbide, chromium oxide, explosion-proof fiber, coke, methyl cellulose and water according to the mass ratio of 70:40:2:4:2:2, pressing into a cylindrical mixed material rod with the diameter of 30mm and the height of 30mm, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat for 3 hours at the temperature of 20 ℃, and reducing the vacuum degree to 10-1Heating to 1300 ℃ at the speed of 20 ℃/min under Pa, sintering for 30 hours in vacuum at the temperature of 1300-1350 ℃, and cooling along with the furnace to obtain the metal chromium.
Example 7
(1) Mixing the aluminum-chromium slag and graphite according to the mass ratio of 100:4, putting the mixture into a three-phase electric arc furnace at the temperature of 1900-2000 ℃, smelting for 4 hours, naturally cooling, and separating out lower-layer chromium carbide;
(2) grinding chromium carbide into particles with the particle size of 80-150 meshes, uniformly mixing the chromium carbide, chromium oxide, explosion-proof fiber, coke, methyl cellulose and water according to the mass ratio of 70:40:2:4:2:2, pressing into a cylindrical mixed material rod with the diameter of 50mm and the height of 50mm, placing the cylindrical mixed material rod into a vacuum sintering furnace, preserving heat for 2 hours at 70 ℃, and reducing the vacuum degree to 10-1Heating to 1450 deg.c at 10 deg.c/min under Pa, vacuum sintering at 1450-1500 deg.c for 10 hr, and furnace cooling to obtain chromium metal.
Table 3 table (wt%) of results of physical and chemical component measurement of examples 6 and 7 of the present invention
Examples | Cr | C | O | Al | Fe | P | S |
Example 6 | 93.89 | 0.89 | 1.02 | 2.19 | 1.95 | 0.03 | 0.02 |
Example 7 | 93.69 | 0.97 | 0.87 | 2.34 | 1.99 | 0.03 | 0.02 |
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A process for producing metallic chromium by using aluminum chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace is characterized by comprising the following steps of:
the method comprises the following steps:
(1) mixing the aluminum-chromium slag with a carbonaceous raw material, wherein the carbonaceous raw material comprises at least one of petroleum coke, graphite and carbon black; the mass ratio of the aluminum chromium slag to the carbonaceous raw material is 100: (3-4); smelting in a three-phase arc furnace at 1900-2000 deg.c for 4-8 hr, and naturally cooling to separate out lower chromium carbide layer;
(2) grinding the chromium carbide obtained in the step (1) into particles with the particle size of 80-150 meshes, and uniformly mixing the chromium carbide, chromium oxide, explosion-proof fibers, a carbonaceous raw material, methyl cellulose and water, wherein the carbonaceous raw material comprises at least one of petroleum coke, graphite and carbon black;
the mass ratio of the chromium carbide to the chromium oxide to the explosion-proof fiber to the carbonaceous raw material to the methyl cellulose to the water is 70: (35-40), 70: (1.5-2) and 70: (3-4) and 70: (1.5-2) and 70: (1.5-2), the diameter of the explosion-proof fiber is less than or equal to 0.5mm, and the length of the explosion-proof fiber is 10-15 mm; the softening and shrinking temperature of the explosion-proof fiber is 100-130 ℃, the explosion-proof fiber is pressed into a cylindrical mixing rod, the diameter of the mixing rod is 20mm, the height of the mixing rod is 20mm, the mixing rod is placed in a vacuum sintering furnace, the temperature is kept at 25-70 ℃ for 2-3 hours, and the vacuum degree is reduced to 10-1And (4) continuously heating to 1300-1500 ℃ below Pa, carrying out vacuum sintering for 10-30 hours, and cooling along with the furnace to obtain the metal chromium.
2. The process for producing metallic chromium by using aluminum-chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace according to claim 1, which is characterized by comprising the following steps: the aluminum chromium slag particles are smelting ferrochromium alloyThe main phases of the generated slag are corundum phase and aluminum chromium solid solution phase; the main chemical components of the aluminum chromium slag particles are as follows: al (Al)2O375 to 85 weight percent of Cr2O310 to 15 weight percent of CaO, less than or equal to 3 weight percent of CaO, Fe2O3Less than or equal to 2 weight percent, and less than or equal to 2 weight percent of MgO; wherein the grain diameter of the aluminum chromium slag is 0.1 mm-5 mm.
3. The process for producing metallic chromium by using aluminum-chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace according to claim 1, which is characterized by comprising the following steps: the main chemical component Cr of the chromium oxide2O3Not less than 99 wt%; the grain diameter of the chromium oxide is less than or equal to 200 meshes.
4. The process for producing metallic chromium by using aluminum-chromium slag as a main material and performing vacuum decarburization in a vacuum sintering furnace according to claim 1, which is characterized by comprising the following steps: and (3) when the temperature is continuously increased in the step (2), the temperature increasing speed is 10-20 ℃/min.
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CN105568004A (en) * | 2016-03-03 | 2016-05-11 | 锦州集信高温材料有限公司 | Method for smelting chromium metal from aluminum-chromium slag in electric arc furnace |
CN105861818A (en) * | 2015-01-23 | 2016-08-17 | 鞍钢股份有限公司 | High performance composite bentonite for pelletizing |
CN107779613A (en) * | 2017-10-30 | 2018-03-09 | 王景军 | A kind of crome metal smelting process of low-aluminum-content |
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JPS63199833A (en) * | 1987-02-13 | 1988-08-18 | Tosoh Corp | Manufacture of high-purity metallic chromium |
JPH07216474A (en) * | 1994-01-31 | 1995-08-15 | Tosoh Corp | Production of high purity metallic chromium |
CN102557715A (en) * | 2012-01-18 | 2012-07-11 | 晋城市富基新材料股份有限公司 | Molding sintering process of alpha-alumina |
CN105861818A (en) * | 2015-01-23 | 2016-08-17 | 鞍钢股份有限公司 | High performance composite bentonite for pelletizing |
CN105568004A (en) * | 2016-03-03 | 2016-05-11 | 锦州集信高温材料有限公司 | Method for smelting chromium metal from aluminum-chromium slag in electric arc furnace |
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