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WO2017209034A1 - Procédé et dispositif de purification de matière, dispositif de chauffage et de retenue de métal fondu, et système de purification continue pour matière de pureté élevée - Google Patents

Procédé et dispositif de purification de matière, dispositif de chauffage et de retenue de métal fondu, et système de purification continue pour matière de pureté élevée Download PDF

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Publication number
WO2017209034A1
WO2017209034A1 PCT/JP2017/019876 JP2017019876W WO2017209034A1 WO 2017209034 A1 WO2017209034 A1 WO 2017209034A1 JP 2017019876 W JP2017019876 W JP 2017019876W WO 2017209034 A1 WO2017209034 A1 WO 2017209034A1
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WO
WIPO (PCT)
Prior art keywords
molten metal
cooling body
crucible
substance
molten
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2017/019876
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English (en)
Japanese (ja)
Inventor
勝起 吉田
萩原　靖久
雄一郎 大関
雅生 前田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Resonac Holdings Corp
Original Assignee
Showa Denko KK
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2016110658A external-priority patent/JP6746383B2/ja
Priority claimed from JP2016128018A external-priority patent/JP6751604B2/ja
Priority claimed from JP2016226471A external-priority patent/JP6762206B2/ja
Application filed by Showa Denko KK filed Critical Showa Denko KK
Priority to CN201780033783.5A priority Critical patent/CN109219669B/zh
Publication of WO2017209034A1 publication Critical patent/WO2017209034A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
    • C22B9/02—Refining by liquating, filtering, centrifuging, distilling, or supersonic wave action including acoustic waves
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • the present invention relates to a purification method and apparatus for substances such as metals, and a continuous purification system for high-purity substances. More specifically, the present invention relates to aluminum, silicon, magnesium, lead, zinc containing eutectic impurities using the principle of segregation solidification. The present invention relates to a method and apparatus for producing a high-purity substance by reducing the content of eutectic impurities from the original substance and the like, a molten metal heating and holding apparatus, and further relates to a continuous purification system for a high-purity substance.
  • Patent Document 1 the impurity concentrated layer near the solidification interface is thinned by rotating the cooling body so that the relative speed between the outer peripheral portion of the cooling body and molten aluminum is 1600 mm / s to 8000 mm / s.
  • Patent Document 1 it has been proposed to increase the purity of purified aluminum.
  • Patent Document 2 proposes a method for preventing the molten aluminum from flowing in the same direction as the cooling body rotates and ensuring the relative speed between the cooling body and the molten aluminum. That is, a plurality of baffle plates for lowering the flow rate of molten aluminum are arranged in the circumferential direction on the inner circumferential surface of the crucible for holding molten aluminum, and the upper end of the baffle plate is provided below the surface of the molten aluminum.
  • the shortest distance between the inner peripheral surface of the crucible and the outer peripheral surface of the cooling body in the molten metal existing portion in the crucible is set to 1/2 of the longest distance between the inner peripheral surface of the crucible and the outer peripheral surface of the cooling body. It has been proposed that by performing the refining with the following settings, a narrow part and a wide part of the flow path of the molten metal are intentionally set, the flow velocity in the circumferential direction of the molten metal is decreased, and the relative speed is increased.
  • Patent Document 4 describes a molten metal heating and holding device in which an electric heater is installed in a bottomed cylindrical ceramic heater cover provided in a hanging shape on the lid of a molten metal treatment tank.
  • this molten metal heating and holding device it is possible to heat both the molten metal portion in the molten metal treatment tank and the space above the molten metal by the heater held on the lid, and it is possible to suppress the adhesion and solidification of metal on the inner wall of the molten metal treatment tank due to molten metal scattering. .
  • Patent Document 5 discloses that the space above the molten metal in the crucible is made of aluminum by winding an electric heater around the crucible for the purpose of preventing the adhesion of solidified aluminum on the inner wall of the crucible. It has been proposed to heat to above its melting point.
  • the baffle plate has an effect of suppressing the flow velocity of the entire molten metal or causing turbulence
  • the range of the effect is a range inward from the inner peripheral surface of the crucible by the length of the baffle plate. It will be limited to the outer peripheral part.
  • the baffle may be damaged.
  • Patent Document 5 has a problem that it is difficult to replace the heater because the crucible body becomes an obstacle when the heater is replaced. Moreover, even if a lid is installed on the crucible, there is a possibility that the electric heater may be damaged because the molten metal may be scattered outside the lid.
  • the object of the present invention has been made in view of such circumstances, and is a substance refining method and apparatus, which has high purification efficiency, can suppress hot water splashing, has high energy cost, and does not have a high degree of difficulty in equipment installation. It is to provide a continuous purification system for a pure substance.
  • An object of the present invention has been made in view of such a technical background, and can effectively prevent the adhesion and solidification of the molten substance on the inner wall of the crucible due to molten metal splash, and the heater can be easily replaced.
  • An object of the present invention is to provide a molten metal holding device, a material refining device and a method which are less likely to damage a heater.
  • the above problem is solved by the following means.
  • (1) In the method for purifying a substance in which a cooling body is immersed in a molten substance to be purified contained in a molten metal holding container, and crystals of the substance are crystallized on the surface of the cooling body while rotating the cooling body, the molten metal holding container
  • the shortest distance L1 in the horizontal direction between the inner peripheral surface of the upper surface of the molten metal and the outer peripheral surface of the cooling body is 150 mm or more, and the entire inner surface of the molten metal holding container is cooled in the entire area where the molten substance exists in the molten metal holding container.
  • a method for purifying a substance, wherein a horizontal distance L2 at the lowermost end of the body is 100 mm or more.
  • the shortest horizontal distance L1 between the inner peripheral surface on the upper surface of the molten metal holding container and the outer peripheral surface of the cooling body is 200 mm or more and 500 mm or less, and the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body.
  • the ratio A / a between the distance A from the bottom surface to the bottom surface of the molten metal holding container and the immersion depth a in the molten material of the cooling body is 0.3 ⁇ A / a ⁇ 3.0.
  • the temperature of the cooling body when immersed in the molten material is immersed in the molten material while rotating the cooling body so that the peripheral speed of the cooling body is 700 mm / s or more and less than 8000 mm / s.
  • the peripheral speed at the interface between the crystal portion crystallized on the cooling body and the molten material is 700 mm. 10.
  • the method for purifying a substance according to any one of items 1 to 10 wherein the maximum peripheral speed of the cooling body at the initial stage of purification after immersion in the cooling body is higher than the average peripheral speed thereafter.
  • the substance purification method according to item 11, wherein the initial stage of purification is from the start of purification to the total purification time ⁇ 0.1 (however, 10 seconds to 120 seconds).
  • An inner circumference on the upper surface of the molten metal including a molten metal holding container for storing the molten material to be purified, and a rotatable cooling body immersed in the molten material stored in the molten metal holding container.
  • the horizontal shortest distance L1 between the surface and the outer peripheral surface of the cooling body is 150 mm or more, and in the entire area where the molten substance exists in the molten metal holding container, the horizontal surface at the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body A substance refining device, wherein the direction distance L2 is set to 100 mm or more.
  • the shortest horizontal distance L1 between the inner peripheral surface on the upper surface of the molten metal holding container and the outer peripheral surface of the cooling body is 200 mm or more and 500 mm or less, and the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body.
  • an outer diameter d of the cooling body on the upper surface of the molten material is 200 mm or more and an inner diameter D on the upper surface of the molten metal holding container is 500 mm or more.
  • a / a is 0.5 ⁇ A / a ⁇ 2.0.
  • An apparatus main body having a crucible arrangement space therein, one or a plurality of crucibles that are disposed in the crucible arrangement space of the apparatus main body and containing a molten metal that is a molten material, and an upper end opening of the crucible A first lid that is closed; a second lid that is separate from the first lid that closes an upper portion of the surrounding space of the crucible; and a lower region in the height direction of the crucible in the surrounding space of the crucible.
  • a series of devices for discharging the molten metal from the final molten metal holding container to the outside of the system is a set of lines, and the N-th line (where 2 ⁇ N) is used as a plurality of the lines, )
  • the high-purity substance lump collected and adhered to the cooling body in the next line (however, 2 ⁇ n ⁇ N) is melted in the subsequent n-th line melting furnace, and the molten metal melted in the melting furnace sequentially It will be discharged through the molten metal holding container, and the nth order line
  • Purification system. (36) A plurality of melts connected in series, which are used in a melting furnace for melting a substance and the material purification apparatus according to any one of items 14 to 21 above, and the melts from the melting furnace are sequentially sent A holding vessel and a rotatable cooling body used in the substance purifying apparatus according to any one of the preceding items 14 to 21 and paired with each molten metal holding vessel to crystallize a high-purity substance in the molten metal; And a series of devices for discharging the molten metal from the final molten metal holding container to the outside of the system is defined as one set of lines, and is composed of an N-th order line (where 2 ⁇ N), and (n ⁇ 1) The high-purity substance lump collected and adhered to the rotating cooling body in the
  • the shortest horizontal distance L1 between the inner peripheral surface of the upper surface of the molten metal in the container and the outer peripheral surface of the cooling body is 150 mm or more, and Since the distance L2 in the horizontal direction at the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body is 100 mm or more in the entire area where the molten substance exists, there are many gaps between the cooling body and the inner peripheral surface of the molten metal holding container. Molten material is present.
  • the molten material itself becomes a resistance, and the swirling flow of the molten material due to the rotation of the cooling body is sufficiently slowed.As a result, the dispersion of the impurity concentrated layer generated near the solidification interface is promoted, and the purification efficiency of the material is increased. improves. If the swirl flow of the molten metal is slowed down, refining can be performed while suppressing the scattering of the molten metal. In particular, securing a large shortest distance L1 between the inner peripheral surface of the upper surface of the molten metal in the container and the outer peripheral surface of the cooling body has a great effect of slowing the swirling flow on the upper surface of the molten metal and preventing the molten metal from scattering.
  • the shortest horizontal distance L1 between the inner peripheral surface of the upper surface of the molten metal holding container and the outer peripheral surface of the cooling body is 200 mm or more and 500 mm or less, Since the horizontal distance L2 between the inner peripheral surface of the holding container and the lowermost end of the cooling body is 150 mm or more and 500 mm or less, higher purification efficiency can be obtained, and jumping can be further suppressed.
  • the outer diameter d of the cooling body on the molten metal upper surface is 200 mm or more, high purification efficiency can be obtained while ensuring productivity.
  • the inner diameter D on the upper surface of the molten metal holding container is 500 mm or more, even if the outer diameter d of the cooling body is 200 mm or more, the inner peripheral surface on the upper surface of the molten metal in the molten metal holding container and the outer peripheral surface of the cooling body.
  • the horizontal distance L2 between the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body can be 100 mm or more.
  • the outer diameter d of the cooling body on the molten metal upper surface is 500 mm or less, it is possible to avoid the cooling body rotating device from becoming large-scale, The difficulty level of equipment installation can be suppressed.
  • the inner diameter D on the upper surface of the molten metal holding container is 650 mm or more and 1300 mm or less, even if the outer diameter d of the cooling body is set to 200 mm or more, the molten metal Since the horizontal shortest distance L1 between the inner peripheral surface of the molten metal upper surface of the holding container and the outer peripheral surface of the cooling body and the horizontal distance L2 between the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body can be secured sufficiently large. Thus, productivity can be secured and excellent purification efficiency can be obtained.
  • the ratio A / a between the distance A from the bottom surface of the cooling body to the bottom surface of the molten metal holding container and the immersion depth a of the cooling body into the molten material is Since 0.3 ⁇ A / a ⁇ 3.0, there is a large amount of molten material between the cooling body and the inner peripheral surface of the molten metal holding container. For this reason, the molten material itself becomes a resistance, and the swirling flow of the molten material due to the rotation of the cooling body is sufficiently slowed.As a result, the dispersion of the impurity concentrated layer generated near the solidification interface is promoted, and the purification efficiency of the material is increased. improves. If the swirl flow of the molten metal is slowed down, refining can be performed while suppressing the scattering of the molten metal.
  • the immersion depth a of the cooling body in the molten material is 150 mm or more and 500 mm or less, and the distance A from the bottom surface of the cooling body to the bottom surface of the molten metal holding container is 700 mm. Since it is the following, productivity and energy efficiency are good and the difficulty of installation can be suppressed.
  • the solid body temperature of the molten substance x 0.7 or more is immersed in the molten substance while rotating at a peripheral speed of 700 mm / s or higher. From the initial stage of purification, high-purity crystals with good adhesion to the cooling body can be crystallized, and separation from the cooling body can be prevented, and the amount of purified substance recovered can be increased. In addition, since the cooling body is set to a peripheral speed of less than 8000 mm / s, it is possible to prevent the occurrence of operational problems such as scattering of the molten material.
  • the cooling body since the maximum peripheral speed of the cooling body at the initial stage of purification is set larger than the average peripheral speed thereafter, the cooling body is immersed in the molten material to be purified.
  • the initial stage of purification even if a crystallized product having a high solidification rate and poor adhesion is purified, it can be positively separated from the rotary cooling body and redissolved in the molten material.
  • the crystallized material with poor adhesion to the cooling body is removed at an extremely early stage, so that it is possible to avoid the situation where the crystallized material with a high solidification rate grows to a certain extent and then peels off from the cooling body, and is actively peeled off.
  • the later purified material can be grown without peeling, and the recovery amount of the purified material can be increased.
  • the inner wall of the crucible exposed in the space above the molten metal can be heated by the upper heater. Therefore, even if the molten material adheres to the inner wall of the crucible due to the rocking or scattering of the molten metal, it is solidified by heating. Therefore, the molten material flows down and returns to the molten metal, and adhesion and solidification of the molten material to the inner wall of the crucible can be prevented.
  • the upper heater is provided separately from the lower heater, the temperature of the inner wall of the crucible exposed in the space above the molten metal can be controlled separately from the temperature of the molten metal, and the temperature of the inner wall of the crucible can be controlled. It can be controlled to an optimum temperature to prevent coagulation.
  • the first lid for closing the upper end opening of the crucible and the second lid for closing the upper part of the space surrounding the crucible are separately provided, and the upper heater is held by the second lid, By removing the second lid, the upper heater can be taken out. Therefore, maintenance and replacement of the heater can be easily performed, and the maintainability is excellent.
  • the upper end opening of the crucible for containing the molten metal is closed with the first lid, and the upper part of the space around the crucible is closed with the second lid, so that the molten metal in the crucible is scattered outside the crucible. Even if it does, it can block
  • the hole corresponding to the upper shape of the crucible is provided in the second lid, when the first lid is removed, for the treatment of the molten metal, purification, etc.
  • the member can be easily put in and out of the crucible.
  • the heater since the upper heater extends in the horizontal direction, the heater can be arranged along the outer peripheral shape of the crucible.
  • the upper heater is arranged along the shape of the outer peripheral surface of the crucible, heat from the upper heater can be uniformly applied to the outer peripheral surface of the crucible, and consequently The inner wall of the crucible exposed in the space above the molten metal can be efficiently and uniformly heated.
  • the upper heater has a communicating rod. Since it is arranged along the shape of the outer peripheral surface of the crucible while being avoided, the inner wall of the crucible can be efficiently and uniformly heated.
  • the upper heater since the upper heater is covered with the heat-resistant material, even if the molten metal in the crucible scatters to the surrounding space outside the crucible, the upper heater is prevented from being damaged immediately. be able to.
  • a high-purity substance can be purified more efficiently than a serially continuous purification facility. That is, when the recovery rate (recovered weight / original input weight) is the same, higher purity can be obtained.
  • the number of the melt holding tanks in the n-th line and the rotary cooling bodies arranged in pairs with the holding tanks are smaller than that of the (n-1) -th line, the melt holding tanks and the rotation cooling in each line. Compared to the case where the number of bodies is the same, a smaller facility area is required.
  • the desired purity can be obtained more efficiently and the operability is excellent.
  • peritectic impurities can be reduced when high-purity aluminum is purified.
  • peritectic impurities can be further reduced.
  • peritectic impurities of aluminum can be efficiently reduced when high-purity aluminum is purified.
  • peritectic impurities can be further efficiently reduced.
  • FIG. 3 is a cross-sectional view taken along line III-III in FIG. It is a longitudinal cross-sectional view of a crucible. It is a perspective view of an upper heater.
  • FIG. 7 is a cross-sectional view taken along line VII-VII in FIG. 6. It is a perspective view of an upper heater. It is a figure which shows the structure of the continuous purification system of the high purity substance which concerns on other embodiment of this invention. It is a figure which shows the structure of the one part line of the system of FIG. 2 in detail. It is a figure which shows the structure of the continuous refining system of the high purity material which concerns on further another embodiment of this invention. 2 is a diagram showing a configuration of a continuous purification system used in Example 51.
  • FIG. 6 is a diagram showing a configuration of a continuous purification system used in Example 52.
  • FIG. 6 is a diagram showing a configuration of a continuous purification system used in Example 53.
  • FIG. It is a figure which shows the structure of the continuous refining system used in Example 54.
  • FIG. 6 is a diagram showing a configuration of a continuous purification system used in Example 55.
  • FIG. 6 is a diagram showing a configuration of a continuous purification system used in Example 57.
  • 6 is a diagram showing a configuration of a continuous purification system used in Example 58.
  • FIG. 6 is a diagram showing a configuration of a continuous purification system used in Example 59.
  • FIG. 6 is a diagram showing a configuration of a continuous purification system used in Example 60.
  • FIG. Fig. (A) is a longitudinal cross-sectional view of a crucible in which a molten substance adheres and solidifies on the inner wall due to the splash of molten metal
  • Fig. (B) is a cross-sectional view taken along the line IX-IX in Fig. (A). .
  • FIG. 1A is a diagram for explaining a schematic configuration of a substance purification apparatus according to an embodiment of the present invention and a substance purification method using the same.
  • the substance is a metal such as aluminum.
  • reference numeral 1 denotes a crucible having a bottomed cylindrical shape as a molten metal holding container and a bottom surface formed in a downward arcuate surface, and a molten metal (also referred to as molten metal) 6 such as aluminum is accommodated and held in the crucible 1.
  • a molten metal also referred to as molten metal
  • the crucible 1 is constituted by a heating furnace and is heated so that the molten metal 6 has a constant temperature.
  • the shape of the crucible 1 is not limited to a bottomed cylindrical shape with a bottom surface formed into a downward arcuate surface.
  • the bottom may be a flat crucible type crucible or a rectangular tube.
  • a tank made of refractory or the like may be used.
  • the heating method of the furnace which comprises the crucible 1 may be an electric heating or a gas burner.
  • the temperature of the molten metal 6 only needs to exceed the solidification temperature, but it is more desirable that the temperature is lower than the temperature at which no solid phase exists in the molten metal while the cooling body 2 is immersed in the molten metal 6.
  • the cooling body 2 is formed in a truncated cone shape having a large diameter at the upper end side, and is installed at the lower end of the rotary shaft 3 that can move up and down.
  • the shape of the cooling body 2 is not limited and may be formed in a columnar shape having a constant outer diameter.
  • the rotating shaft 3 has a tubular shape, and a space is also formed inside the cooling body 2.
  • a refrigerant supply pipe 4 and a refrigerant discharge pipe 5 are inserted into the rotary shaft 3 so that air is supplied as a refrigerant. The supplied air is jetted into the internal space of the cooling body 2 through the refrigerant supply pipe 4 and then discharged through the refrigerant discharge pipe 5 inside the rotating shaft 3. Can be cooled from the inside.
  • the cooling body 2 is configured such that the rotating shaft 3 moves downward and can be immersed and rotated in the molten metal 6, and the cooling body 2 is immersed for a certain period of time while circulating air to cool the cooling body 2.
  • the refined lump adheres to the outer peripheral surface of 2 and grows. Then, the rotating shaft 3 is raised, the cooling body 2 to which the refined lump is attached is pulled up from the molten metal 6 and moved together with the rotating shaft 3 to a place where the purified lump is scraped off. Scrape and collect.
  • the horizontal minimum distance L1 between the inner peripheral surface of the crucible 1 and the outer peripheral surface of the cooling body 2 on the surface of the molten metal 6 is 150 mm or more, and in the entire area where the molten metal exists in the crucible.
  • the horizontal distance L2 between the inner peripheral surface of the molten metal holding container and the lowermost end of the cooling body is set to 100 mm or more.
  • the molten metal itself becomes a resistance, and the swirling flow of the molten metal 6 due to the rotation of the cooling body 2 is sufficiently slowed.
  • the dispersion of the impurity concentrated layer generated in the vicinity of the solidification interface is promoted, and the metal is purified. Efficiency is improved.
  • the swirling flow of the molten metal 6 is slowed down, purification with the molten metal prevented from being scattered is possible.
  • ensuring a large horizontal minimum distance L1 between the inner peripheral surface of the molten metal upper surface in the crucible 1 and the outer peripheral surface of the cooling body 2 is effective in slowing the swirling flow on the upper surface of the molten metal 6 and preventing the molten metal from scattering. Is big.
  • the distance L1 is preferably 200 mm or more and 500 mm or less
  • the horizontal distance L2 between the inner peripheral surface of the crucible 1 and the lowermost end of the cooling body 2 is preferably set to 150 mm or more and 500 mm or less. Even if L1 and L2 are set to be larger than 500 mm, it is not possible to obtain a further effect of slowing the swirl flow of the molten metal 6 and the purification efficiency is saturated, which is useless.
  • the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is preferably 200 mm or more. If the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is less than 200 mm, the weight of each lump is reduced and the productivity is not good. Therefore, by setting the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 to 200 mm or more, high purification efficiency can be obtained while ensuring productivity.
  • the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is preferably set to 500 mm or less.
  • the rotating device for rotationally driving the cooling body 2 becomes large.
  • the cooling body It is possible to prevent the rotating device 2 from becoming large and to suppress the difficulty of installation.
  • the shortest horizontal distance L1 between the inner peripheral surface of the upper surface of the molten metal 6 in the crucible 1 and the outer peripheral surface of the cooling body 2 is 150 mm or more.
  • the inner diameter D of the upper surface of the molten metal of the crucible 1 is 500 mm or more. In particular, it should be 650 mm or more.
  • the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is set to 200 mm or more by setting the inner diameter D on the upper surface of the molten metal of the crucible 1 to 650 mm or more, the inner peripheral surface and the cooling body 2 on the upper surface of the molten metal of the crucible 1. Since the horizontal distance L1 between the outer peripheral surface of the steel plate and the horizontal distance L2 between the inner peripheral surface of the crucible 1 and the lowermost end of the cooling body 2 can be secured sufficiently large, productivity can be secured and excellent purification efficiency can be obtained. Can do.
  • the inner diameter D on the upper surface of the molten metal of the crucible 1 is preferably 1300 mm or less. If the inner diameter D is larger than 1300 mm, the weight of the molten metal 6 that must be maintained at a temperature increases, so that a large amount of energy for heating such as a heater is required. Particularly preferably, the inner diameter D of the upper surface of the molten metal of the crucible 1 is 1000 mm or less.
  • the crucible 1 includes a crucible depth H, a length A from the bottom of the crucible to the bottom of the cooling body 2, an immersion depth a in the molten metal 6 in the cooling body 2,
  • the relationship of the inner diameter of the opening (in this embodiment, equal to the inner diameter of the upper surface of the molten metal of the crucible 1) D preferably satisfies the condition of H ⁇ A + 2a ⁇ D / 20. When such a condition is satisfied, the length from the surface of the molten metal 6 to the upper part of the crucible 1 is sufficiently secured for the immersion depth a in the molten metal 6 in the cooling body 2. It is possible to further suppress the dispersion of the molten metal to the outside.
  • FIG. 1 is a diagram for explaining a schematic configuration of a substance purification apparatus according to an embodiment of the present invention and a substance purification method using the same.
  • the substance is a metal such as aluminum.
  • reference numeral 1 denotes a crucible having a bottomed cylindrical shape as a molten metal holding container and a bottom surface formed in a downward arcuate surface, and a molten metal (also referred to as molten metal) 6 such as aluminum is accommodated and held in the crucible 1.
  • the crucible 1 is constituted by a heating furnace and is heated so that the molten metal 6 has a constant temperature.
  • the shape of the crucible 1 is not limited to a bottomed cylindrical shape with a bottom surface formed into a downward arcuate surface.
  • the bottom may be a flat crucible type crucible or a rectangular tube.
  • a tank made of refractory or the like may be used.
  • the heating method of the furnace which comprises the crucible 1 may be an electric heating or a gas burner.
  • the temperature of the molten metal 6 only needs to exceed the solidification temperature, but it is more desirable that the temperature is lower than the temperature at which no solid phase exists in the molten metal while the cooling body 2 is immersed in the molten metal 6.
  • the cooling body 2 is formed in a truncated cone shape having a large diameter at the upper end side, and is installed at the lower end of the rotary shaft 3 that can move up and down.
  • the shape of the cooling body 2 is not limited and may be formed in a columnar shape having a constant outer diameter.
  • the rotating shaft 3 has a tubular shape, and a space is also formed inside the cooling body 2.
  • a refrigerant supply pipe 4 and a refrigerant discharge pipe 5 are inserted into the rotary shaft 3 so that air is supplied as a refrigerant. The supplied air is jetted into the internal space of the cooling body 2 through the refrigerant supply pipe 4 and then discharged through the refrigerant discharge pipe 5 inside the rotating shaft 3. Can be cooled from the inside.
  • the cooling body 2 is configured such that the rotating shaft 3 moves downward and can be immersed and rotated in the molten metal 6, and the cooling body 2 is immersed for a certain period of time while circulating air to cool the cooling body 2.
  • the refined lump adheres to the outer peripheral surface of 2 and grows. Then, the rotating shaft 3 is raised, the cooling body 2 to which the refined lump is attached is pulled up from the molten metal 6 and moved together with the rotating shaft 3 to a place where the purified lump is scraped off. Scrape and collect.
  • the ratio A / a between the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 and the immersion depth a of the cooling body 2 in the molten metal 6 is 0.3 ⁇
  • Purification is performed with A / a ⁇ 3.0.
  • the axis of the cooling body 2 may be shifted from the center of the crucible 1, but at this time, the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 is such that the axis of the cooling body 2 is as shown in FIG. It is the distance from the center of the bottom surface of the cooling body 2 that passes through to the bottom surface of the crucible 1 directly below.
  • the ratio A / a between the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 and the immersion depth a of the cooling body 2 in the molten metal 6 is set to 0.3 ⁇ A / a ⁇ 3.0.
  • a large amount of the molten metal 6 exists between the inner peripheral surfaces of the cooling body 2 and the crucible 1, so that the molten metal 6 itself becomes a resistance, and the swirling flow of the molten metal 6 due to the rotation of the cooling body 2 occurs.
  • the dispersion of the impurity concentrated layer generated in the vicinity of the solidification interface is promoted, and the metal purification efficiency is improved.
  • a particularly preferable value of the ratio A / a between the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 and the immersion depth a of the cooling body 2 in the molten metal 6 is 0.5 ⁇ A / a ⁇ 2. 0.
  • the immersion depth a of the cooling body 2 in the molten metal 6 is preferably 150 mm or more and 500 mm or less, and the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 is preferably 700 mm or less. If the immersion depth “a” of the cooling body 2 in the molten metal 6 is less than 150 mm, the total height of the refined mass is low and the mass is low, which may result in poor productivity. On the contrary, if the immersion depth a of the cooling body 2 in the molten metal 6 exceeds 500 mm, the rotating device of the cooling body 2 becomes large, and the degree of difficulty in equipment installation becomes high.
  • the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 exceeds 700 mm, the amount of molten metal held in the crucible 1 increases, and a large amount of energy for heating such as a heater may be required.
  • a more preferable value of the immersion depth a in the molten metal 6 of the cooling body 2 is 200 mm or more and 400 mm or less, and a more preferable value of the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 is 600 mm or less.
  • the inner peripheral surface of the molten metal holding container is in the entire shortest distance L1 in the horizontal direction between the inner peripheral surface of the crucible 1 and the outer peripheral surface of the cooling body 2 on the surface of the molten metal 6 over 150 mm.
  • the distance L2 in the horizontal direction at the lowermost end of the cooling body is preferably 100 mm or more.
  • the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is preferably 200 mm or more. If the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is less than 200 mm, the weight of each lump is reduced and the productivity is not good. Therefore, by setting the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 to 200 mm or more, high purification efficiency can be obtained while ensuring productivity.
  • the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is preferably set to 500 mm or less.
  • the rotating device for rotationally driving the cooling body 2 becomes large.
  • the cooling body It is possible to prevent the rotating device 2 from becoming large and to suppress the difficulty of installation.
  • the shortest horizontal distance L1 between the inner peripheral surface of the upper surface of the molten metal 6 in the crucible 1 and the outer peripheral surface of the cooling body 2 is 150 mm or more.
  • the inner diameter D of the upper surface of the molten metal of the crucible 1 is 500 mm or more. In particular, it should be 650 mm or more.
  • the outer diameter d of the cooling body 2 on the upper surface of the molten metal 6 is set to 200 mm or more by setting the inner diameter D on the upper surface of the molten metal of the crucible 1 to 650 mm or more, the inner peripheral surface and the cooling body 2 on the upper surface of the molten metal of the crucible 1. Since the horizontal distance L1 between the outer peripheral surface of the steel plate and the horizontal distance L2 between the inner peripheral surface of the crucible 1 and the lowermost end of the cooling body 2 can be secured sufficiently large, productivity can be secured and excellent purification efficiency can be obtained. Can do.
  • the inner diameter D on the upper surface of the molten metal of the crucible 1 is preferably 1300 mm or less. If the inner diameter D is larger than 1300 mm, the weight of the molten metal 6 that must be maintained at a temperature increases, so that a large amount of energy for heating such as a heater is required. Particularly preferably, the inner diameter D of the upper surface of the molten metal of the crucible 1 is 1000 mm or less.
  • H is 1000 mm or more
  • a + 2a ⁇ D / 20 is 1000 mm or more, the crucible height becomes excessive with respect to the molten metal splash, and the crucible cost is increased. Therefore, a value of ⁇ 200 mm is an appropriate value.
  • the peripheral speed of the outer peripheral surface of the cooling body 2 when the cooling body 2 is immersed in the molten metal 6 is preferably in the range of 700 mm / s or more and less than 8000 mm / s, more preferably 1500 mm / s. As mentioned above, it is the range below 6000 mm / s.
  • the peripheral speed here refers to the moving speed of the outer peripheral surface of the cooling body 2 itself, and is a value unrelated to the moving speed of the molten metal 6.
  • the time from when the lower end of the cooling body 2 touches the molten metal 6 until the cooling body 2 is immersed to the maximum depth is “when immersed”. That is, the peripheral speed of the outer peripheral surface of the cooling body 2 is set to 700 mm / s or more and less than 8000 mm / s until the cooling body 2 is immersed to a predetermined depth after the lower end of the cooling body 2 touches the molten metal 2. It is good to hold.
  • the peripheral speed is less than 700 mm / s, the impurity concentration in the metal crystallized in the vicinity of the outer peripheral surface of the cooling body 2 is high, and as a result, the impurity concentration in the crystallized metal is high.
  • the peripheral speed of the outer peripheral surface of the cooling body 2 is preferably as fast as possible, but the peripheral speed is too high at 8000 mm / s or more, and the molten metal on the molten metal surface scatters when the cooling body 2 is immersed. May cause operational problems.
  • the shape of the cooling body 2 is not particularly limited, and may be formed in a columnar shape with a constant outer diameter, and the outer diameter as it reaches the lower end as in this embodiment. May be formed in an inverted frustoconical shape (tapered shape) that is continuously reduced, or other shapes, but in all parts immersed in the molten metal of the cooling body 2,
  • the peripheral speed is preferably maintained at 700 mm / s or more and less than 8000 mm / s.
  • the temperature of the cooling body 2 is preferably set to a metal solidus temperature x 0.7 or higher (470 ° C. or higher in the case of aluminum) and lower than the solidus temperature. If necessary, it may be heated by a heating device such as a heater.
  • a heating device such as a heater.
  • the preferable temperature of the cooling body 2 when immersed in the molten metal 6 is the solidus temperature x 0.8 or more and the solidus temperature or less, more preferably the solidus temperature x 0.9 or more and the solidus temperature or less. It is.
  • the metal crystallizes on the outer peripheral surface of the cooling body 2 by the rotation of the cooling body 2 immersed in the molten metal 6. If the cooling body 2 is pulled up from the molten metal 6 with the rotation of the cooling body 2 stopped after a predetermined amount of metal has crystallized, the following problems may occur.
  • the peripheral speed of the cooling body 2 when the cooling body 2 is pulled up from the molten metal 6 is preferably as fast as possible.
  • the peripheral speed at the interface between the refined metal adhering (crystallized) to the cooling body 2 and the molten metal 6 is preferably set to 700 mm / s or more.
  • the peripheral speed is less than 700 mm / s, a metal having a high impurity concentration is crystallized on the surface of the refined metal, and as a result, the impurity concentration of the entire refined metal may be increased. More preferably, it is set to 1500 mm / s or more.
  • the peripheral speed of the refined metal adhering (crystallized) to the cooled body 2 when the cooled body 2 is pulled up at the interface with the molten metal 6 is 8000 mm / s or more, the centrifugal force is too large.
  • the adhering molten metal 6 scatters above the liquid surface.
  • it is set to less than 7000 mm / s.
  • the time from when the uppermost portion of the refined metal crystallized on the cooling body 2 is pulled up from the molten metal 6 until the lowermost end of the refined metal is separated from the molten metal 6 is referred to as “when pulling up”. That is, the peripheral speed at the interface between the refined metal 6 and the molten metal 6 is maintained at 700 mm / s or more and less than 8000 mm / s until the top end of the refined metal is pulled up from the melt 6 and the bottom end of the refined metal is separated from the melt 6. It is desirable to do.
  • the peripheral speed of the cooling body 2 is intentionally increased at the initial stage of purification to increase the centrifugal force, so that a lump with weak adhesion to the cooling body 2 can be obtained in a short period of time during the initial stage of purification. It is good to make it peel off positively. That is, during the initial stage of purification immediately after the cooling body 2 is immersed, the maximum peripheral speed of the cooling body 2 is preferably set larger than the average peripheral speed of the cooling body 2 after the initial purification period. Specifically, it is preferable to set the maximum peripheral speed of the cooling body at the initial stage of purification to 1.1 times or more the average peripheral speed of the cooling body 2 after the initial purification period. If it is less than 1.1 times, sufficient centrifugal force cannot be obtained, and the purified metal having low adhesion to the cooling body 2 may not be sufficiently peeled off.
  • the initial purification period refers to the time from the start of purification to 0.1 times the total purification time. However, it is in the range of 10 seconds to 120 seconds.
  • the purification start here means when the cooling body 2 is immersed in the molten metal 6 to a specified depth. Even if the peripheral speed of the cooling body 2 is increased after exceeding 0.1 times the total purification time, or after exceeding 120 seconds from the start of purification, the purification metal is separated at a too late timing, and purification is performed for a certain period of time. This is not preferable because it reduces the amount of metal recovered. Further, if the time for increasing the peripheral speed of the cooling body 2 is less than 10 seconds from the start of purification, the purified metal having weak adhesion to the cooling body 2 cannot be sufficiently peeled off, which is not preferable.
  • examples of the substance to be purified include metals including eutectic impurities, metals such as silicon, magnesium, lead, and zinc, but substances other than metals may also be used.
  • the substance purified by the above has high purity, excellent properties and functions can be exhibited by using it for various processing and applications.
  • the material to be refined is a metal
  • the refined metal may be used for casting to produce a cast product, or the cast product may be rolled and used as various metal plates or metal foils. .
  • the purified metal when it is aluminum, it contains a peritectic element that forms peritectic crystals with aluminum and boron, and boron is in excess of 5 to 80 ppm by mass over the total chemical equivalent calculated as a metal boride with the peritectic element.
  • a metal boride is generated, a reaction step of removing peritectic elements by removing the generated metal boride and the metal boride generated in the dissolution step, and the molten metal obtained in the reaction step is moved to a purification chamber, In the refining chamber, segregation coagulation is performed to crystallize high purity aluminum from which eutectic elements including unreacted boron are removed by segregation solidification from the molten metal obtained in the reaction step. It is desirable to carry out the process. More preferably, the peritectic element in the aluminum refining raw material is at least one selected from the group consisting of Ti, Zr and V.
  • the boron concentration in the aluminum refining raw material is 5 to 80 ppm by mass in excess of the total chemical equivalent calculated as the metal boride with the peritectic element.
  • the crystal element and boron react with each other, and a longer reaction time is secured in combination with the reaction step to generate more metal boride, and the peritectic element is removed to obtain high-purity aluminum.
  • the thermal energy of dissolution is used for the reaction, the energy cost can be reduced.
  • the eutectic element containing unreacted boron can be removed from the molten metal, and aluminum with higher purity can be obtained.
  • the productivity of high-purity aluminum is good. Furthermore, since the molten metal obtained in the reaction process is moved to the refining chamber and the segregation solidification process is performed, the productivity of high-purity aluminum is good.
  • FIG. 2 is a plan view of a substance refining apparatus using the molten metal heating and holding apparatus 100 according to one embodiment of the present invention
  • FIG. 3 is a cross-sectional view taken along line III-III in FIG. 2
  • FIG. 6 is a longitudinal sectional view of a crucible 61.
  • the substance is a metal such as aluminum will be described.
  • reference numeral 200 denotes an apparatus main body having an upper surface opening formed of a refractory material, and the apparatus main body 200 has a substantially cubic crucible housing space 201.
  • a crucible 61 having a circular cross section in a circular cross section is placed in a state of being placed on a placing table 62.
  • the crucible 61 contains a molten metal 63 that is a molten metal to be refined.
  • the upper opening of the crucible 61 is covered and closed by a first lid 64 having a diameter larger than that of the opening so that the temperature in the crucible 61 is prevented from being lowered, and the first lid 64 is thickened.
  • a cooling body 66 that penetrates in the vertical direction and is attached to the lower end of the rotating shaft 65 is disposed.
  • the rotating shaft 65 supports the cooling body 66 so as to be rotatable and vertically and horizontally movable by a rotation drive device (not shown), and the cooling body 66 moves downward at the time of metal refining, so that the molten metal 63 in the crucible 61 is moved. It is supposed to be immersed in it.
  • the case where the first lid 64 is formed by a single member is shown, but a plurality of members may be combined in a plane.
  • the material of the crucible 61 is not limited, but since the inner surface is in contact with the molten metal 63 and is heated from the outer surface, it is necessary to have heat resistance that does not melt at a high temperature and does not cause an extreme decrease in strength. . Specifically, graphite, ceramics, composite materials of these, and the like can be recommended.
  • the upper part of the space surrounding the crucible 61 is covered and closed by a second lid 67 separate from the first lid 64 so that the upper opening of the apparatus main body 200 can be opened. It is closed by the second lid 67 except for the heat to prevent the heat from escaping.
  • a hole 671 corresponding to the upper shape of the crucible is provided at the center of the second lid 67, and the upper end of the crucible 61 is inserted into the hole 671.
  • the first lid 64 is placed over the opening of the crucible 61 in a state where the lower surface peripheral end portion of the first lid 64 is in contact with the second lid 67 or through a heat-resistant packing or the like.
  • the department is closed.
  • the second lid 67 may also be formed by a single member, or may be formed by combining a plurality of members in a plane.
  • an upper heater 70 and a lower heater 80 are disposed below the second lid 67.
  • the upper heater 70 is a heater for heating the crucible inner wall 61a exposed in the space 61b above the molten metal.
  • the upper heater 70 is provided in the upper region in the height direction of the crucible 61 in the space around the crucible 61.
  • H2 shown in FIG. 4 is the height of the crucible inner wall 61a exposed to the space 61b above the molten metal, and the upper heater 70 is provided so as to cover the region of the height H2.
  • the upper heater 70 is configured by bending a thin rod-shaped heater material so as to be arranged along the outer peripheral surface of the crucible 61. Specifically, on both outer sides in the radial direction of the crucible 61, two rod-like support members 71, 71 having upper ends fixed to the second lid 67 are arranged in a hanging manner. While being supported by the two support members 71, 71, and as necessary, the heater material is folded up and down by the support members 71, 71, as if extending in the horizontal direction over the entire outer periphery of the crucible 61. The ring-shaped heater material is arranged as if it were arranged at intervals in the vertical direction.
  • the upper heater 70 is held by the second lid 67 via the support members 71 and 71. And by connecting the power supply unit of the power supply device drawn from the outside of the molten metal heating and holding device to the connection terminals 72 and 72 at both ends of the heater material and energizing, power is supplied from the power supply device to the upper heater 70, The upper heater 70 generates heat to heat the upper region of the crucible 61, and consequently heat the crucible inner wall 61a exposed in the space 61b above the molten metal.
  • the example using one heater material was shown as the upper heater 70, two or more heater materials may be used.
  • the upper heater 70 is bent so as to surround the crucible 61 as described above, it is desirable to use a metal heater, and a material that can withstand high temperatures such as stainless steel, nichrome, cantal, and the like. It is desirable to use it.
  • the material of the support member 71 is not particularly limited, but the upper heater 70 may be supported by the support member 71 through an insulating material such as insulator to ensure insulation with the upper heater 70.
  • the upper heater 70 is preferably covered with a heat-resistant insulating material such as ceramic so that even if the molten metal 63 scatters outside the crucible, no disconnection occurs immediately.
  • the upper heater 70 may be disposed close to the outer peripheral surface of the crucible 61. However, when the upper heater 70 is covered with a heat-resistant insulating material, the outer peripheral surface of the upper heater 70 and the crucible 61 may be in contact with each other.
  • the upper heater 70 is held by the second lid 67 via the support member 71, the upper heater 70 is removed from the apparatus main body 200 by removing the second lid 67 from the apparatus main body 200. This makes it easy to replace and maintain the heater 70.
  • the lower heater 80 is a heater for heating the molten metal 63 accommodated in the crucible 61.
  • the lower heater 80 is provided in the lower region in the height direction of the crucible 61 in the space around the crucible 61.
  • H1 shown in FIG. 4 is the height of the crucible 61 in the molten metal accommodating part (depth of the molten metal 63), and the lower heater 80 is provided so as to cover the region of the height H1.
  • the lower heater 80 is composed of a plurality of rod-shaped heater materials that penetrate the apparatus main body 200 horizontally in the front-rear direction of the drawing on both outer sides of the crucible 61 and are spaced apart in the height direction. Each heater material can be exchanged from outside the apparatus by pulling out in the length direction, and a connection terminal with the power supply apparatus exists outside the apparatus.
  • the lower heater 80 may be made of the same material as the upper heater 70 or may be covered with a heat-resistant insulating material such as ceramic. However, since the complicated bending process is not required, the ceramic itself becomes a heating element. A heater may be used.
  • the metal purification by the substance purification apparatus shown in FIG. 2 is performed as follows. That is, after the molten metal 63 is accommodated in the crucible 61, the space around the crucible 61 is closed by the second lid 67, the opening of the crucible 61 is closed by the first lid 64, and the inside of the crucible 61 is closed by the lower heater 80. While the molten metal 63 is heated and the crucible inner wall 61a exposed to the space 61b above the molten metal is heated by the upper heater 70, the cooling body 66 is immersed in the molten metal 63 in the crucible 61 and the refrigerant is supplied into the cooling body 66.
  • the refined metal is slowly crystallized on the peripheral surface of the cooling body 66.
  • This order is not particularly limited, and there is no problem even if the cooling body 66 is immersed in the molten metal 63 while rotating.
  • the eutectic impurities are discharged into the liquid phase, and an impurity concentrated layer of the eutectic impurities is formed in the liquid phase near the solidification interface.
  • the relative speed between the cooling body 66 and the molten metal 63 causes the impurity in the impurity concentrated layer. Impurities are dispersed throughout the liquid phase. When solidification proceeds in this state, a mass of metal with a purity much higher than that of the original molten metal is obtained on the peripheral surface of the cooling body 66.
  • the molten metal 63 Due to the rotation of the cooling body 66 immersed in the molten metal 63, the molten metal 63 swings or adheres to the crucible inner wall 61a that scatters upward. However, since the crucible inner wall 61a is heated by the upper heater 70, it adheres to the crucible inner wall 61a. The metal thus obtained flows down and merges into the molten metal 63 without solidifying, and adhesion and solidification to the crucible inner wall 61a can be prevented.
  • the upper heater 70 is provided separately from the lower heater 80, the temperature of the crucible inner wall 61a exposed to the space 61b above the molten metal can be controlled separately from the temperature of the molten metal 63, and the temperature of the crucible inner wall 61a. Can be controlled to an optimum temperature for preventing adhesion and solidification of the molten metal, and adhesion and solidification of the molten metal can be further prevented.
  • the output of the upper heater 70 is P (W), and the surface area of the crucible inner wall 61a exposed to the space 61b above the molten metal.
  • the output of the upper heater 70 is preferably set so as to satisfy 1000 ⁇ P / B ⁇ 12000. If P / B is less than 1000, the effect of preventing the adhesion and solidification of the molten metal on the crucible inner wall 61a may not be exhibited more satisfactorily. Even if P / B exceeds 12000, an increase in the effect cannot be expected, resulting in an increase in energy loss. It is particularly preferable to set 2000 ⁇ P / B ⁇ 9000.
  • the electric power of the upper heater 70 and the lower heater 80 may be collectively controlled by the same electric system instead of individually controlling by separate electric systems. Further, it is desirable that temperature measuring means such as a thermocouple for temperature adjustment be provided separately for the upper heater control and the lower heater control.
  • a first lid 64 that closes the upper end opening of the crucible 61 and a second lid 67 that closes the upper part of the space around the crucible 61 are provided separately, and the upper heater 70 is a second heater. Since the upper heater 70 can be taken out of the apparatus main body 200 by removing the second lid 67, maintenance and replacement work of the upper heater 70 can be easily performed. And maintainability is excellent.
  • the upper end opening of the crucible 61 that accommodates the molten metal 63 is closed by the first lid 64 and the upper part of the space around the crucible 61 is closed by the second lid 67, the inside of the crucible 61 is compared. Even if the molten metal 63 is scattered outside the crucible, the second lid 67 can prevent the scattered molten metal from entering the surrounding space of the crucible 61, and there is a risk of damage to the upper heater 70 and the lower heater 80. Can be reduced.
  • the metal is refined, the crucible 61 from which the first lid 64 has been removed is opened after a lapse of a certain time, the cooling body 66 is pulled up together with the purified purified metal 5 and the periphery of the cooling body 66 is removed by a scraping device (not shown). Scrape off the purified metal crystallized on the surface.
  • the cooling body 66 may be stationary or may be rotated. Then, the cooling body 66 is heated so that it may become predetermined temperature, and it moves to the crucible 61 again and refine
  • This modified example relates to a material refining device using a molten metal holding device as in the third embodiment shown in FIGS. 2 and 3, but a plurality of crucibles are used instead of one. ing.
  • reference numeral 200 denotes an apparatus main body having an upper surface opening formed of a refractory.
  • the apparatus main body 200 has a crucible housing space 201 having a rectangular cross section and a substantially rectangular vertical section. Yes.
  • a plurality of crucibles 61, 61... Having a circular cross section in a circular cross section are arranged at equal intervals in a state where they are placed on a pedestal 62, respectively.
  • Each crucible 61 contains a molten metal 63 to be purified. Similar to the embodiment shown in FIG. 2, the upper opening of each crucible 61 is closed by a first lid 64 and penetrates the first lid 64 in the thickness direction to A cooling body 66 attached to the lower end is arranged. Further, the upper part of the surrounding space of each crucible 61 is covered and closed by a second lid 67 separate from the first lid 64 so as to be opened and closed.
  • the upper opening of the apparatus main body 200 is closed by the plurality of second lids 67 except for the opening of each crucible 61.
  • a hole 671 corresponding to the upper shape of the crucible 61 is provided at the center of the second lid 67, and the upper end of the crucible 61 is inserted into the hole 671.
  • the first lid 64 is placed on the opening of the crucible 61 in a state where the lower surface peripheral end portion of the first lid 64 is in contact with the second lid 67 and closes the opening.
  • a communication rod 90 is connected to the upper part of each crucible 61, and communicates with other crucibles 61 adjacent to each other via the communication rod 90.
  • the communication rod 90 is provided for the purpose of performing a refining operation while simplifying the operation of housing the molten metal 63 in each crucible 61. That is, when the molten metal 63 is poured into one of the crucibles 61 or overflows, the molten metal 63 automatically flows into other crucibles 61 adjacent to each other via the communication rod 90.
  • an upper heater 70 for heating the crucible inner wall 61a exposed in the space 61b above the molten metal and a lower heater 80 for heating the molten metal 63 are provided in the surrounding space of each crucible 61.
  • the upper heater 70 is provided in an upper region in the height direction of the crucible 61 in the space around the crucible 61, and is provided so as to cover the region of the height H2 of the crucible inner wall 61a exposed to the space 61b above the molten metal. ing.
  • the lower heater 80 is provided in a lower region in the height direction of the crucible 61 in the space around the crucible 61 so as to cover a region of the height H1 of the molten metal accommodating portion in the crucible 61.
  • the configuration of the lower heater 80 is the same as that of the embodiment shown in FIG.
  • the upper heater 70 is arranged along the shape of the outer peripheral surface of the crucible 61 while avoiding the communication rod 90. Specifically, in the upper part of the crucible 61, two upper ends are fixed to the second lid 67 at positions where the communication rods 90 projecting on both sides in the radial direction are sandwiched.
  • the support member 71 is arranged in a hanging shape. Then, as shown in FIG. 8, while being supported by two left and right support members 71 located on one side of the front and rear upper half surfaces divided by the two communication rods 90, a heater is used as necessary.
  • the upper heater 70 is arranged in close proximity along the shape of the upper half circumferential surface.
  • the upper heater 70 is disposed close to the upper half surface along the shape of the upper half surface.
  • the upper heater 70 is divided into two heater groups for each of the upper half circumferential surfaces of the front and rear of the crucible 61, both of which are held by the second lid 67 via the support member 71. Then, power is supplied from the power supply device to the upper heater 70 by connecting the power supply portion of the power supply device drawn from outside the molten metal heating and holding device 100 to the connection terminals 72 at both ends of the heater material in each heater group.
  • the crucible inner wall 61a that is supplied and heated by the upper heater 70 and exposed to the space 61b above the molten metal is heated.
  • two or more heater materials may be used.
  • the material of the upper heater 70 it is desirable to use, for example, stainless steel, which is a material that can be bent and can withstand high temperatures, and is preferably covered with a heat-resistant insulating material such as ceramic. When covered with a heat-resistant insulating material, the upper heater 70 and the crucible 61 may be in contact with each other.
  • the molten metal 63 is swung or scattered above the molten metal by the rotation of the cooling body 66 immersed in the molten metal 63, and adheres to the crucible inner wall 61a. Since the crucible inner wall 61a is heated by the upper heater 70, the molten metal scattered and adhering can flow down and join the molten metal 63 without solidifying, thereby preventing the molten metal from adhering and solidifying.
  • the upper heater 70 is provided separately from the lower heater 80, the temperature of the crucible inner wall 61a exposed to the space 61b above the molten metal can be controlled separately from the temperature of the molten metal 63, and the crucible inner wall 61a The temperature can be controlled to an optimum temperature for preventing adhesion and solidification of the molten metal, and adhesion and solidification of the molten metal can be further prevented.
  • the output of the upper heater 70 is A (W), and the surface area of the crucible inner wall 61a exposed to the space 61b above the molten metal.
  • the output of the upper heater 70 is preferably set so as to satisfy 1000 ⁇ A / B ⁇ 12000, and temperature measuring means such as a thermocouple for temperature adjustment is used for controlling the upper heater It is desirable to be provided separately from the lower heater control.
  • the upper heater 70 can be removed from the apparatus main body 200 by removing the second lid 67, even when the plurality of crucibles 61 are communicated by the communication rod 90 and the removal of the upper heater 70 is not easy.
  • the maintenance work and the replacement work of the upper heater 70 can be easily performed, and the maintainability is excellent.
  • the second lid 67 can prevent the scattered molten metal 63 from entering the surrounding space of the crucible 61.
  • the crucible and cooling body used in this system are the same as the crucible and cooling body described in the above-mentioned [First Embodiment] to [Third Embodiment].
  • the conditions for purifying a substance such as metal using each crucible and cooling body are also the same as the purification conditions described in the above-mentioned [First Embodiment] to [Third Embodiment].
  • 1) Primary line The continuous purification apparatus for high-purity aluminum according to this embodiment includes a melting furnace for melting aluminum, and sequentially sends the molten metal from the melting furnace to a plurality of crucibles connected in series.
  • a primary line is formed by using a series of devices for discharging molten metal from the crucible to the outside as a set of lines. At this time, it is assumed that each crucible is paired with a rotatable cooling body for crystallizing high-purity aluminum in the molten metal.
  • a plurality of crucibles may be divided into a plurality of compartments by dividing a large tank into partitions, and each compartment may be used as a crucible, and a communicating port may be provided in the partition so that the molten metal passes through each crucible.
  • a plurality of crucibles may be arranged in series, and the crucibles may be connected by a basket.
  • the aluminum is crystallized out of the crucible by rotating it up while rotating.
  • the refining system defined in the present embodiment is composed of an Nth-order line (provided that 2 ⁇ N) provided with two or more sets of the above-mentioned lines.
  • the high-purity aluminum mass recovered by adhering and solidifying is melted in the subsequent n-th line melting furnace, and the molten metal is fed into a plurality of serially connected crucibles through a gutter or a communication hole. Then, aluminum is crystallized again on the cooling body, and recovery and purification are repeated.
  • the number of crucibles and pairs of crucibles in the nth order line needs to be reduced from the number of crucibles and pairs of crucibles in the (n-1) th order line.
  • recovery total weight SW2 of the high purity aluminum refinery lump with respect to input aluminum raw material weight SW1 be a collection rate (SW2 / SW1).
  • the recovery rate (SW2 / SW1) is always less than 1, and in order to reduce the impurity concentration from the recovered aluminum lump, it is necessary to lower the recovery rate.
  • the number of crucibles is n in order to link the time required for the aluminum block to be extracted in the n-th line by the cooling body and the time required for the aluminum block to be extracted in the (n-1) -th line. In the next line, it must be reduced according to the recovery rate than the (n-1) th order.
  • b When the number of crucibles in the n-th order line is smaller than the number of crucibles in the n-th order line, the smaller the ratio of the recovered weight of the n-th order line to the recovered weight of the n-th order line, the higher the purity. An aluminum mass is obtained.
  • c The purification line in which the crucible is reduced with the order as described above is installed in parallel up to the n-th line, thereby improving the energy efficiency and reducing the eutectic impurities with a small equipment area. Equipment and systems that can be reduced more than equipment can be obtained. At this time, for the purpose of comprehensively improving the energy efficiency of this line, it is desirable that the distance between the lines be as close as possible.
  • the molten metal discharged from the secondary or higher n-th line may be immediately returned to the (n-1) next-line melting furnace without being cooled and solidified, and may be reused.
  • the melting furnace of the (n-1) th line can use a raw material having the same level of purity as the melting raw material without requiring melting energy, and the energy efficiency is further increased.
  • the order of the line (Nth order) is preferably secondary or tertiary. Even if the equipment is constructed beyond the third order, the complexity of the equipment increases and the superiority in terms of operation and economy becomes poor.
  • the impurity concentration of the molten metal in the crucibles that are continuously connected in series in each of the primary to n-th lines gradually increases from the first holding tank toward the final holding tank. For this reason, the more crucibles connected to one line, the higher the collection efficiency of the refined lump (Al purity with respect to the same recovered weight). However, if the amount is excessive, operation such as control of the molten metal temperature becomes difficult.
  • the number of crucibles consecutive in series is 8 to 25 in the primary line, and the ratio of the number of n-th crucibles to the number of (n-1) -th crucibles is 0.5 to 0.8. It is preferable to set to. 4) Addition of boron In at least one of the N-th lines, boron may be added to the melting furnaces 11, 21, and 31 to react peritectic impurities such as Ti, Zr, and V with boron. Moreover, the stirring tank which can add a boron may be installed between the melting furnace and the crucible with a cooling body.
  • boron and peritectic impurities such as Ti, Zr, and V can be reacted.
  • boron may be added not only in the melting furnace and the stirring tank but also in a tank connecting the melting furnace and the stirring tank.
  • Boron is generally added as an Al—B (boron / boron) master alloy, but is not limited thereto.
  • a non-contact type molten metal stirring with a permanent magnet there are a non-contact type molten metal stirring with a permanent magnet, a stirring with a graphite rotor, or a method of blowing a processing gas into the molten metal.
  • peritectic impurities By adding boron and stirring as described above, peritectic elements such as Ti, Zr, V and the like react with boron to form an insoluble boron compound and remove it from the molten metal. Impurities can be removed. At this time, the separation of the insoluble boron compound can be mechanically removed as a float on the surface of the stirring tank.
  • the aluminum refining system comprises a plurality of sets of lines, each of which is composed of a device that continuously purifies aluminum to obtain high-purity aluminum.
  • a melting furnace 11 for melting aluminum to be purified containing eutectic impurities and peritectic impurities, and preferably a stirring tank 12 is arranged continuously in the melting furnace 11.
  • boron is added as an Al—B master alloy to the molten aluminum received from the melting furnace 11, and bubbles are released from Ar gas and the dispersing device is lowered to be immersed in the molten aluminum in the stirring tank 12. Then, bubbles are released by the driving means and rotated. This state will be described in detail with reference to FIG.
  • crucibles 13, 13... are continuously arranged in series. These melting furnace 11, stirring tank 12, crucibles 13, 13... Are connected to each other by a bowl 15 for feeding molten metal.
  • the cooling bodies 130, 130... Cooled with the cooling fluid are immersed. If the temperature of the molten aluminum in the crucibles 13, 13... Is maintained at a temperature exceeding the freezing point, the purity of the purity to be purified on the surface of each cooling body 130, 130. High aluminum crystallizes out and a high purity aluminum mass is formed.
  • the molten aluminum having a high impurity concentration in the crucibles 13, 13... Is discharged to the discharged molten metal receiver 14.
  • each cooling body 130, 130... The aluminum lump crystallized and extracted on the surface of each cooling body 130, 130... Is pulled up while rotating, and after the rotation stops, it is mechanically recovered from the cooling bodies 130, 130.
  • the cooling fluid supplied to each of the cooling bodies 130, 130... Is more productive as the cooling capacity is larger.
  • the solidification rate is excessively high, the impurity concentration of the recovered aluminum mass is high. Become. For this reason, it is necessary to give consideration to the optimum purification conditions for the balance between the recovered weight suitable for the purity of the aluminum mass to be purified and the impurity concentration.
  • the collected refined mass is subsequently fed into the melting furnace 21 of the secondary line, and the molten metal is sent from the melting furnace 21 to the stirring tank 22 and the continuous crucibles 23, 23,.
  • a method of simultaneously collecting from all the cooling bodies 130, 130... May be used, but a method of sequentially collecting in order to provide continuity in operation is desirable.
  • the number of crucibles 23 in the secondary line is set to five, which is smaller than the number of crucibles 13 in the primary line.
  • the molten metal having a low impurity concentration dissolved in the melting furnace 21 in the secondary line is stirred in the stirring tank 22 after adding boron in the melting furnace 21 or the stirring tank 22 as in the primary line.
  • the molten metal from the stirring tank 22 is sent to the crucibles 23, 23,... Continuously connected in series, and when the predetermined amount is satisfied, the inside is filled with air, gas, water vapor, etc.
  • the cooling bodies 230, 230... Cooled by the cooling fluid are immersed in the molten aluminum in the crucibles 23, 23.
  • Aluminum that is higher than the purity obtained in the primary line crystallizes and forms a lump.
  • the molten aluminum having a high impurity concentration in the crucible is discharged to the discharged molten metal receiver 24.
  • each cooling body 230, 230 ... in the secondary line is pulled up while rotating, and is recovered after the rotation stops.
  • the recovered refined mass is put into the melting furnace 31 of the subsequent third line, and the molten metal is sent from the melting furnace 31 to the stirring tank 32 and the continuous crucibles 33, 33,. .. Are successively collected by the cooling bodies 330, 330... Corresponding to the crucibles 33, 33.
  • the number of crucibles 33 in the tertiary line is set to three, which is smaller than the number of crucibles 13 in the secondary line.
  • a separation tank capable of removing the insoluble boron compound purified in the stirring tank may be provided between the stirring tank and the crucible.
  • the separation tank 35 is provided between the stirring tank 32 and the crucible 33 of the tertiary line.
  • the separation tank 35 not only separates the insoluble boron compound that has been floated and separated by bubbles, but also removes the insoluble boron compound that settles in the molten metal. For this reason, a filter may be installed in the separation tank. At this time, the molten aluminum having a high impurity concentration in the crucibles 33, 33... Is discharged to the discharged molten metal receiver 34.
  • FIG. 10 illustrates the configuration of the melting furnace 31, the stirring tank 32, the crucible 33, and the like in the tertiary line, but the configuration of the melting furnace, the stirring tank, and the crucible in the other lines is the same.
  • a connecting rod 36 is provided as a receiving rod for receiving the molten metal supplied from the melting furnace 31, and the connecting rod 36 as a molten metal discharge rod is disposed at the upper end of the crucible 33 farthest from the melting furnace 31.
  • the connecting rod 36 as a molten metal discharge rod is disposed at the upper end of the crucible 33 farthest from the melting furnace 31.
  • a dispersing device including a rotating shaft 321 that is driven to rotate up and down by a driving means (not shown) and a dispersing rotator 322 that is fixed to the lower end of the rotating shaft 321.
  • 320 is arranged.
  • a processing gas passage extending in the lengthwise direction is formed in the rotating shaft 321, and a processing gas blowout port (not shown) communicating with the processing gas passage is provided at the lower end surface of the dispersing rotator 322.
  • a plurality of stirring promoting protrusions are formed at intervals in the circumferential direction.
  • the vertical cross section of a substantially U-shaped horizontal section covering the inner end of the hot water outlet 323 and the portion of the inner surface of the stirring tank 32 that continues to the lower side of the hot water outlet 323.
  • a partition wall 324 is provided. The vertical partition wall 324 can prevent the insoluble boron compound generated by the reaction between boron and the peritectic element from flowing out into the crucible on the downstream side.
  • the molten metal that has passed through the stirring tank 32 flows into the separation tank 35.
  • the separation tank 35 is provided with a partition wall 351, and the molten metal 60 from which the insoluble boron compound and the insoluble boron compound settled in the molten metal are removed flows into the crucible 33 at the next stage.
  • Each of the crucibles 33, 33... Is arranged with the cooling bodies 330, 330.
  • Each rotary shaft 331 is formed with a cooling fluid passage (not shown) extending in the longitudinal direction.
  • each cooling body 330 has a bottomed inverted truncated cone shape whose cross-sectional area decreases downward, and an internal space communicating with the cooling fluid passage is formed, and the cooling fluid is passed through the cooling fluid passage to the internal space.
  • the outer peripheral surface in contact with the molten metal can be maintained at a predetermined temperature by supplying to the molten metal. Therefore, the cooling body 330 is preferably made of a material having good thermal conductivity, such as graphite, as well as not contaminating the molten metal by reaction with the molten aluminum.
  • the cooling body 330 is set to a height at which the portion excluding the upper end is immersed in the molten aluminum.
  • FIG. 11 shows another embodiment. In this example, it is composed of tertiary lines as in the system shown in FIG. 9, and the configuration of the apparatus in each line is shown in FIG. 9 except that the separation tank 35 in the tertiary line is not installed. It is the same as that.
  • the system shown in FIG. 11 has an opening through which an Al—B alloy or a boron-containing material equivalent thereto can be appropriately introduced in the melting furnace 21 and the stirring tank 22 in the secondary line.
  • the molten metal received from the melting furnace 21 by the receiving bowl reaches the stirring tank 22.
  • the surplus molten metal that has passed through the crucibles 33, 33,... Of the tertiary line is also returned from the final crucible 33 to the melting furnace 21 of the secondary line by the return device 37. .
  • Example 1 A molten aluminum (original molten metal) made of an aluminum raw material having an impurity concentration (mass ppm) shown in Table 1 was placed in the crucible 1 and purified.
  • the purification apparatus and purification conditions are as follows.
  • the crucible 1 uses a bottomed cylindrical shape with an inner diameter D (same as the inner diameter of the opening) D of 520 mm and a depth H of 800 mm on the upper surface of the molten metal, and the bottom surface is formed in a downward arc surface. It was.
  • the cooling body 2 is made of graphite having a large truncated cone shape on the upper end side and having an outer diameter d of 220 mm on the upper surface of the molten metal.
  • the shortest horizontal distance L1 between the inner peripheral surface on the upper surface of the molten metal of the crucible 1 and the outer peripheral surface of the cooling body 2 is 150 mm, and the inner peripheral surface of the crucible and the cooling body in the entire area of the molten aluminum in the crucible 1.
  • the horizontal distance L2 at the lowest end of 2 was 100 mm
  • the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 was 300 mm
  • the immersion depth a of the cooling body 2 in the molten aluminum 6 was 200 mm.
  • the temperature of the cooling body 2 was set to 350 ° C. when immersed in the molten metal 6, and the cooling body 2 was not rotated when the molten body 6 was immersed in the molten metal 6 and pulled up from the molten metal after purification for 6 minutes.
  • Examples 2 to 9, Comparative Example 1 At the shortest distance L1 in the horizontal direction between the inner peripheral surface of the molten metal upper surface of the crucible 1 and the outer peripheral surface of the cooling body 2, in the entire area where the molten metal is present in the crucible 1, The purification was performed under the same conditions as in Example 1 except that the horizontal distance L2, the inner diameter D on the upper surface of the molten metal of the crucible 1, and the outer diameter d of the cooling body 2 on the upper surface of the molten metal were set as shown in Table 1. The impurity concentration of the molten aluminum was as shown in Table 1. (Example 10) Under the conditions of Example 5, the temperature of the cooling body 2 was set to 470 ° C.
  • the cooling body 2 was immersed while rotating at a peripheral speed of 5000 mm / s, and the peripheral speed was maintained from the start of purification to the total purification time ⁇ 0.1. Thereafter, the peripheral speed was set to 4000 mm / s.
  • the peripheral speed of the bottom surface of the purified aluminum crystallized on the cooling body 2 is set to 2500 mm / s, and the bottom end of the cooling body 2 is completely removed from the molten aluminum. The rotational speed was maintained until it was pulled up.
  • Table 1 shows the weight, impurity concentration, and purification efficiency of the aluminum refined lump obtained as described above.
  • the purification efficiency is calculated by the ratio of the impurity concentration of the obtained aluminum refined lump to the impurity concentration contained in the original molten aluminum.
  • Table 1 shows the quality of energy efficiency, facility difficulty, and molten metal splash.
  • ⁇ is very good, ⁇ is good, ⁇ is normal, equipment difficulty is ⁇ is low, ⁇ is slightly low, ⁇ is normal, ⁇ about molten metal splash, ⁇ is not at all, ⁇ is almost Indicates no.
  • Example 10 As understood from the results in Table 1, Examples 1 to 10 had higher purification efficiency than Comparative Examples. Moreover, in Example 10, compared with Example 5, the refinement
  • Example 21 A molten aluminum (original molten metal) made of an aluminum material having an impurity concentration (mass ppm) shown in Table 2 was placed in the crucible 1 and subjected to a purification treatment.
  • the purification apparatus and purification conditions are as follows.
  • the crucible 1 has a bottomed cylindrical shape with an inner diameter D (same as the inner diameter of the opening) D of 480 mm and a depth H of 850 mm on the upper surface of the molten metal, and has a bottom surface formed in a downward arcuate surface. It was.
  • the cooling body 2 was made of graphite having a large truncated conical shape on the upper end side and having an outer diameter d of 180 mm on the molten metal upper surface.
  • the shortest horizontal distance L1 between the inner peripheral surface of the upper surface of the molten metal of the crucible 1 and the outer peripheral surface of the cooling body 2 is 150 mm, and the inner peripheral surface of the crucible 1 and the cooling in the entire region of the molten aluminum in the crucible 1.
  • the horizontal distance L2 at the lowermost end of the body 2 is 100 mm
  • the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 is 430 mm
  • the immersion depth a of the cooling body 2 in the molten aluminum 6 is 200 mm.
  • the value of A / a was 2.15.
  • the temperature of the cooling body 2 was set to 350 ° C. when immersed in the molten metal 6, and the cooling body 2 was not rotated when the molten body 6 was immersed in the molten metal 6 and pulled up from the molten metal after purification for 6 minutes.
  • Examples 22 to 30, Comparative Examples 21 to 22 Under the same conditions as in Example 21, except that the distance A from the bottom surface of the cooling body 2 to the bottom surface of the crucible 1 and the value of the immersion depth a in the molten aluminum 6 of the cooling body 2 were changed as shown in Table 1. Purification was performed. The impurity concentration of the molten aluminum was as shown in Table 1.
  • Example 31 Under the conditions of Example 24, the temperature of the cooling body 2 was set to 470 ° C. (solidus temperature of aluminum ⁇ 0.7) when immersing in the molten metal 6, and the minimum diameter portion of the eroded portion of the molten metal 6 was set. The cooling body 2 was immersed while rotating at a peripheral speed of 5000 mm / s, and the peripheral speed was maintained from the start of purification to the total purification time ⁇ 0.1. Thereafter, the peripheral speed was set to 4000 mm / s.
  • the peripheral speed of the bottom surface of the purified aluminum crystallized on the cooling body 2 is set to 2500 mm / s, and the bottom end of the cooling body 2 is completely removed from the molten aluminum. The rotational speed was maintained until it was pulled up.
  • Table 2 shows the weight, impurity concentration, and purification efficiency of the aluminum refined lump obtained as described above.
  • the purification efficiency is calculated by the ratio of the impurity concentration of the obtained aluminum refined lump to the impurity concentration contained in the original molten aluminum.
  • Table 2 shows the quality of energy efficiency and facility difficulty. As for energy efficiency, ⁇ is very good, ⁇ is good, ⁇ is normal, and facility difficulty is ⁇ is low, ⁇ is slightly low, and ⁇ is normal. About molten metal splashes, ⁇ means nothing, and ⁇ means almost none.
  • Examples 21 to 31 had higher purification efficiency than Comparative Example 21. Moreover, in Example 31, compared with Example 24, the refinement
  • Example according to the third embodiment (Example 41) Using the refining apparatus shown in FIG. 2, molten aluminum 63 was accommodated in one crucible 61 and the refining process was performed.
  • the purification apparatus and purification conditions are as follows.
  • the crucible 61 has a cylindrical shape with an inner diameter D of 500 mm and a height of 500 mm.
  • the crucible height H2 of the molten metal container is 300 mm, and the height H1 of the crucible inner wall 61a exposed in the space 61b above the molten metal is 200 mm. did.
  • the surface area B (heated surface area) of the crucible inner wall 61a is 0.314 m 2 .
  • the cooling body 66 is made of graphite having an outer diameter of 150 mm, compressed air: 1480 liters / minute is circulated in the hollow portion of the cooling body 66 as a cooling medium, and the rotational peripheral speed is 4.0 m / s. The product was purified for 6 minutes while rotating at a constant speed.
  • the output A of the upper heater 70 was set to 250 W, and the output of the lower heater 80 was set to 1000 W.
  • Examples 42-45 Except for changing the output setting value of the upper heater 70 as shown in Table 3, the refining process was performed under the same conditions as in Example 41, and the adhesion state of the molten aluminum on the crucible inner wall 61a exposed in the space 61b above the molten metal The energy consumption was evaluated.
  • Example 42-45 which satisfies the conditions, can suppress adhesion of aluminum to the crucible inner wall 1a as compared with Example 41 in which A / B is less than 1000.
  • Table 4 shows the composition of the aluminum raw material subjected to the purification system and the aluminum mass after purification
  • Table 5 shows each purification condition.
  • Example 51 As shown in FIG. 12, aluminum is purified by a continuous double purification system in which the number of crucibles 13 and 23 in which cooling bodies 130 and 230 are arranged is set to 10 for the primary line and 5 for the secondary line. did.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003% by weight.
  • the rotational speed of the carbon cooling body was 400 rpm, the inner surface was cooled by flowing air, purified in molten metal for 8 minutes, and the crystallized high-purity aluminum was pulled up and collected. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line and the secondary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate total weight recovered high-purity aluminum refining lump / input aluminum raw material weight
  • the average composition of the high-purity aluminum block obtained in the secondary line was Fe0.0016%, Si0.0023%, Ti0.002%, and V0.005%.
  • Example 52 aluminum is purified by a continuous double purification system in which the number of crucibles 13 and 23 in which cooling bodies 130 and 230 are arranged is set to 10 for the primary line and 5 for the secondary line. did.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%. Boron was added to the stirring tanks 12 and 22 arranged in the next stage of the melting furnaces 11 and 21 in the primary line and the secondary line so that the concentration became 0.007%.
  • the rotational speed of the soot cooling body was 400 rpm, the inner surface was cooled by flowing air, purified in molten metal for 8 minutes, and the crystallized high-purity aluminum was pulled up and collected. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line and the secondary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 51, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 33%.
  • the average composition of the high-purity aluminum block obtained in the secondary line was Fe0.0015%, Si0.0022%, Ti0.0001%, V0.0003%, and B0.0015%.
  • Example 53 As shown in FIG. 14, the number of crucibles 13, 23, 33 on which the cooling bodies 130, 230, 330 are arranged is set to 10 for the primary line, 5 for the secondary line, and 3 for the tertiary line.
  • Aluminum was purified in a continuous 3 times purification system. The composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%. Boron was added to the stirring tanks 12, 22, and 32 arranged in the next stage of the melting furnaces 11, 21, and 31 in the primary line, the secondary line, and the tertiary line so that the concentration became 0.006%.
  • the purification conditions such as the number of rotations of the cooling body (material carbon), the cooling conditions, and the molten metal immersion time are the same as those in Example 51. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line, the secondary line, and the tertiary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 18%.
  • the average composition of the high-purity aluminum block obtained in the tertiary line was Fe0.0005%, Si0.0011%, Ti0.0001%, V0.0002%, and B0.0012%.
  • Example 54 As shown in FIG. 15, the number of crucibles 13, 23, 33 on which the cooling bodies 130, 230, 330 are arranged is set to 10 for the primary line, 5 for the secondary line, and 3 for the tertiary line.
  • Aluminum was purified in a continuous 3 times purification system.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%. Boron was added to the stirring tanks 12, 22, and 32 arranged in the next stage of the melting furnaces 11, 21, and 31 in the primary line, the secondary line, and the tertiary line so that the concentration became 0.006%.
  • separation tanks 16, 26, and 35 were installed between the stirring tanks 12, 22, and 32 and the crucibles 13, 23, and 33 added with B in each line.
  • the purification conditions such as the number of revolutions of the cooling body (material carbon), the cooling conditions, the molten metal immersion time, and the like are the same as in Example 51. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line, the secondary line, and the tertiary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 18%.
  • the average composition of the high-purity aluminum block obtained in the tertiary line was Fe0.0005%, Si0.0010%, Ti0.0001%, V0.0001%, and B0.0011%.
  • the number of crucibles 13, 23, 33, 43 on which the cooling bodies 130, 230, 330, 430 are arranged is 10 for the primary line, 5 for the secondary line, and 3 for the tertiary line.
  • Aluminum was purified by a continuous four-time purification system set to 2 pieces on the 4th and 4th lines.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%.
  • the concentration of boron is 0.005% in the stirring tanks 12, 22, 32, 42 arranged in the next stage of each melting furnace 11, 21, 31, 41 in the primary line, secondary line, tertiary line, and quaternary line. It added so that it might become.
  • the purification conditions such as the number of rotations of the cooling body (material carbon), the cooling conditions, and the molten metal immersion time are the same as those in Example 51. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line, the secondary line, the tertiary line, and the fourth line were performed under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 12%.
  • the average composition of the high-purity aluminum ingot obtained in the quaternary line was Fe0.0003%, Si0.0006%, Ti0.0001%, V0.0001%, and B0.0009%.
  • Comparative Example 56 Refining was performed under the same conditions as in Example 51 except that the crucibles 13 and 23 and the cooling bodies 130 and 230 having the same specifications as those in Comparative Example 1 according to the first embodiment were used.
  • the recovery rate at this time was 33%, and the average composition of the obtained high-purity aluminum ingot was Fe0.0022%, Si0.003%, Ti0.002%, and V0.005%.
  • Table 6 shows the composition of the aluminum base material subjected to the purification system and the aluminum lump after purification
  • Table 7 shows the purification conditions.
  • Example 57 As shown in FIG. 17, the aluminum is purified by a continuous double purification system in which the number of crucibles 13 and 23 in which the cooling bodies 130 and 230 are arranged is set to 10 for the primary line and 5 for the secondary line. did.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003% by weight.
  • the molten metal is returned from the last crucible 23 of the secondary line to the melting furnace 11 of the primary line through the molten metal returning device 27.
  • the rotational speed of the carbon cooling body was 400 rpm, the inner surface was cooled by flowing air, purified in molten metal for 8 minutes, and the crystallized high-purity aluminum was pulled up and collected. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line and the secondary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate total recovered weight of high-purity aluminum lump / original aluminum supply amount
  • the average composition of the high-purity aluminum block obtained in the secondary line was Fe0.0015%, Si0.0022%, Ti0.002%, and V0.005%.
  • Example 58 aluminum is purified by a continuous double purification system in which the number of crucibles 13 and 23 in which cooling bodies 130 and 230 are arranged is set to 10 for the primary line and 5 for the secondary line. did.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%. Boron was added to the stirring tanks 12 and 22 arranged in the next stage of the melting furnaces 11 and 21 in the primary line and the secondary line so that the concentration became 0.007%.
  • the molten metal is returned from the last crucible 23 of the secondary line to the melting furnace 11 of the primary line through the molten metal returning device 27.
  • the rotation speed of the cooling body was 400 rpm, the inner surface was cooled by flowing air, purified in molten metal for 8 minutes, and the crystallized high-purity aluminum was pulled up and collected. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line and the secondary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 75%.
  • the average composition of the high-purity aluminum block obtained in the secondary line was Fe0.0015%, Si0.0021%, Ti0.0001%, V0.0003%, and B0.0012%.
  • the number of crucibles 13, 23, and 33 in which the cooling bodies 130, 230, and 330 are arranged is set to 10 for the primary line, 5 for the secondary line, and 3 for the tertiary line.
  • Aluminum was purified in a continuous 3 times purification system.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001% and V 0.003% by weight. Boron was added to the stirring tanks 12, 22, and 32 arranged in the next stage of the melting furnaces 11, 21, and 31 in the primary line, the secondary line, and the tertiary line so that the concentration became 0.006%.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 75%.
  • the average composition of the high-purity aluminum block obtained in the tertiary line was Fe0.0005%, Si0.0011%, Ti0.0001%, V0.0002%, and B0.0010%.
  • Example 60 As shown in FIG. 20, the number of crucibles 13, 23, 33 on which the cooling bodies 130, 230, 330 are arranged is set to 10 for the primary line, 5 for the secondary line, and 3 for the tertiary line. Aluminum was purified in a continuous 3 times purification system. The composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%. Boron was added to the stirring tanks 12, 22, and 32 arranged in the next stage of the melting furnaces 11, 21, and 31 in the primary line, the secondary line, and the tertiary line so that the concentration became 0.006%.
  • separation tanks 16, 26, and 35 were installed between the stirring tanks 12, 22, and 32 and the crucibles 13, 23, and 33 added with B in each line.
  • the purification conditions such as the number of revolutions of the cooling body (material carbon), the cooling conditions, the molten metal immersion time, and the like are the same as in Example 51. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line, the secondary line, and the tertiary line were carried out under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 75%.
  • the average composition of the high-purity aluminum block obtained in the tertiary line was Fe0.0005%, Si0.001%, Ti0.0001%, V0.0001%, and B0.0010%.
  • Example 61 As shown in FIG. 21, the number of crucibles 13, 23, 33, 43 on which the cooling bodies 130, 230, 330, 430 are arranged is 10 for the primary line, 5 for the secondary line, and 3 for the tertiary line.
  • Aluminum was purified by a continuous four-time purification system set to 2 pieces on the 4th and 4th lines.
  • the composition contained in the original aluminum is Fe 0.04%, Si 0.02%, Ti 0.001%, and V 0.003%.
  • the concentration of boron is 0.005% in the stirring tanks 12, 22, 32, 42 arranged in the next stage of each melting furnace 11, 21, 31, 41 in the primary line, secondary line, tertiary line, and quaternary line. It added so that it might become.
  • the purification conditions such as the number of rotations of the cooling body (material carbon), the cooling conditions, and the molten metal immersion time are the same as those in Example 51. This operation was repeated for more than a day, and during the operation, the original aluminum was always melted and supplied, and consideration was given to always maintaining a constant level.
  • the primary line, the secondary line, the tertiary line, and the fourth line were performed under the same conditions.
  • each crucible is formed with a communication hole so that the value of A + a, which is the height of the molten metal surface, is the same as in Example 1, and the molten metal is fed from the upstream side beyond the liquid surface at that height. In such a case, the melt is discharged to the downstream side through the communication hole.
  • the recovery rate is 75%.
  • the average composition of the high-purity aluminum block obtained in the quaternary line was Fe0.0003%, Si0.0006%, Ti0.0001% or less, V0.0001%, and B0.0008%.
  • the crucibles 13 and 23 and the cooling bodies 130 and 230 having the same specifications as those of the example 21 according to the second embodiment are used under the same conditions as those of the examples 51 to 61 described above. When aluminum was purified, results equivalent to those of Examples 51 to 61 were obtained. Further, as the crucibles 13 and 23 and the cooling bodies 130 and 230, aluminum having the same specifications as those of the comparative example 21 according to the second embodiment was purified under the same conditions as in the example 51. However, the same result as in Comparative Example 56 was obtained.
  • the present invention relates to a material refining method for immersing a cooling body 2 in a molten material 6 to be purified contained in a molten metal holding container 1, and crystallizing crystals of the substance on the surface of the cooling body while rotating the cooling body 2. Available to the device.

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Abstract

La présente invention vise à proposer un procédé et un dispositif de purification de matière qui présentent un rendement de purification élevé, qui peuvent supprimer les éclaboussures de matière fondue, améliorer les coûts d'énergie et qui n'ont pas un degré élevé de difficulté de mécanisation. La présente invention concerne un procédé de purification de matériau dans lequel un corps de refroidissement 2 est plongé dans une matière fondue 6 à purifier, ladite matière fondue 6 étant contenue dans un récipient de rétention de métal fondu 1, et le corps de refroidissement 2 étant mis en rotation tandis que des cristaux de la matière sont cristallisés sur une surface du corps de refroidissement 2, où la distance la plus courte L1 dans la direction horizontale entre la surface périphérique interne du récipient de rétention de métal fondu 1 au niveau de la surface supérieure du métal fondu et la surface périphérique extérieure du corps de refroidissement 2 est d'au moins 150 mm, et la distance la plus courte L2 dans la direction horizontale entre la surface périphérique interne du récipient de rétention de métal fondu 1 et le bord le plus bas du corps de refroidissement 2 est d'au moins 100 mm dans la région entière où la matière fondue 6 est présente dans le récipient de rétention de métal fondu 1.
PCT/JP2017/019876 2016-06-02 2017-05-29 Procédé et dispositif de purification de matière, dispositif de chauffage et de retenue de métal fondu, et système de purification continue pour matière de pureté élevée Ceased WO2017209034A1 (fr)

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JP2016128018A JP6751604B2 (ja) 2016-06-28 2016-06-28 物質精製方法及び装置、高純度物質の連続精製システム
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JP2016226471A JP6762206B2 (ja) 2016-11-22 2016-11-22 溶湯加熱保持装置、物質精製装置及び物質精製方法

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