CN111519054A - Aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum and production method thereof - Google Patents

Aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum and production method thereof Download PDF

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CN111519054A
CN111519054A CN202010310693.XA CN202010310693A CN111519054A CN 111519054 A CN111519054 A CN 111519054A CN 202010310693 A CN202010310693 A CN 202010310693A CN 111519054 A CN111519054 A CN 111519054A
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aluminum
percent
less
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intermediate frequency
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CN111519054B (en
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刘新锋
李坤
赵文龙
袁志刚
赵蕾
李海峰
范钦玉
李铁峰
李晓庆
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Henan Zhongfu Technology Center Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/03Making non-ferrous alloys by melting using master alloys
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • C22C1/026Alloys based on aluminium
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/06Making non-ferrous alloys with the use of special agents for refining or deoxidising
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C21/00Alloys based on aluminium

Abstract

The invention discloses an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum, which comprises the following components in percentage by weight: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of V, less than or equal to 0.0006 percent of Mn, less than or equal to 0.0005 percent of Ti, 2.5 to 3.5 percent of P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurities and the balance of aluminum. The production method comprises the following steps: adding 99.95% of high-purity aluminum standard ingot into an intermediate frequency furnace, heating and melting, feeding potassium fluoborate ingredient into a material box, controlling the feeding temperature to be 720 ℃, keeping 30% of power of the intermediate frequency furnace in the feeding process, mechanically stirring by using a graphite carbonization stirrer, ensuring that the whole process does not exceed 750 ℃, adding alumina powder by using a special medium package, and treating the mixture at the casting temperature of 730-750 ℃. The aluminum intermediate alloy ingot product for high-efficiency purification of high-purity aluminum obtained by the invention has uniform boron B component and AlB2Uniform distribution of phase grainsThe cloth and the surface are bright and clean, no impurities exist, the product quality integrally reaches the highest level of the same industry, and the cloth and the surface are worth of popularization and use.

Description

Aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum and production method thereof
The technical field is as follows:
the invention relates to a composition of an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum and a production method thereof, which are widely applied to a production process for producing high-purity aluminum and belong to the technical field of aluminum deep processing.
Secondly, background art:
the production of high-purity aluminum requires that the impurity elements are as low as possible, so that the higher requirements are put on the used high-purity aluminum intermediate alloy, and the lower the impurity element content of the used intermediate alloy is, the better. Published AlB3The production method of the intermediate alloy has high impurity content, easily forms boride with a net-shaped amorphous structure by the components, and has low boron yield. In order to reduce energy consumption, reduce investment and shorten production period, the production process preparation method developed by the applicant is successful in breakthrough after the production practice research of nearly two years, and an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum and a production method thereof are produced.
Thirdly, the invention content:
the technical problem to be solved by the invention is as follows: provides a crystallized AlB with low impurity element content and uniform boron B component2The aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum with uniformly distributed phases and the production method thereof meet the requirements of markets and enterprises.
The technical scheme adopted by the invention for solving the technical problem is as follows:
an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following chemical components in percentage by mass: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of V, less than or equal to 0.0006 percent of Mn, less than or equal to 0.0005 percent of Ti, 2.5 to 3.5 percent of P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurities and the balance of aluminum.
The production method of the aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following specific steps:
A. firstly, adding 0.38 ton of high-purity aluminum standard ingot into a crucible of a 1 ton intermediate frequency furnace, and taking the rest 0.12 ton as a cooling ingot in the production process; wherein, the content requirement of the high-purity aluminum standard ingot is as follows: less than or equal to 0.01 percent of silicon Si, less than or equal to 0.01 percent of iron Fe, less than or equal to 0.001 percent of vanadium V, less than or equal to 0.001 percent of manganese Mn, less than or equal to 0.001 percent of titanium Ti, less than 0.002 percent of other single impurities, less than 0.002 percent of total impurities, and more than or equal to 99.95 percent of aluminum Al;
B. starting a crucible of the intermediate frequency furnace, raising the temperature for 40 minutes at a power of 60%, and fully melting and raising the temperature of the high-purity aluminum ingot to 720 ℃;
C. a 1.5m crucible shovel maintained by titanium dioxide shovels slag on the crucible wall from top to bottom along the crucible wall; then, a proper amount of slag removing agent is scattered, and slag is removed;
D. the quality requirement and the adding amount of the potassium fluoborate are calculated as follows:
the quality requirement is as follows: the mass fraction of the potassium fluoborate is more than or equal to 98 percent; white powder or crystal, and other impurities cannot be mixed;
the calculation method comprises the following steps: calculating the addition amount of potassium fluoborate according to the content of 2.5-3.5% of the boron internal control range, wherein the weight of the potassium fluoborate = the total weight of the high-purity aluminum standard ingot multiplied by 0.4;
E. adding the potassium fluoborate into a movable material box according to the calculated amount of the item D, and adding the potassium fluoborate into the intermediate frequency furnace in batches according to the process requirements;
F. after the potassium fluoborate is added and the layered solution is completely formed, the material conveying box is lifted, the smoke baffle plate is reserved to seal the furnace mouth, and the dense smoke is prevented from leaking; starting the power of a crucible of the intermediate frequency furnace to 60%, stirring for 30 minutes to fully alloy, and controlling the temperature to be below 830 ℃;
G. skimming upper layer of scum to a special slag basin, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag spoon maintained by titanium dioxide;
H. tipping the alloy aluminum liquid in the furnace and pouring the alloy aluminum liquid into a 1-ton transfer ladle, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a mixture of surface alumina powder and the solution by using a slag ladle maintained by titanium dioxide;
I. pouring the alloy aluminum liquid in the transfer ladle back into the crucible of the intermediate frequency furnace, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid again, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag ladle maintained by titanium dioxide;
J. controlling the temperature of the alloy aluminum liquid at 720-750 ℃, and casting to obtain an aluminum intermediate alloy material; wherein, the surface of the ingot mould for casting is maintained and treated by titanium dioxide.
In the step E, the step of adding the potassium fluoborate into the crucible of the intermediate frequency furnace in batches comprises the following steps:
firstly, a movable material box is hoisted to a furnace mouth of an intermediate frequency furnace, two sealed smoke baffle plates are installed at the furnace mouth of the intermediate frequency furnace, and a feed opening of the movable material box is fed into the intermediate frequency furnace through the smoke baffle plates, wherein the movable material box, the smoke baffle plates and the intermediate frequency furnace are tightly assembled, and more than 99% of dense smoke generated in the production process is collected by a dust collector to reach the environmental protection emission standard;
secondly, controlling the temperature of high-purity aluminum liquid in a crucible of the intermediate frequency furnace to be 720 +/-5 ℃, adjusting the power to be 30 percent, controlling the frequency to be 150-160 Hz, opening a discharge port valve of a movable material box, discharging a small amount of the aluminum liquid to the surface of the highest rolling position of the aluminum liquid, and taking the standard that the contacted potassium fluoborate is quickly dispersed to the periphery of the aluminum liquid and aggregation does not occur; meanwhile, a graphite silicon carbide impeller stirrer is used for mechanically stirring the surface of the aluminum liquid, so that potassium fluoborate is prevented from condensing and burning, the temperature in the small-amount feeding process is controlled at 750 ℃, and when the temperature is ultrahigh, a high pure aluminum standard ingot is added for timely cooling;
thirdly, during the feeding process, 1kg of potassium fluotitanate is added for each time when the molten aluminum is sticky, and the whole feeding process is carried out for 5 times;
fourthly, potassium fluoborate is generated around the rolling aluminum liquid to form a layered solution, and when the ring surface reaches the radius, the material box is started to start a large amount of material discharging;
mechanically stirring the surface of the aluminum liquid by using a graphite silicon carbide impeller stirrer in the blanking process to avoid the coagulation of potassium fluoborate, controlling the temperature of the aluminum liquid below 780 ℃ in the feeding process, and increasing a pure aluminum standard ingot to cool in time when the temperature is ultrahigh;
sixthly, when the potassium fluoborate in the material box is completely discharged, the residual high-purity aluminum standard ingot is also completely added into the crucible of the intermediate frequency furnace, so that the high-purity aluminum standard ingot is fully mixed and completely reacted.
In step ③, the addition of 1 kg/time of potassium fluotitanate when the aluminum liquid is tacky means that the layered solution generated after the potassium fluoborate is added into the alloy aluminum liquid is treated, the fluidity can be improved through stirring reaction, and TiB is preferentially generated2Promotes the boron to generate higher absorption rate in the aluminum liquid at lower temperature, and the TiB2The conductivity of the aluminum liquid is not greatly influenced.
The parameters of the aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum produced by the invention are as follows:
alloy components: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of V, less than or equal to 0.0006 percent of Mn, less than or equal to 0.0005 percent of Ti, 2.5 to 3.5 percent of P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurity content, and the balance of aluminum;
the product specification is as follows: 680 x 95 x 50 mm;
the product appearance is as follows: the surface is smooth and bright, and no flash, burr, slag and the like exist;
fracture organization: the AlB2 phase crystal grains are evenly distributed, and have no net structure, inclusion and other defects.
The invention can produce the following positive effects:
1. by adopting a thermal reduction method, potassium fluoborate reacts with high-purity aluminum liquid in a crucible of an intermediate frequency furnace, the stirring force is high, and the potassium fluoborate aggregation loss is avoided; simultaneously, graphite silicon nitride impeller mechanical stirring is used, so that AlB is effectively increased2The uniform distribution of phase grains destroys the generation of an amorphous reticular structure, and obviously improves the yield of boron.
2. The invention has strong pertinence, the whole process scheme is tested, summarized and improved for more than two years for countless times, the temperature parameter of each process reaction link of the alloy molten aluminum is accurate, the unnecessary waste of energy is avoided, and the AlB is avoided at the same time2Opposite AlB12The transformation of the alloy ingot influences the tissue structure of the alloy ingot and the quality of the product.
3. Book (I)The invention reasonably and accurately uses potassium fluotitanate, promotes boron to generate higher yield in aluminum liquid at lower temperature, and also destroys AlB2Amorphous network structure, improved fluidity.
4. The production preparation process uses alumina powder when treating surface solution, and uses a transfer ladle to repeatedly turn over, so that the obtained aluminum intermediate alloy ingot for high-efficiency purification of high-purity aluminum has bright and clean appearance.
5. The aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum produced by the production process scheme of the invention adopts the production processes of selection and use of proper raw and auxiliary materials, scientific feeding coefficient, stirring of a graphite silicon carbide stirrer added in an intermediate frequency furnace, strict temperature control of each channel, proper addition of proper amount of auxiliary materials of potassium fluotitanate and alumina powder in due time, introduction of a transfer platform bag to repeatedly treat solution on the surface of alloy aluminum liquid and the like, so that the boron B content of an alloy ingot is uniform, and the high-power tissue AlB is high2Uniform phase grain distribution, generation of an amorphous net structure, no inclusion, bright appearance and cleanness.
6. The aluminum intermediate alloy ingot produced by the invention has the product quality which integrally reaches the highest level of the same industry, is suitable for improving the purification effect and speed of high-purity aluminum production, and is worth popularizing and using.
Fourthly, the specific implementation mode:
the technical solutions of the present invention will be further described in detail and clearly in the following with reference to specific examples, but the scope of the present invention is not limited thereto.
Example 1:
an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following chemical components in percentage by mass: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of V, less than or equal to 0.0006 percent of Mn, less than or equal to 0.0005 percent of Ti, 2.5 percent of P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurities and the balance of aluminum.
The production method of the aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following specific steps:
A. firstly, adding 0.38 ton of high-purity aluminum standard ingot into a crucible of a 1 ton intermediate frequency furnace, and taking the rest 0.12 ton as a cooling ingot in the production process; wherein, the content requirement of the high-purity aluminum standard ingot is as follows: less than or equal to 0.01 percent of silicon Si, less than or equal to 0.01 percent of iron Fe, less than or equal to 0.001 percent of vanadium V, less than or equal to 0.001 percent of manganese Mn, less than or equal to 0.001 percent of titanium Ti, less than 0.002 percent of other single impurities, less than 0.002 percent of total impurities, and more than or equal to 99.95 percent of aluminum Al;
B. starting a crucible of the intermediate frequency furnace, raising the temperature for 40 minutes at a power of 60%, and fully melting and raising the temperature of the high-purity aluminum ingot to 720 ℃;
C. a 1.5m crucible shovel maintained by titanium dioxide shovels slag on the crucible wall from top to bottom along the crucible wall; then, a proper amount of slag removing agent is scattered, and slag is removed;
D. the quality requirement and the adding amount of the potassium fluoborate are calculated as follows:
the quality requirement is as follows: the mass fraction of the potassium fluoborate is more than or equal to 98 percent; white powder or crystal, and other impurities cannot be mixed;
the calculation method comprises the following steps: calculating the addition of potassium fluoborate according to the content of 2.5 percent of the boron internal control range, wherein the weight of the potassium fluoborate = the total weight of the high-purity aluminum standard ingot multiplied by 0.4;
E. adding the potassium fluoborate into a movable material box according to the calculated amount of the item D, and adding the potassium fluoborate into the intermediate frequency furnace in batches according to the process requirements;
F. after the potassium fluoborate is added and the layered solution is completely formed, the material conveying box is lifted, the smoke baffle plate is reserved to seal the furnace mouth, and the dense smoke is prevented from leaking; starting the power of a crucible of the intermediate frequency furnace to 60%, stirring for 30 minutes to fully alloy, and controlling the temperature to be below 830 ℃;
G. skimming upper layer of scum to a special slag basin, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag spoon maintained by titanium dioxide;
H. tipping the alloy aluminum liquid in the furnace and pouring the alloy aluminum liquid into a 1-ton transfer ladle, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a mixture of surface alumina powder and the solution by using a slag ladle maintained by titanium dioxide;
I. pouring the alloy aluminum liquid in the transfer ladle back into the crucible of the intermediate frequency furnace, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid again, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag ladle maintained by titanium dioxide;
J. controlling the temperature of the alloy aluminum liquid at 730 ℃, and casting to obtain an aluminum intermediate alloy material; wherein, the surface of the ingot mould for casting is maintained and treated by titanium dioxide.
In the step E, the step of adding the potassium fluoborate into the crucible of the intermediate frequency furnace in batches comprises the following steps:
firstly, a movable material box is hoisted to a furnace mouth of an intermediate frequency furnace, two sealed smoke baffle plates are installed at the furnace mouth of the intermediate frequency furnace, and a feed opening of the movable material box is fed into the intermediate frequency furnace through the smoke baffle plates, wherein the movable material box, the smoke baffle plates and the intermediate frequency furnace are tightly assembled, and more than 99% of dense smoke generated in the production process is collected by a dust collector to reach the environmental protection emission standard;
secondly, controlling the temperature of high-purity aluminum liquid in a crucible of the intermediate frequency furnace to be 720 +/-5 ℃, adjusting the power to be 30 percent, controlling the frequency to be 150Hz, opening a discharge port valve of a movable material box, discharging a small amount of the aluminum liquid to the surface of the highest rolling position of the aluminum liquid, and taking the standard that the potassium fluoborate is rapidly dispersed around the aluminum liquid without aggregation; meanwhile, a graphite silicon carbide impeller stirrer is used for mechanically stirring the surface of the aluminum liquid, so that potassium fluoborate is prevented from condensing and burning, the temperature in the small-amount feeding process is controlled at 750 ℃, and when the temperature is ultrahigh, a high pure aluminum standard ingot is added for timely cooling;
thirdly, during the feeding process, 1kg of potassium fluotitanate is added for each time when the molten aluminum is sticky, and the whole feeding process is carried out for 5 times;
fourthly, potassium fluoborate is generated around the rolling aluminum liquid to form a layered solution, and when the ring surface reaches the radius, the material box is started to start a large amount of material discharging;
mechanically stirring the surface of the aluminum liquid by using a graphite silicon carbide impeller stirrer in the blanking process to avoid the coagulation of potassium fluoborate, controlling the temperature of the aluminum liquid below 780 ℃ in the feeding process, and increasing a pure aluminum standard ingot to cool in time when the temperature is ultrahigh;
sixthly, when the potassium fluoborate in the material box is completely discharged, the residual high-purity aluminum standard ingot is also completely added into the crucible of the intermediate frequency furnace, so that the high-purity aluminum standard ingot is fully mixed and completely reacted.
In step ③, potassium fluotitanate is added when the molten aluminum is sticky1 kg/time means that the layered solution generated after the potassium fluoborate is added into the alloy aluminum liquid is treated, the fluidity can be improved through stirring reaction, and TiB is preferentially generated2And the boron absorption rate in the aluminum liquid is promoted to be higher at lower temperature.
The aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum produced by the production process scheme adopts the production processes of selecting and using proper raw and auxiliary materials, scientific feeding coefficient, stirring by a medium-frequency furnace and a graphite silicon carbide stirrer, strict temperature control of each channel, proper addition of potassium fluotitanate and alumina powder auxiliary materials in due time, introduction of a transfer platform bag to repeatedly treat solution on the surface of alloy aluminum liquid and the like, so that the boron B content of an alloy ingot is uniform, and the high-power structure AlB is high2Uniform phase grain distribution, generation of an amorphous net structure, no inclusion, bright appearance and cleanness.
The product quality of the invention integrally reaches the highest level of the same industry, is suitable for improving the purification effect and speed of high-purity aluminum production, and is worthy of popularization and use.
Example 2:
an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following chemical components in percentage by mass: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of vanadium V, less than or equal to 0.0006 percent of manganese Mn, less than or equal to 0.0005 percent of titanium Ti, 3.5 percent of boron P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurities and the balance of aluminum.
The production method of the aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following specific steps:
A. firstly, adding 0.38 ton of high-purity aluminum standard ingot into a crucible of a 1 ton intermediate frequency furnace, and taking the rest 0.12 ton as a cooling ingot in the production process; wherein, the content requirement of the high-purity aluminum standard ingot is as follows: less than or equal to 0.01 percent of silicon Si, less than or equal to 0.01 percent of iron Fe, less than or equal to 0.001 percent of vanadium V, less than or equal to 0.001 percent of manganese Mn, less than or equal to 0.001 percent of titanium Ti, less than 0.002 percent of other single impurities, less than 0.002 percent of total impurities, and more than or equal to 99.95 percent of aluminum Al;
B. starting a crucible of the intermediate frequency furnace, raising the temperature for 40 minutes at a power of 60%, and fully melting and raising the temperature of the high-purity aluminum ingot to 720 ℃;
C. a 1.5m crucible shovel maintained by titanium dioxide shovels slag on the crucible wall from top to bottom along the crucible wall; then, a proper amount of slag removing agent is scattered, and slag is removed;
D. the quality requirement and the adding amount of the potassium fluoborate are calculated as follows:
the quality requirement is as follows: the mass fraction of the potassium fluoborate is more than or equal to 98 percent; white powder or crystal, and other impurities cannot be mixed;
the calculation method comprises the following steps: calculating the addition of potassium fluoborate according to the content of 3.5 percent of the boron internal control range, wherein the weight of the potassium fluoborate = the total weight of the high-purity aluminum standard ingot multiplied by 0.4;
E. adding the potassium fluoborate into a movable material box according to the calculated amount of the item D, and adding the potassium fluoborate into the intermediate frequency furnace in batches according to the process requirements;
F. after the potassium fluoborate is added and the layered solution is completely formed, the material conveying box is lifted, the smoke baffle plate is reserved to seal the furnace mouth, and the dense smoke is prevented from leaking; starting the power of a crucible of the intermediate frequency furnace to 60%, stirring for 30 minutes to fully alloy, and controlling the temperature to be below 830 ℃;
G. skimming upper layer of scum to a special slag basin, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag spoon maintained by titanium dioxide;
H. tipping the alloy aluminum liquid in the furnace and pouring the alloy aluminum liquid into a 1-ton transfer ladle, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a mixture of surface alumina powder and the solution by using a slag ladle maintained by titanium dioxide;
I. pouring the alloy aluminum liquid in the transfer ladle back into the crucible of the intermediate frequency furnace, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid again, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag ladle maintained by titanium dioxide;
J. controlling the temperature of the alloy aluminum liquid at 750 ℃, and casting to obtain an aluminum intermediate alloy material; wherein, the surface of the ingot mould for casting is maintained and treated by titanium dioxide.
In the step E, the step of adding the potassium fluoborate into the crucible of the intermediate frequency furnace in batches comprises the following steps:
firstly, a movable material box is hoisted to a furnace mouth of an intermediate frequency furnace, two sealed smoke baffle plates are installed at the furnace mouth of the intermediate frequency furnace, and a feed opening of the movable material box is fed into the intermediate frequency furnace through the smoke baffle plates, wherein the movable material box, the smoke baffle plates and the intermediate frequency furnace are tightly assembled, and more than 99% of dense smoke generated in the production process is collected by a dust collector to reach the environmental protection emission standard;
secondly, controlling the temperature of high-purity aluminum liquid in a crucible of the intermediate frequency furnace to be 720 +/-5 ℃, adjusting the power to be 30 percent, controlling the frequency to be 160Hz, opening a discharge port valve of a movable material box, discharging a small amount of the aluminum liquid to the surface of the highest rolling position of the aluminum liquid, and taking the standard that the potassium fluoborate is rapidly dispersed around the aluminum liquid without aggregation; meanwhile, a graphite silicon carbide impeller stirrer is used for mechanically stirring the surface of the aluminum liquid, so that potassium fluoborate is prevented from condensing and burning, the temperature in the small-amount feeding process is controlled at 750 ℃, and when the temperature is ultrahigh, a high pure aluminum standard ingot is added for timely cooling;
thirdly, during the feeding process, 1kg of potassium fluotitanate is added for each time when the molten aluminum is sticky, and the whole feeding process is carried out for 5 times;
fourthly, potassium fluoborate is generated around the rolling aluminum liquid to form a layered solution, and when the ring surface reaches the radius, the material box is started to start a large amount of material discharging;
mechanically stirring the surface of the aluminum liquid by using a graphite silicon carbide impeller stirrer in the blanking process to avoid the coagulation of potassium fluoborate, controlling the temperature of the aluminum liquid below 780 ℃ in the feeding process, and increasing a pure aluminum standard ingot to cool in time when the temperature is ultrahigh;
sixthly, when the potassium fluoborate in the material box is completely discharged, the residual high-purity aluminum standard ingot is also completely added into the crucible of the intermediate frequency furnace, so that the high-purity aluminum standard ingot is fully mixed and completely reacted.
In step ③, the addition of 1 kg/time of potassium fluotitanate when the aluminum liquid is tacky means that the layered solution generated after the potassium fluoborate is added into the alloy aluminum liquid is treated, the fluidity can be improved through stirring reaction, and TiB is preferentially generated2And the boron absorption rate in the aluminum liquid is promoted to be higher at lower temperature.
Example 3:
an aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following chemical components in percentage by mass: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of vanadium V, less than or equal to 0.0006 percent of manganese Mn, less than or equal to 0.0005 percent of titanium Ti, 3.0 percent of boron P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurities and the balance of aluminum.
The production method of the aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum comprises the following specific steps:
A. firstly, adding 0.38 ton of high-purity aluminum standard ingot into a crucible of a 1 ton intermediate frequency furnace, and taking the rest 0.12 ton as a cooling ingot in the production process; wherein, the content requirement of the high-purity aluminum standard ingot is as follows: less than or equal to 0.01 percent of silicon Si, less than or equal to 0.01 percent of iron Fe, less than or equal to 0.001 percent of vanadium V, less than or equal to 0.001 percent of manganese Mn, less than or equal to 0.001 percent of titanium Ti, less than 0.002 percent of other single impurities, less than 0.002 percent of total impurities, and more than or equal to 99.95 percent of aluminum Al;
B. starting a crucible of the intermediate frequency furnace, raising the temperature for 40 minutes at a power of 60%, and fully melting and raising the temperature of the high-purity aluminum ingot to 720 ℃;
C. a 1.5m crucible shovel maintained by titanium dioxide shovels slag on the crucible wall from top to bottom along the crucible wall; then, a proper amount of slag removing agent is scattered, and slag is removed;
D. the quality requirement and the adding amount of the potassium fluoborate are calculated as follows:
the quality requirement is as follows: the mass fraction of the potassium fluoborate is more than or equal to 98 percent; white powder or crystal, and other impurities cannot be mixed;
the calculation method comprises the following steps: calculating the addition of potassium fluoborate according to the content of 3.0 percent of the boron internal control range, wherein the weight of the potassium fluoborate = the total weight of the high-purity aluminum standard ingot multiplied by 0.4;
E. adding the potassium fluoborate into a movable material box according to the calculated amount of the item D, and adding the potassium fluoborate into the intermediate frequency furnace in batches according to the process requirements;
F. after the potassium fluoborate is added and the layered solution is completely formed, the material conveying box is lifted, the smoke baffle plate is reserved to seal the furnace mouth, and the dense smoke is prevented from leaking; starting the power of a crucible of the intermediate frequency furnace to 60%, stirring for 30 minutes to fully alloy, and controlling the temperature to be below 830 ℃;
G. skimming upper layer of scum to a special slag basin, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag spoon maintained by titanium dioxide;
H. tipping the alloy aluminum liquid in the furnace and pouring the alloy aluminum liquid into a 1-ton transfer ladle, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a mixture of surface alumina powder and the solution by using a slag ladle maintained by titanium dioxide;
I. pouring the alloy aluminum liquid in the transfer ladle back into the crucible of the intermediate frequency furnace, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid again, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag ladle maintained by titanium dioxide;
J. controlling the temperature of the alloy aluminum liquid at 740 ℃, and casting to obtain an aluminum intermediate alloy material; wherein, the surface of the ingot mould for casting is maintained and treated by titanium dioxide.
In the step E, the step of adding the potassium fluoborate into the crucible of the intermediate frequency furnace in batches comprises the following steps:
firstly, a movable material box is hoisted to a furnace mouth of an intermediate frequency furnace, two sealed smoke baffle plates are installed at the furnace mouth of the intermediate frequency furnace, and a feed opening of the movable material box is fed into the intermediate frequency furnace through the smoke baffle plates, wherein the movable material box, the smoke baffle plates and the intermediate frequency furnace are tightly assembled, and more than 99% of dense smoke generated in the production process is collected by a dust collector to reach the environmental protection emission standard;
secondly, controlling the temperature of high-purity aluminum liquid in a crucible of the intermediate frequency furnace to be 720 +/-5 ℃, adjusting the power to be 30 percent, controlling the frequency to be 150Hz, opening a discharge port valve of a movable material box, discharging a small amount of the aluminum liquid to the surface of the highest rolling position of the aluminum liquid, and taking the standard that the potassium fluoborate is rapidly dispersed around the aluminum liquid without aggregation; meanwhile, a graphite silicon carbide impeller stirrer is used for mechanically stirring the surface of the aluminum liquid, so that potassium fluoborate is prevented from condensing and burning, the temperature in the small-amount feeding process is controlled at 750 ℃, and when the temperature is ultrahigh, a high pure aluminum standard ingot is added for timely cooling;
thirdly, during the feeding process, 1kg of potassium fluotitanate is added for each time when the molten aluminum is sticky, and the whole feeding process is carried out for 5 times;
fourthly, potassium fluoborate is generated around the rolling aluminum liquid to form a layered solution, and when the ring surface reaches the radius, the material box is started to start a large amount of material discharging;
mechanically stirring the surface of the aluminum liquid by using a graphite silicon carbide impeller stirrer in the blanking process to avoid the coagulation of potassium fluoborate, controlling the temperature of the aluminum liquid below 780 ℃ in the feeding process, and increasing a pure aluminum standard ingot to cool in time when the temperature is ultrahigh;
sixthly, when the potassium fluoborate in the material box is completely discharged, the residual high-purity aluminum standard ingot is also completely added into the crucible of the intermediate frequency furnace, so that the high-purity aluminum standard ingot is fully mixed and completely reacted.
In step ③, the addition of 1 kg/time of potassium fluotitanate when the aluminum liquid is tacky means that the layered solution generated after the potassium fluoborate is added into the alloy aluminum liquid is treated, the fluidity can be improved through stirring reaction, and TiB is preferentially generated2And the boron absorption rate in the aluminum liquid is promoted to be higher at lower temperature.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, and 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. An aluminum intermediate alloy material for high-efficiency purification of high-purity aluminum is characterized in that: the chemical composition components of the aluminum intermediate alloy material are as follows by mass percent: less than or equal to 0.02 percent of Si, less than or equal to 0.02 percent of Fe, less than or equal to 0.0009 percent of V, less than or equal to 0.0006 percent of Mn, less than or equal to 0.0005 percent of Ti, 2.5 to 3.5 percent of P, less than 0.002 percent of other single impurities, less than 0.02 percent of total impurities and the balance of aluminum.
2. The production method of the aluminum master alloy material for high-efficiency purification of high-purity aluminum, which is disclosed by claim 1, comprises the following specific steps:
A. firstly, adding 0.38 ton of high-purity aluminum standard ingot into a crucible of a 1 ton intermediate frequency furnace, and taking the rest 0.12 ton as a cooling ingot in the production process; wherein, the content requirement of the high-purity aluminum standard ingot is as follows: less than or equal to 0.01 percent of silicon Si, less than or equal to 0.01 percent of iron Fe, less than or equal to 0.001 percent of vanadium V, less than or equal to 0.001 percent of manganese Mn, less than or equal to 0.001 percent of titanium Ti, less than 0.002 percent of other single impurities, less than 0.002 percent of total impurities, and more than or equal to 99.95 percent of aluminum Al;
B. starting a crucible of the intermediate frequency furnace, raising the temperature for 40 minutes at a power of 60%, and fully melting and raising the temperature of the high-purity aluminum ingot to 720 ℃;
C. a 1.5m crucible shovel maintained by titanium dioxide shovels slag on the crucible wall from top to bottom along the crucible wall; then, a proper amount of slag removing agent is scattered, and slag is removed;
D. the quality requirement and the adding amount of the potassium fluoborate are calculated as follows:
the quality requirement is as follows: the mass fraction of the potassium fluoborate is more than or equal to 98 percent; white powder or crystal, and other impurities cannot be mixed;
the calculation method comprises the following steps: calculating the addition amount of potassium fluoborate according to the content of 2.5-3.5% of the boron internal control range, wherein the weight of the potassium fluoborate = the total weight of the high-purity aluminum standard ingot multiplied by 0.4;
E. adding the potassium fluoborate into a movable material box according to the calculated amount of the item D, and adding the potassium fluoborate into the intermediate frequency furnace in batches according to the process requirements;
F. after the potassium fluoborate is added and the layered solution is completely formed, the material conveying box is lifted, the smoke baffle plate is reserved to seal the furnace mouth, and the dense smoke is prevented from leaking; starting the power of a crucible of the intermediate frequency furnace to 60%, stirring for 30 minutes to fully alloy, and controlling the temperature to be below 830 ℃;
G. skimming upper layer of scum to a special slag basin, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag spoon maintained by titanium dioxide;
H. tipping the alloy aluminum liquid in the furnace and pouring the alloy aluminum liquid into a 1-ton transfer ladle, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid, uniformly stirring, attaching the solution to the alumina powder, and skimming a mixture of surface alumina powder and the solution by using a slag ladle maintained by titanium dioxide;
I. pouring the alloy aluminum liquid in the transfer ladle back into the crucible of the intermediate frequency furnace, scattering 2kg of pure and dry alumina powder on the surface of the alloy aluminum liquid again, uniformly stirring, attaching the solution to the alumina powder, and skimming a surface aluminum oxide powder solution mixture by using a slag ladle maintained by titanium dioxide;
J. controlling the temperature of the alloy aluminum liquid at 720-750 ℃, and casting to obtain an aluminum intermediate alloy material; wherein, the surface of the ingot mould for casting is maintained and treated by titanium dioxide.
3. The method for producing an aluminum master alloy material for efficiently purifying high-purity aluminum according to claim 2, wherein in the step "E", the step of adding the potassium fluoborate to the crucible of the intermediate frequency furnace in batches comprises the following steps:
firstly, a movable material box is hoisted to a furnace mouth of an intermediate frequency furnace, two sealed smoke baffle plates are installed at the furnace mouth of the intermediate frequency furnace, and a feed opening of the movable material box is fed into the intermediate frequency furnace through the smoke baffle plates, wherein the movable material box, the smoke baffle plates and the intermediate frequency furnace are tightly assembled, and more than 99% of dense smoke generated in the production process is collected by a dust collector to reach the environmental protection emission standard;
secondly, controlling the temperature of high-purity aluminum liquid in a crucible of the intermediate frequency furnace to be 720 +/-5 ℃, adjusting the power to be 30 percent, controlling the frequency to be 150-160 Hz, opening a discharge port valve of a movable material box, discharging a small amount of the aluminum liquid to the surface of the highest rolling position of the aluminum liquid, and taking the standard that the contacted potassium fluoborate is quickly dispersed to the periphery of the aluminum liquid and aggregation does not occur; meanwhile, a graphite silicon carbide impeller stirrer is used for mechanically stirring the surface of the aluminum liquid, so that potassium fluoborate is prevented from condensing and burning, the temperature in the small-amount feeding process is controlled at 750 ℃, and when the temperature is ultrahigh, a high pure aluminum standard ingot is added for timely cooling;
thirdly, during the feeding process, 1kg of potassium fluotitanate is added for each time when the molten aluminum is sticky, and the whole feeding process is carried out for 5 times;
fourthly, potassium fluoborate is generated around the rolling aluminum liquid to form a layered solution, and when the ring surface reaches the radius, the material box is started to start a large amount of material discharging;
mechanically stirring the surface of the aluminum liquid by using a graphite silicon carbide impeller stirrer in the blanking process to avoid the coagulation of potassium fluoborate, controlling the temperature of the aluminum liquid below 780 ℃ in the feeding process, and increasing a pure aluminum standard ingot to cool in time when the temperature is ultrahigh;
sixthly, when the potassium fluoborate in the material box is completely discharged, the residual high-purity aluminum standard ingot is also completely added into the crucible of the intermediate frequency furnace, so that the high-purity aluminum standard ingot is fully mixed and completely reacted.
4. The method for producing an aluminum master alloy material for efficiently purifying high-purity aluminum according to claim 3, wherein the step ③ of adding 1 kg/time of potassium fluotitanate when the molten aluminum is tacky means that the layered solution produced by adding the potassium fluoborate into the molten aluminum alloy is treated and reacted by stirringCapable of improving fluidity and preferentially generating TiB2And the boron absorption rate in the aluminum liquid is promoted to be higher at lower temperature.
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US4469512A (en) * 1982-07-29 1984-09-04 Showa Aluminum Corporation Process for producing high-purity aluminum
EP0732414A1 (en) * 1995-03-17 1996-09-18 KBALLOYS, Inc. Aluminum base alloy and method for preparing same
CN101988163A (en) * 2009-08-05 2011-03-23 包头铝业有限公司 Method for preparing Al-B intermediate alloy with high boron content
KR20140078496A (en) * 2012-12-17 2014-06-25 현대자동차주식회사 Method for producing aluminum alloy
CN104775058A (en) * 2015-04-22 2015-07-15 铜山县超特有色金属添加剂厂 Aluminum-boron intermediate alloy AlB8 and preparation method thereof
CN105671343A (en) * 2016-03-25 2016-06-15 沈阳大学 Preparation method of aluminum boron intermediate alloy wire for electrician aluminum melt purification
CN109161708A (en) * 2018-11-13 2019-01-08 河北四通新型金属材料股份有限公司 A kind of high-purity high concentration of aluminium boron intermediate alloy and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4469512A (en) * 1982-07-29 1984-09-04 Showa Aluminum Corporation Process for producing high-purity aluminum
EP0732414A1 (en) * 1995-03-17 1996-09-18 KBALLOYS, Inc. Aluminum base alloy and method for preparing same
CN101988163A (en) * 2009-08-05 2011-03-23 包头铝业有限公司 Method for preparing Al-B intermediate alloy with high boron content
KR20140078496A (en) * 2012-12-17 2014-06-25 현대자동차주식회사 Method for producing aluminum alloy
CN104775058A (en) * 2015-04-22 2015-07-15 铜山县超特有色金属添加剂厂 Aluminum-boron intermediate alloy AlB8 and preparation method thereof
CN105671343A (en) * 2016-03-25 2016-06-15 沈阳大学 Preparation method of aluminum boron intermediate alloy wire for electrician aluminum melt purification
CN109161708A (en) * 2018-11-13 2019-01-08 河北四通新型金属材料股份有限公司 A kind of high-purity high concentration of aluminium boron intermediate alloy and preparation method thereof

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