CN111549237B - Method for separating iron element impurities from pulse current in secondary aluminum melt - Google Patents
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Abstract
A method for separating iron element impurities from pulse current in a recycled aluminum melt belongs to the technical field of recycled aluminum melt purification. Placing the regenerated aluminum alloy melt with the content of the iron element exceeding the standard in a crucible, connecting two electrodes with a pulse power supply and inserting the two electrodes into the aluminum melt in parallel, continuously applying pulse current until corresponding time, and selecting corresponding pulse parameters according to the volume and the temperature of the melt. Pulse current processing parameter range: a frequency of 20 to 50kHz, a voltage of 1 to 100V, and a current density of 0.1 to 700A/cm2The action time is 1 min-10 h. The method utilizes the electromigration of Al element and Fe element in the melt in different directions under the action of pulse current to ensure that the Al element and the Fe element are respectively enriched at the anode and the cathode, thereby achieving the purpose of purifying the aluminum melt. The invention can carry out pulse current treatment on the aluminum melt without adding any neutralizing element to pollute the melt, realize the separation of iron impurity elements in the aluminum melt and purify the melt. The method is simple to operate, efficient and pollution-free, greatly improves the iron removal efficiency, and meets the requirements of the current industrial green development planning.
Description
Technical Field
The invention belongs to the technical field of purification of secondary aluminum melt, and particularly relates to a method for removing iron impurity elements in the secondary aluminum melt by separating Al-Fe in the aluminum melt through pulse current.
Background
The aluminum alloy has been widely used in the fields of automobiles, aviation, electronics, buildings and the like due to its excellent properties. And the aluminum alloy thereof have high recoverability, are metal materials with the highest recovery value, and have remarkable environmental benefit and economic benefit in the recovery and the reutilization of the aluminum and the aluminum alloy thereof. Compared with the production of raw aluminum, the comprehensive energy consumption for producing the secondary aluminum is only 5 percent of that of electrolytic aluminum, but CO2The discharge amount of the catalyst can be reduced by more than 90 percent. Therefore, the energy and the bauxite resources are reasonably developed and utilizedAt the same time as the source, it is necessary to pay attention to recycling of the renewable resources. One of the major difficulties in recycling high quality recycled aluminum alloys is to remove harmful elements such as Fe, Zn, Mg, etc., and then adjust alloying components to meet the use standards. Among them, iron is the most harmful element in aluminum alloys and is also the most difficult element to remove. The solid solubility of iron in the aluminum alloy is very low, a small amount of iron can be combined with aluminum or other elements in the aluminum alloy to form a needle-shaped iron-rich phase, a matrix is severely cut, and the mechanical properties, particularly the elongation, of the aluminum alloy are greatly reduced. The removal of impurity element iron has become an international problem which besets the development of the secondary aluminum industry, and the key of the removal of impurity element iron is self-evident to the expansion of the application of secondary aluminum and the improvement of the quality of secondary aluminum products. Therefore, the high-efficiency iron removal technology for the regenerated aluminum alloy is a key technology for developing high-quality aluminum alloy and products thereof.
Conventional methods for reducing and eliminating the deleterious effects of iron phases include: element neutralization, overheating, natural sedimentation, centrifugation, and composite purification. The patent (CN103572080A) discloses a method for removing iron, refining crystal grains and improving the iron-rich phase morphology of aluminum-silicon secondary aluminum, which adopts Al-B, Al-Mn intermediate alloy as an iron remover, forms high-melting-point and high-density mass points such as Fe-B, Al-Si-Mn-Fe through Mn and B elements and Al, Si, Fe and the like in the aluminum-silicon secondary aluminum, one part is naturally settled and removed, and the other part is supplemented with mechanical vibration in the casting process to refine the crystal grains and improve the elongation of the aluminum-silicon secondary aluminum. The patent (CN104674010A) discloses a method for removing harmful elements in the regeneration process of aluminum scrap, which comprises the steps of classifying and sorting the recovered aluminum scrap, carrying out primary modification, and then putting the aluminum scrap into a smelting furnace for low-temperature smelting treatment. And stirring by adopting an electromagnetic iron removal stirring device in the process, removing iron by utilizing magnetic adsorption, adding an impurity removing agent, and skimming the aluminum liquid after impurity removal to obtain a qualified pure aluminum solution. The patent (CN1354267A) discloses an electromagnetic separation method for removing iron element in aluminum-silicon alloy, firstly, adding manganese into eutectic aluminum-silicon alloy to fully separate out iron element in the melt in the form of primary iron-rich phase, and separating the primary phase from the melt by 'displacement' by utilizing different motion laws of the primary iron-rich phase and the melt under the action of electromagnetic force, and enriching the primary phase on the wall of a filter to remove the iron element, thereby reducing the content of the iron element in the aluminum-silicon alloy. But this treatment method still has major drawbacks. Firstly, the method must alloy the melt to make the primary iron-rich phase fully separated out from the melt, and the addition of alloying elements will inevitably pollute the melt. Secondly, the treatment method disclosed by the invention adopts a steady-flow magnetic field and a direct current or high-frequency magnetic field, so that the melt is easy to be unstable and the separation efficiency is low. Thirdly, the method is to make the alloy melt flow through the pipeline of the induced magnetic field during the casting process, and not to directly pass current through the melt. The invention directly connects the pulse current into the alloy melt, and the high-speed electron current directly acts on Al element and Fe element in the melt, but not on the iron-rich phase in the melt. The aim of purifying the regenerated aluminum melt is achieved by utilizing the difference of the migration directions of the Al element and the Fe element under the action of pulse current. The separation methods have the advantages and disadvantages, the operation is complex, the time period is long, the efficiency is low, and intermediate elements are required to be added into the melt to serve as an iron remover, so that the aluminum alloy melt is further polluted. With the continuous development of the secondary aluminum industry and the improvement of the quality requirement of high-performance aluminum alloy, the limitation on the content of iron impurity in the aluminum alloy is more and more strict, and a new iron removal technology is urgently required to be developed.
The content of iron element in the regenerated aluminum alloy directly determines the quality and the performance of the regenerated aluminum alloy. Pulsed current is an important transient non-equilibrium processing technique that is simple, easy to operate, clean, efficient and has gained increasing attention due to its specific role in metallic materials.
Disclosure of Invention
The invention aims to provide a novel method for removing iron impurities in regenerated aluminum alloy by realizing Al-Fe separation in aluminum melt through pulse current treatment by using an unconventional external field treatment means. The method can effectively remove iron element impurities in the regenerated aluminum alloy, avoid adverse effects caused by excessive iron element impurities in the regenerated aluminum alloy, and remarkably improve the quality of the regenerated aluminum alloy.
The invention is composed of:
an Al-2.2% Fe alloy is prepared by adopting 99% (mass fraction, the same below) of industrial pure aluminum and Al-20% Fe alloy. The alloy material is taken as a research object, the material is melted in a crucible, and pulse current parameters (the frequency is 20-50 kHz, the voltage is 1-100V, and the current density is 0.1-700A/cm)2And the acting time is 1 min-10 h) to act on the aluminum melt, so that the Al-Fe in the melt is separated, and the purpose of purifying the aluminum alloy melt is achieved.
A method for removing iron impurity elements in a regenerated aluminum alloy melt is characterized in that the regenerated aluminum alloy melt is subjected to pulse current treatment, and the method has the characteristics of high efficiency, cleanness, easy operation and no pollution to the melt; parameter ranges of the pulse processing: a frequency of 20 to 50kHz, a voltage of 1 to 100V, and a current density of 0.1 to 700A/cm2The action time is 1 min-10 h.
Further, the specific steps of the pulse current processing are as follows:
(1) an Al-2.2% Fe alloy sample was prepared from 99% commercial purity aluminum and an Al-20% Fe master alloy. And placing the sample in a crucible, heating the sample to 1200 ℃ in a resistance furnace, and preserving heat for 50-70min to completely melt the alloy material and homogenize the aluminum melt.
(2) The temperature of the melt is reduced to 900 ℃ along with the furnace, the two electrodes are connected with a pulse power supply by pure copper wires and are parallelly inserted into the aluminum melt, the aluminum melt is subjected to pulse current treatment according to planned parameters, and the temperature is kept for 9-11min at the temperature. Pulse parameters: a frequency of 20 to 50kHz, a voltage of 1 to 100V, and a current density of 0.1 to 700A/cm2The action time is 1 min-10 h.
(3) Turning off a heating power supply of the resistance furnace, cooling the sample along with the furnace, and applying electric pulse all the time during the period;
(4) and when the sample is cooled to 700 ℃ along with the furnace, cutting off the pulse power supply, taking out the sample and carrying out water cooling.
Further, suitable pulsed current processing parameters are selected according to melt volume and temperature: the pulse current treatment temperature of the aluminum melt is 900 ℃, the size of the crucible is phi 50mm (inner diameter) x 60mm, and the pulse current parameters are selected to be 31kHz, 8V and 9.8A/cm2The action time is 70 min; the pulse current treatment temperature of the aluminum melt is 900 DEG CThe crucible size is phi 50mm (inner diameter) x 60mm, and the pulse current parameters are 10kHz, 12V and 24.5A/cm2The action time is 70 min; the pulse current treatment temperature of the aluminum melt is 750 ℃, the size of the crucible is phi 70mm (inner diameter) x 70mm, and the pulse current parameters are 200Hz, 24V and 49A/cm2Action time is 10 min.
The equipment adopted by the pulse current treatment is a pulse power supply.
The pulse treatment of the melt is carried out in a resistance furnace.
The electrode is made of graphite and has the size of phi 10mm multiplied by 30 cm.
The pulse current treatment of the aluminum melt can cause iron atoms in the aluminum melt to directionally move to the negative electrode and aluminum atoms in the melt to directionally move to the positive electrode, thereby realizing the separation of Al-Fe in the melt and purifying the melt. More importantly, compared with the existing iron removal method, the pulse current treatment does not need to add intermediate elements, so that the aluminum melt is not polluted, the operation is simple, the aluminum melt can be directly treated, the method is easy to implement, and the continuous treatment of the aluminum melt can be realized. The invention provides a novel simple and efficient method for removing iron element impurities in an aluminum melt, which can effectively improve the quality and performance of secondary aluminum.
Compared with the prior method for removing Fe element impurities in the aluminum melt, such as a neutralization element method, a natural sedimentation method, a centrifugal method, a composite purification method, an electromagnetic purification method and the like, the method can directly treat the aluminum melt without adding the neutralization element to pollute the aluminum melt, and effectively separate the Fe element impurities in the aluminum melt. The method is simple to operate, can efficiently and continuously treat the aluminum melt, achieves the purpose of removing Fe, and meets the requirements of the current industrial green development planning.
Drawings
FIG. 1 is a schematic view of a pulse current processing apparatus in embodiment 1.
FIG. 2 example 1 shows the Fe element content distribution between the positive and negative electrodes in the cast ingot after the Al-2.2% Fe alloy is treated by the pulse current.
Detailed Description
The invention selects Al-2.2% Fe alloy, which is prepared by 99% industrial pure aluminum and Al-20% Fe intermediate alloy. The present invention is further illustrated by the following specific examples.
Example 1:
this example was carried out on an Al-2.2% Fe melt in a crucible by pulsed current treatment. The method comprises the following specific steps:
the first step is as follows: and (3) putting the prepared Al-2.2% Fe alloy material into a crucible, placing the crucible into a resistance furnace, heating to 1200 ℃, and preserving heat for 60 min. To ensure complete dissolution of the needle-like iron-rich phase in the master alloy Al-20% Fe and to homogenize the melt. The crucible size was phi 50mm (inner diameter) × 60 mm.
The second step is that: pulse processing parameters are determined. Setting the parameter range of the pulse current, and determining the parameters of the pulse current as 31kHz, 8V of voltage and 9.8A/cm of pulse current density2Action time is 70 min.
The third step: and (5) pulse current processing. When the temperature of the Al-2.2% Fe melt is reduced to 900 ℃ along with the furnace, two electrodes are inserted into the melt in parallel, and the pulse current treatment is started. Keeping the temperature for 10min at the temperature, cutting off the heating power supply of the resistance furnace to cool the sample along with the furnace, applying pulse current all the time, connecting the electrode and the copper wire in a winding manner to ensure good contact, and the schematic diagram of the processing equipment is shown in figure 1.
Fourthly, stopping the pulse current processing when the pulse current processing time is 70 min. At this time, the temperature of the aluminum melt was 700 ℃, the sample did not start to solidify, and the sample was taken out and water-cooled.
The fifth step: the cooled tissue change of the sample was observed under a light microscope. Cutting an effective area between two electrodes from the cooled cast ingot sample, sequentially grinding and polishing the surface of the effective area by 600-mesh, 800-mesh and 1500-mesh sand paper, and adopting 1mL of concentrated HF, 1.5mL of concentrated HCl and 2.5mL of concentrated HNO3And 95mL of distilled water as a caustic. And observing a metallographic structure from the positive electrode to the negative electrode of the sample after the pulse current treatment and a metallographic structure from the bottom to the top of the sample after the pulse current treatment through an optical microscope.
And a sixth step: and (5) detecting the content of iron elements at different positions. The content of iron elements at different positions of an effective sample between the two electrodes is detected in an electron microscope mirror scanning mode, and the distribution of the content of the Fe elements between the positive electrode and the negative electrode in the cast ingot after the Al-2.2% Fe alloy is treated by pulse current is shown in figure 2.
Example 2:
this example was carried out on an Al-2.2% Fe melt in a crucible by pulsed current treatment. The method comprises the following specific steps:
the first step is as follows: and (3) putting the prepared Al-2.2% Fe alloy material into a crucible, placing the crucible into a resistance furnace, heating to 1200 ℃, and preserving heat for 60 min. To ensure complete dissolution of the needle-like iron-rich phase in the master alloy Al-20% Fe and to homogenize the melt. The crucible size was phi 50mm (inner diameter) × 60 mm.
The second step is that: pulse current processing parameters are determined. Setting the parameter range of the pulse current, and determining the parameters of the pulse current as 10kHz, 12V of voltage and 24.5A/cm of pulse current density2Action time is 70 min.
The third step: and (5) pulse current processing. When the temperature of the Al-2.2% Fe melt is reduced to 900 ℃ along with the furnace, two electrodes are inserted into the melt in parallel, and the pulse current treatment is started. Keeping the temperature for 10min at the temperature, cutting off the heating power supply of the resistance furnace to cool the sample along with the furnace, and applying pulse current all the time. The electrodes are connected with the copper wires in a winding manner, so that good contact is ensured.
The fourth step: and when the pulse current treatment time is up to 70min, stopping the pulse current treatment, taking out the sample and carrying out water cooling.
The fifth step: the cooled tissue change of the sample was observed under a light microscope. Cutting an effective area between two electrodes from the cooled cast ingot sample, sequentially grinding and polishing the surface of the effective area by 600-mesh, 800-mesh and 1500-mesh sand paper, and adopting 1mL of concentrated HF, 1.5mL of concentrated HCl and 2.5mL of concentrated HNO3And 95mL of distilled water as a caustic. And observing a metallographic structure from the positive electrode to the negative electrode of the pulse current post-treatment sample and a metallographic structure from the bottom to the top of the pulse current post-treatment sample through an optical microscope.
And a sixth step: and (4) detecting the content of Fe elements at different positions. And detecting the content of the Fe element at different positions of the effective sample between the two electrodes in an electron microscope mirror scanning mode.
Example 3:
this example was carried out on an Al-2.2% Fe melt in a crucible by pulsed current treatment. The method comprises the following specific steps:
the first step is as follows: and (3) putting the prepared Al-2.2% Fe alloy material into a crucible, placing the crucible into a resistance furnace, heating to 1200 ℃, and preserving heat for 60 min. To ensure complete dissolution of the needle-like iron-rich phase in the master alloy Al-20% Fe and to homogenize the melt. The crucible size was phi 70mm (inner diameter) × 70 mm.
The second step is that: pulse current processing parameters are determined. Setting the parameter range of the pulse current, and determining the parameters of the pulse current as 200Hz, 24V and 49A/cm2Action time is 10 min.
The third step: and (5) pulse current processing. When the temperature of the Al-2.2% Fe melt is reduced to 750 ℃ along with the furnace, two electrodes are inserted into the melt in parallel, and the pulse current treatment is started to be carried out on the melt. Keeping the temperature for 10min at the temperature, cutting off the heating power supply and the pulse power supply of the resistance furnace, taking out the sample and cooling by water. The electrodes are connected with the copper wires in a winding manner, so that good contact is ensured.
The fourth step: the cooled tissue change of the sample was observed under a light microscope. Cutting an effective area between two electrodes from the cooled cast ingot sample, sequentially grinding and polishing the surface of the effective area by 600-mesh, 800-mesh and 1500-mesh sand paper, and adopting 1mL of concentrated HF, 1.5mL of concentrated HCl and 2.5mL of concentrated HNO3And 95mL of distilled water as a caustic. And observing a metallographic structure from the positive electrode to the negative electrode of the pulse current post-treatment sample and a metallographic structure from the bottom to the top of the pulse current post-treatment sample through an optical microscope.
The fifth step: and (5) detecting the content of iron elements at different positions. And detecting the content of the iron element at different positions of the effective sample between the two electrodes in an electron microscope mirror scanning mode.
The above description is only the best embodiment of the present invention for removing iron from recycled aluminum alloy, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute similar materials, equipments or adjust related technical parameters within the technical scope of the present invention.
Claims (5)
1. A method for removing iron impurity elements in a regenerated aluminum alloy melt is characterized in that the regenerated aluminum alloy melt is subjected to pulse current treatment, and the method has the characteristics of high efficiency, cleanness, easy operation and no pollution to the melt; parameter ranges of the pulse processing: a frequency of 20 to 50kHz, a voltage of 1 to 100V, and a current density of 0.1 to 700A/cm2The action time is 1min to 10 hours;
the pulse current processing comprises the following specific steps:
(1) preparing an Al-2.2% Fe alloy sample from 99% of industrial pure aluminum and an Al-20% Fe intermediate alloy; placing the sample in a crucible, heating the sample to 1200 ℃ in a resistance furnace, and preserving heat for 50-70min to completely melt the alloy material and homogenize the aluminum melt;
(2) cooling the melt to 900 ℃ along with the furnace, connecting two electrodes with a pulse power supply by using pure copper wires and inserting the two electrodes into the aluminum melt in parallel, carrying out pulse current treatment on the aluminum melt according to planned parameters, and preserving heat for 9-11min at the temperature; pulse parameters: a frequency of 20 to 50kHz, a voltage of 1 to 100V, and a current density of 0.1 to 700A/cm2The action time is 1min to 10 hours;
(3) turning off a heating power supply of the resistance furnace, cooling the sample along with the furnace, and applying electric pulse all the time during the period;
(4) and when the sample is cooled to 700 ℃ along with the furnace, cutting off the pulse power supply, taking out the sample and carrying out water cooling.
2. The method for removing iron impurity elements from a regenerated aluminum alloy melt according to claim 1, wherein the pulse current treatment parameters are selected according to the melt volume and temperature: the pulse current treatment temperature of the aluminum melt is 900 ℃, the size of the crucible is phi 50mm multiplied by 60mm, and the pulse current parameters are selected to be 31kHz, 8V and 9.8A/cm2Action time is 70 min.
3. The method for removing iron impurity elements from a regenerated aluminum alloy melt as set forth in claim 1, wherein the pulse power is selected to be suitable in accordance with the melt volume and temperatureStream processing parameters: the pulse current treatment temperature of the aluminum melt is 900 ℃, the size of the crucible is phi 50mm multiplied by 60mm, and the pulse current parameters are selected to be 10kHz, 12V and 24.5A/cm2Action time is 70 min.
4. The method for removing iron impurity elements from a regenerated aluminum alloy melt according to claim 1, wherein the pulse current treatment parameters are selected according to the melt volume and temperature: the pulse current treatment temperature of the aluminum melt is 750 ℃, the size of the crucible is phi 70mm multiplied by 70mm, the pulse current parameters are 200Hz, 24V and 49A/cm2Action time is 10 min.
5. The method for removing iron impurity elements from a regenerated aluminum alloy melt according to claim 1, wherein the pulse current treatment is carried out by using a pulse power supply; the pulse treatment of the melt is carried out in a resistance furnace; the electrode is made of graphite and has the size of phi 10mm multiplied by 30 cm.
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| US20240043964A1 (en) * | 2022-05-10 | 2024-02-08 | University Of Science And Technology Beijing | Device and method for preparing low-impurity regenerated brass alloy through step-by-step insertion of electrode |
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