WO2022098119A1 - 마그네슘 용탕 정련용 플럭스 및 이를 이용한 마그네슘 용탕의 정련방법 - Google Patents

마그네슘 용탕 정련용 플럭스 및 이를 이용한 마그네슘 용탕의 정련방법 Download PDF

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Publication number
WO2022098119A1
WO2022098119A1 PCT/KR2021/015904 KR2021015904W WO2022098119A1 WO 2022098119 A1 WO2022098119 A1 WO 2022098119A1 KR 2021015904 W KR2021015904 W KR 2021015904W WO 2022098119 A1 WO2022098119 A1 WO 2022098119A1
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WIPO (PCT)
Prior art keywords
magnesium
refining
flux
molten metal
5caf
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PCT/KR2021/015904
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English (en)
French (fr)
Korean (ko)
Inventor
배준호
문병기
문영훈
김영민
김하식
서병찬
서종식
유봉선
이상은
임창동
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한국재료연구원
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Priority to CN202180064656.8A priority Critical patent/CN116209780A/zh
Publication of WO2022098119A1 publication Critical patent/WO2022098119A1/ko

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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
    • C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
    • 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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • 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 technical idea of the present invention relates to a magnesium smelting process, and more particularly, to a flux for refining molten magnesium and a method for refining molten magnesium using the same.
  • the conventional flux for refining molten magnesium has a higher density than that of molten magnesium or molten magnesium alloy.
  • this flux is injected into the upper surface of the molten metal, it is precipitated in the molten metal due to a density difference, while physically and chemically adsorbing and removing impurities in the molten metal.
  • the plus remains as sludge at the bottom of the molten metal.
  • a technical problem to be achieved by the technical idea of the present invention is a flux for refining molten magnesium that has a low density compared to that of molten magnesium, and thus removes impurities while floating from the bottom to the top of the molten magnesium, and a method for refining molten magnesium using the same is to provide
  • a flux for refining molten magnesium and a method for refining molten magnesium using the same.
  • the flux for refining magnesium molten metal includes at least two halogen compounds essentially including LiCl, and is 1.45 g/cm 3 to 1.63 g/cm at a temperature in the range of 650° C. to 750° C. It may have a density in the range of cm 3 .
  • the flux for refining the magnesium molten metal is 5 wt% to 20 wt% CaCl 2 ; 8 wt% to 27 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 10 wt% to 20 wt% CaCl 2 ; 8 wt% to 12 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 10 wt% CaCl 2 ; 23 wt % to 27 wt % KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 75LiCl-10CaCl 2 -10KCl-5CaF 2 , 70LiCl-15CaCl 2 -10KCl-5CaF 2 , 65LiCl-20CaCl 2 -10KCl-5CaF 2 , 65LiCl-5CaCl 2 -25KCl-5CaF 2 , 60LiCl-10CaCl 2 -25KCl-5CaF 2 , 60LiCl-30MgCl 2 -5KCl-5CaF 2 , and 60LiCl-30MgCl 2 -5NaCl-5CaF 2 .
  • the flux for refining the magnesium molten metal is 5 wt% to 30 wt% MgCl 2 ; 4 wt% to 6 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 30 wt% MgCl 2 ; 4 wt% to 6 wt% NaCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the method for refining the molten magnesium includes: providing the molten magnesium; adding flux for refining the molten magnesium to a lower portion of the molten magnesium; absorbing and removing impurities in the magnesium molten metal while the flux for refining the magnesium molten metal floats from a lower portion to an upper portion of the magnesium molten metal; and removing dross formed from the flux for refining the magnesium molten metal that has absorbed the impurities from the upper portion of the molten magnesium.
  • the flux for refining the magnesium molten metal may include two or more kinds of halogen compounds essentially including LiCl.
  • the flux for refining the magnesium molten metal may have a density in the range of 1.45 g/cm 3 to 1.63 g/cm 3 at a temperature in the range of 650° C. to 750° C.
  • the flux for refining the magnesium molten metal is 5 wt% to 20 wt% CaCl 2 ; 8 wt% to 27 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 10 wt% to 20 wt% CaCl 2 ; 8 wt% to 12 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 10 wt% CaCl 2 ; 23 wt % to 27 wt % KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 30 wt% MgCl 2 ; 4 wt% to 6 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 30 wt% MgCl 2 ; 4 wt% to 6 wt% NaCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 75LiCl-10CaCl 2 -10KCl-5CaF 2 , 70LiCl-15CaCl 2 -10KCl-5CaF 2 , 65LiCl-20CaCl 2 -10KCl-5CaF 2 , 65LiCl-5CaCl 2 -25KCl-5CaF 2 , 60LiCl-10CaCl 2 -25KCl-5CaF 2 , 60LiCl-30MgCl 2 -5KCl-5CaF 2 , and 60LiCl-30MgCl 2 -5NaCl-5CaF 2 .
  • the flux for refining the molten magnesium has a lower density than that of the molten magnesium, and thus impurities can be removed while floating from the bottom to the top of the molten magnesium. Accordingly, since the flux absorbs impurities to form dross on the upper portion of the molten metal, continuous removal of the dross is easy, and thus magnesium casting can be continuously performed without stopping.
  • FIG. 1 is a flowchart illustrating a method for refining molten magnesium according to an embodiment of the present invention.
  • FIG. 2 is a schematic diagram illustrating the refining method of molten magnesium of FIG. 1 according to an embodiment of the present invention.
  • FIG. 1 is a flowchart illustrating a method (S100) for refining molten magnesium according to an embodiment of the present invention.
  • the method for refining molten magnesium includes providing molten magnesium ( S110 ); injecting flux for refining the molten magnesium into the lower portion of the molten magnesium (S120); absorbing and removing impurities in the magnesium molten metal while the flux for refining the magnesium molten metal floats from the lower part to the upper part (S130); and removing the dross formed by the flux for refining the magnesium molten metal having absorbed the impurities from the upper portion of the magnesium molten metal (S140).
  • FIG. 2 is a schematic diagram illustrating the refining method of molten magnesium of FIG. 1 according to an embodiment of the present invention.
  • the magnesium molten metal 120 is accommodated in the molten metal container 110 .
  • the molten metal receiver 110 may be maintained at a temperature at which the magnesium molten metal 120 maintains a liquid state.
  • the magnesium molten metal 120 may include pure magnesium or a magnesium alloy.
  • the magnesium molten metal 120 may be maintained as a liquid phase, for example, at a temperature in the range of 600°C to 900°C, for example, at a temperature in the range of 650°C to 750°C.
  • the flux for refining the magnesium molten metal is introduced into the lower portion of the molten magnesium 120 . Accordingly, the flux 140 for refining the molten magnesium is positioned under the molten magnesium 120 .
  • the flux droplet 150 for refining the magnesium molten metal may float from the lower part of the magnesium molten metal 120 to the upper part. Impurities in the magnesium molten metal 120 may be accommodated in the flux droplet 150 for refining the molten magnesium.
  • the dross 160 may be formed.
  • the refining of the magnesium molten metal 120 can be facilitated, and continuous refining is possible.
  • the flux for refining the molten magnesium must have a density smaller than that of the molten magnesium in order to float in the molten magnesium.
  • the density of the magnesium molten metal has a density greater than about 1.65 g/cm 3 . Accordingly, the flux for refining the magnesium molten metal may have a density of 1.65 g/cm 3 or less, for example, a density in the range of 1.45 g/cm 3 to 1.63 g/cm 3 .
  • the magnesium molten metal refining flux may include a halogen compound, for example, may include chloride and fluoride, for example, LiCl, MgCl 2 , CaCl 2 , KCl, NaCl, CaF 2 At least one of may include
  • the flux for refining the molten magnesium may have a liquid form at a temperature in the range of 650° C. to 750° C. at which the molten magnesium or the molten magnesium alloy is liquid.
  • LiCl When describing the lower limit of the density of the flux for refining the molten magnesium, LiCl may have the lowest density among components included in the flux for refining the molten magnesium.
  • the density of LiCl is 1.485 g/cm 3 at 650° C. and 1.44 g/cm 3 at 750° C. Accordingly, the flux for refining the magnesium molten metal may have a density of 1.45 g/cm 3 or more.
  • the density in the range of 650° C. to 750° C. of the AZ91 alloy which is a commercial magnesium alloy, may be in the range of 1.638 g/cm 3 to 1.611 g/cm 3 .
  • the liquidus of the AZ91 alloy is about 600°C, but in an actual casting process, it has a temperature of about 650°C or higher. Accordingly, the flux for refining the magnesium molten metal may have a density of 1.63 g/cm 3 or less.
  • the chloride has a low surface tension in the liquid phase, so that it harmonizes well with the impurities, surrounds the impurities, and floats them to separate them. However, since the chloride has strong hygroscopicity, caution is required. In addition, since chloride has a high melting point, it is formulated to melt at the operating temperature by combining various kinds of chlorides or fluorides.
  • the fluoride can rapidly melt the mixed chloride by exothermic reaction during decomposition, and serves to re-dissolve the magnesium particles collected in the dross to return it to the molten metal.
  • the LiCl may selectively react with impurities such as CaO to be removed from the magnesium molten metal, thereby reducing the density of the flux.
  • the MgCl 2 may selectively react with impurities such as MgO and CaO to be removed from the magnesium molten metal, and surface oxidation of the dissolved magnesium may be minimized by forming a thin layer on the surface of the molten metal.
  • the MgCl 2 may reduce the melting point by reacting eutectic with KCl.
  • the CaCl 2 performs a function similar to that of the MgCl 2 , and in particular, may replace MgCl 2 in a magnesium alloy molten metal including a rare earth metal. However, since the density of the flux for refining the magnesium molten metal is increased, the content may be limited.
  • the KCl may perform a dehydration action in the magnesium molten metal, and may reduce HCl and MgO-related compounds.
  • the NaCl may perform a dehydration action in the magnesium molten metal, and may undergo a process reaction with MgCl 2 to reduce the melting point.
  • the CaF 2 may increase surface wettability and may increase chemical reactivity with oxide impurities such as MgO. Increase the surface tension between the molten chloride flux and the magnesium molten metal. Since the viscosity and density of the flux for refining the magnesium molten metal are increased, the content may be limited.
  • the magnesium molten metal refining flux includes at least two halogen compounds essentially including LiCl, and has a density in the range of 1.45 g/cm 3 to 1.63 g/cm 3 at a temperature in the range of 650° C. to 750° C. .
  • the flux for refining the magnesium molten metal is 5 wt% to 20 wt% CaCl 2 ; 8 wt% to 27 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the density of the flux for refining the molten magnesium may range from 1.507 g/cm 3 to 1.552 /cm 3 .
  • the density of the flux for refining the magnesium molten metal may be 1.552 g/cm 3 .
  • the density of the flux for refining the magnesium molten metal may be 1.507 g/cm 3 .
  • the 83LiCl-5CaCl 2 -8KCl-4CaF 2 means 83 wt% of LiCl, 5 wt% of CaCl 2 , 8 wt% of KCl, and 4 wt% of CaF 2 .
  • the flux for refining the magnesium molten metal is 10 wt% to 20 wt% CaCl 2 ; 8 wt% to 12 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 10 wt% CaCl 2 ; 23 wt % to 27 wt % KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the density of the flux for refining the molten magnesium may be in the range of 1.522 g/cm 3 to 1.569 /cm 3 .
  • the density of the flux for refining the magnesium molten metal may be 1.569 g/cm 3 .
  • the density of the flux for refining the magnesium molten metal may be 1.522 g/cm 3 .
  • the 68LiCl-5CaCl 2 -23KCl-4CaF 2 refers to 68 wt% of LiCl, 5 wt% of CaCl 2 , 23 wt% of KCl, and 4 wt% of CaF 2 .
  • the flux for refining the magnesium molten metal is 75LiCl-10CaCl 2 -10KCl-5CaF 2 , 70LiCl-15CaCl 2 -10KCl-5CaF 2 , 65LiCl-20CaCl 2 -10KCl-5CaF 2 , 65LiCl-5CaCl 2 -25KCl-5CaF 2 , 60LiCl-10CaCl 2 -25KCl-5CaF 2 , 60LiCl-30MgCl 2 -5KCl-5CaF 2 , and 60LiCl-30MgCl 2 -5NaCl-5CaF 2 .
  • the 75LiCl-10CaCl 2 -10KCl-5CaF 2 refers to 75 wt% of LiCl, 10 wt% of CaCl 2 , 10 wt% of KCl, and 5 wt% of CaF 2 .
  • the 70LiCl-15CaCl 2 -10KCl-5CaF 2 means 70 wt% of LiCl, 15 wt% of CaCl 2 , 10 wt% of KCl, and 5 wt% of CaF 2 .
  • the 65LiCl-20CaCl 2 -10KCl-5CaF 2 means 65 wt% of LiCl, 20 wt% of CaCl 2 , 10 wt% of KCl, and 5 wt% of CaF 2 .
  • the 65LiCl-5CaCl 2 -25KCl-5CaF 2 refers to 65 wt% of LiCl, 5 wt% of CaCl 2 , 25 wt% of KCl, and 5 wt% of CaF 2 .
  • the 60LiCl-10CaCl 2 -25KCl-5CaF 2 means 60 wt% of LiCl, 10 wt% of CaCl 2 , 25 wt% of KCl, and 5 wt% of CaF 2 .
  • the flux for refining the magnesium molten metal may include MgCl 2 instead of 10CaCl 2 .
  • the flux for refining the magnesium molten metal is 5 wt% to 30 wt% MgCl 2 ; 4 wt% to 6 wt% KCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • the flux for refining the magnesium molten metal is 5 wt% to 30 wt% MgCl 2 ; 4 wt% to 6 wt% NaCl; 4% to 6% by weight CaF 2 ; and the balance may include LiCl.
  • Table 1 is a table showing components and compositions of fluxes for refining molten magnesium in Comparative Examples and Examples used in the process of performing the refining process of molten magnesium.
  • % means the weight % with respect to the total weight of the flux.
  • Comparative Example 1 is a case in which the flux for refining molten magnesium is not used
  • Comparative Example 2 is a case in which a flux for refining a sedimentation type magnesium molten metal having a higher density than that of the molten magnesium is used.
  • Examples are LiCl, CaCl 2 , MgCl 2 , KCl, NaCl, and CaF 2 A case in which a flux for refining a floating magnesium molten metal is used.
  • Table 2 is a table showing the content of impurities in magnesium billets prepared by refining molten magnesium using the flux for refining molten magnesium in Comparative Examples and Examples.
  • the magnesium billet was formed by removing the dross floating on the top of the magnesium molten metal. However, the sludge settled at the bottom of the magnesium molten metal was not removed.
  • Comparative Examples 1 and 2 showed a higher impurity content in the lower part of the billet than in Examples.
  • Examples 1 to 3 is a case in which CaCl 2 is included.
  • Example 1 showed a relatively high impurity content, and Example 2 showed the lowest impurity content.
  • Example 1 is the case with the lowest density, and it is analyzed that the time is insufficient to collect impurities in the magnesium molten metal because the flux rises rapidly.
  • Example 3 is a case in which the density is almost similar to that of the molten magnesium, and the content of impurities in the upper part of the billet is small, but the content of impurities in the lower part is high. It is analyzed that the flotation of the flux is limited by the small density difference, and thus the efficiency of flotation and removal of impurities is reduced. Since Example 2 shows a very low impurity content at the top and bottom of the billet, the density of the flux of Example 2 is analyzed most effectively.
  • Examples 4 and 5 are cases in which MgCl 2 included as a main component of a commercial flux for purification is included.
  • a lower impurity content was observed compared to the comparative examples.
  • MgCl 2 which has a high solubility of MgO, continuously collects MgO, which is always generated from the top, increases its density and enters the molten metal again, so the impurity content seems to have increased. It is expected that the purification efficiency will increase.

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  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
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  • Mechanical Engineering (AREA)
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  • Manufacture And Refinement Of Metals (AREA)
  • Treatment Of Steel In Its Molten State (AREA)
PCT/KR2021/015904 2020-11-04 2021-11-04 마그네슘 용탕 정련용 플럭스 및 이를 이용한 마그네슘 용탕의 정련방법 WO2022098119A1 (ko)

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CN202180064656.8A CN116209780A (zh) 2020-11-04 2021-11-04 镁熔液精炼用熔剂及利用该熔剂的镁熔液的精炼方法

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KR1020200146376A KR102444651B1 (ko) 2020-11-04 2020-11-04 마그네슘 용탕 정련용 플럭스 및 이를 이용한 마그네슘 용탕의 정련방법

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4559084A (en) * 1981-05-26 1985-12-17 The Dow Chemical Company Salt-coated magnesium granules
JP2000226622A (ja) * 1999-02-08 2000-08-15 Mitsui Mining & Smelting Co Ltd マグネシウム系廃材の清浄化方法
JP2004027287A (ja) * 2002-06-25 2004-01-29 Honda Motor Co Ltd マグネシウム合金のリサイクル方法
KR100760581B1 (ko) * 2006-06-30 2007-09-20 주식회사 포스코 마그네슘 합금 정련용 용융염
JP2013221209A (ja) * 2012-04-19 2013-10-28 Kansai Univ マグネシウムまたはマグネシウム合金の精製方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4559084A (en) * 1981-05-26 1985-12-17 The Dow Chemical Company Salt-coated magnesium granules
JP2000226622A (ja) * 1999-02-08 2000-08-15 Mitsui Mining & Smelting Co Ltd マグネシウム系廃材の清浄化方法
JP2004027287A (ja) * 2002-06-25 2004-01-29 Honda Motor Co Ltd マグネシウム合金のリサイクル方法
KR100760581B1 (ko) * 2006-06-30 2007-09-20 주식회사 포스코 마그네슘 합금 정련용 용융염
JP2013221209A (ja) * 2012-04-19 2013-10-28 Kansai Univ マグネシウムまたはマグネシウム合金の精製方法

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KR20220060411A (ko) 2022-05-11
CN116209780A (zh) 2023-06-02

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