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EP2446065B2 - Utilisation d'un flux salin binaire de nacl et de mgcl2 pour la purification d'aluminium ou d'alliages d'aluminium et procédé correspondant - Google Patents

Utilisation d'un flux salin binaire de nacl et de mgcl2 pour la purification d'aluminium ou d'alliages d'aluminium et procédé correspondant Download PDF

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Publication number
EP2446065B2
EP2446065B2 EP10785623.9A EP10785623A EP2446065B2 EP 2446065 B2 EP2446065 B2 EP 2446065B2 EP 10785623 A EP10785623 A EP 10785623A EP 2446065 B2 EP2446065 B2 EP 2446065B2
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EP
European Patent Office
Prior art keywords
nacl
aluminum
mgcl
metal
salt
Prior art date
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EP10785623.9A
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German (de)
English (en)
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EP2446065A1 (fr
EP2446065B1 (fr
EP2446065A4 (fr
Inventor
Sylvain Tremblay
Luc Desrosiers
Daniel Levesque
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Pyrotek Inc
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Pyrotek Inc
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Publication of EP2446065A1 publication Critical patent/EP2446065A1/fr
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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
    • C22B21/00—Obtaining aluminium
    • C22B21/06—Obtaining aluminium refining
    • 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
    • C22B21/062—Obtaining aluminium refining using salt or fluxing agents

Definitions

  • the invention relates to the use of a binary salt flux comprising NaCl and MgCl 2 for the purification of a metal selected from the group consisting of aluminum alloys, for the removal of alkali and alkaline-earth metals.
  • the invention also relates to a method for the purification of said metal with said binary salt flux.
  • Fluxes can be used to form a protecting layer at the surface of an alloy to prevent oxidation.
  • fluxes contain chemical active agents, they can be used to clean furnace walls by softening accumulated layers of corundum. Some exothermic fluxes are also used for cleaning dross and removing aluminum trapped in oxide layers.
  • Fluxes that are based on alkali chlorides and alkaline-earth chlorides are also used for the refining of alloys. Those skilled in the art generally define refining as the removal of alkali and alkaline-earth metals, non metallic inclusions and hydrogen from the alloys.
  • Sodium and calcium are always present as impurities in aluminum obtained from the Hall-Heroult process. Lithium fluoride is often added to the electrolytic bath to improve the efficiency of cells. However, a small amount in the metallic state is found dissolved in the aluminum. These impurities entail quality issues. For example, in an alloy containing magnesium, the presence of sodium may interfere during the hot rolling processes. The presence of sodium in aluminum and silicon alloys neutralize the effect of phosphorus used for the refining of grains. For the above-mentioned reasons, the use of fluxes containing sodium is not recommended for aluminum and its alloys, more particularly for aluminum alloys comprising a magnesium content higher than 3 % by weight or a silicon content higher than 10 % by weight.
  • the presence of hydrogen in too high concentration may lead to a too high porosity of the aluminum during its solidification.
  • the presence of non metallic inclusions is important.
  • MgCl 2 is one of the chemical active agents used for the withdrawal of impurities in alloys. Its concentration has a direct effect on the kinetic of withdrawal of calcium and sodium. Its melting point is 714°C, but in common fluxes, it is mixed with other salts to obtain a melting point between 400 and 550°C. However, MgCl 2 is hygroscopic and can not be exposed for a long period of time to the surrounding air. Fluxes obtained by fusion of salts comprising magnesium chloride have hygroscopic properties. Consequently, the packaging is an important factor in limiting the absorption of humidity during the manufacturing of such fluxes.
  • US patent no. 1,377,374 relates to the use of a flux having an equimolar composition of sodium chloride and magnesium chloride for the production of manganese or magnesium alloys.
  • US patent no. 1,754,788 relates to the use of this same flux in a process for the cleaning of magnesium.
  • US patent no. 1,519,128 relates to the addition of calcium chloride to this composition and
  • US patent no. 2,262,105 relates to the addition of potassium chloride and magnesium oxide in addition to the calcium chloride.
  • US patent no. 5,405,427 mentions a flux based on sodium chloride, magnesium chloride, potassium chloride and carbon for the treatment of metal.
  • the refining fluxes are usually composed of alkali chlorides or alkaline-earth chlorides, which are mixed to obtain melting points that are lower than the operating temperature of alloys -- the melting point of pure compounds being usually quite high.
  • US patent no. 4,099,965 relates to a method where a flux of KCI and MgCl 2 is added in solid form in the bottom of a preheated container before the addition of aluminum. More currently, fluxes are added by an inert gas in a pipe under the surface of the metal (lance fluxing). Recently, a method was developed where a hollow shaft brings the salt flux in the alloy with a gas carrier, and the salt flux is dispersed by an agitator (rotary flux injection). This method reduces the amount of salt flux required for carrying out the purification while increasing the dispersion of this salt flux in the alloy. Following the addition of a salt flux to the metal, impurities and salts float on the surface of the liquid metal and can be easily removed.
  • solid compounds obtained by melting of salts controls the granulometry.
  • Particles may be used in batch processes or in continuous processes.
  • salt fluxes such as binary mixtures of magnesium chloride and potassium chloride
  • costs related to salt fluxes are high.
  • the use of salt fluxes having a substantial content in sodium chloride is not recommended by those skilled in the art due to perceived negative effects of sodium content in the resulting aluminum or aluminum alloys.
  • sodium chloride when sodium chloride is present in fluxes for the purification of aluminum or aluminum alloys, those skilled in the art currently will avoid or limit the use of sodium chloride. More particularly, in the case of certain kinds of alloys such as, for example, aluminum alloys having silicon content higher than 10% by weight and more particularly aluminum alloys having magnesium content higher than 3% by weight, those skilled in the art currently recommend not using sodium chloride in salt flux.
  • salt flux for the purification of a metal selected from the group consisting of aluminum alloys, said metal being in a liquid phase, wherein the salt flux is in the form of particles obtained by grinding a fused salt of NaCl and MgCl 2 , said binary mixture comprising from 40 to 50 % by weight of NaCl and from 50 to 60 % by weight of MgCl 2 .
  • the invention relates to a method according to claim 1.
  • the invention pertains to a method as defined hereinabove, wherein the salt flux: consists of particles resulting from the grinding of a fused salt of NaCl and MgCl 2 in solid state.
  • the invention relates to a method as defined in any one of the above-mentioned embodiments, wherein the binary mixture comprises: a) from 40 to 50% by weight of NaCl; and b) from 50 to 60% by weight of MgCl 2 . More particularly, this binary mixture comprises 45% by weight of NaCl and 55% by weight of MgCl 2 to form an eutectic mixture having a melting point of about 439°C.
  • the binary mixture may comprise:
  • Another embodiment of the invention relates to a method as defined in any one of the above-mentioned embodiments, wherein when the salt flux is in the form of particles, those particles have an average particle size between 100 ⁇ m and 3.35 mm.
  • said particles may have a particle size between 0.85 mm and 3.15 mm or between 100 ⁇ m and 1 mm. The present text describes such a use.
  • Another embodiment of the invention relates to a method as defined in any one of the above-mentioned embodiments, wherein the particles are contacted with the liquid metal by injection with a gas injection equipment.
  • a gas injection equipment may consist of a rotary injector known under the tradename SNIF PHD-50 commercialized by the Applicant. The present text discloses such a use.
  • Another embodiment of the invention relates to a method as defined in any one of the above-mentioned embodiments, wherein the metal is an aluminum alloy having a magnesium content higher than 3% by weight.
  • the present text describes such a use.
  • Another embodiment of the invention relates to a method as defined in any one of the above-mentioned embodiments, wherein the metal is an aluminum alloy having a silicon content higher than 10% by weight.
  • the present text discloses such a use.
  • Formulations based on NaCl and MgCl 2 proposed according to the present invention show melting points that are lower than those of salt flux compositions sold by the Applicant under the trademark Promag (40 wt % KCI, 60 wt % MgCl 2 ), for equivalent amounts of MgCl 2 which is the chemically active agent for the withdrawal of impurities.
  • the lowering of melting points represents a lowering of energy costs when melting the solid salt flux.
  • example 1 illustrates an unexpected effect with regard to the sodium concentration in an aluminum alloy when NaCl is added in a liquid aluminum alloy, that is, no increase of the sodium content in the alloy obtained.
  • each salt flux was made by mixing the salts in an anhydrous solid phase in an appropriate oven. Then, by increasing the temperature of the oven, a fused compound in liquid form was obtained. The liquid was then cooled down quickly, grinded and sifted to obtain a granulometry that was appropriate for the selected method.
  • the salt flux was made only by mixing the salts in an anhydrous solid phase.
  • Salt fluxes have shown an optimal efficiency for the withdrawal of Ca, Na and Li when used with a rotary injector such as a SNIF PHD-50 (tradename) commercialized by the Applicant (Pyrotek).
  • a rotary injector such as a SNIF PHD-50 (tradename) commercialized by the Applicant (Pyrotek).
  • concentrations of salt fluxes required to carry out the purification may vary depending on the selected method.
  • a salt flux consisting of a binary mixture of 45 wt % NaCl and 55 wt % MgCl 2 were agitated in 1.5 kg of a liquid AA1100 aluminum alloy (sold under the trademark Alcan) in which 5 wt % of magnesium were added.
  • the crucible was maintained at 720°C during 90 minutes and samples were taken every 30 minutes.
  • the sodium level in the crucible was maintained at a minimal level of 3 ppm during the whole experiment, showing that an addition of a flux comprising NaCl does not involve an absorption of sodium in an aluminum alloy with high magnesium content.
  • the salt flux was prepared from NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL and MgCl 2 in flake form and sold under the trademark SKYLINE.
  • a salt flux consisting of a ternary mixture of 20 wt % NaCl, 20 wt % KCI and 60 wt % MgCl 2 were agitated and added in 1.5 kg of a liquid AA1100 aluminum alloy (sold under the trademark Alcan) in which 5 wt % of magnesium were added.
  • the crucible was maintained at 720°C during 90 minutes and samples were taken every 30 minutes.
  • the sodium level in the crucible was maintained at a minimal level of 3 ppm during the whole experiment, showing that an addition of a ternary flux comprising a small amount of NaCl does not involve an absorption of sodium in an aluminum alloy with high magnesium content.
  • the salt flux was prepared from NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL, KCI in powder form and sold under the trademark IMC KALIUM and MgCl 2 in flake form and sold under the trademark SKYLINE.
  • A356 alloy About seventy-five kilos (75kg) of A356 alloy were melted and maintained in a liquid state at 700°C in a crucible made of silicon carbide. Then, 535g of an aluminum alloy containing 10 % by weight of calcium were added to the liquid A356 alloy while mixing it with an agitator having straight blades. Then the resulting aluminum alloy contained in the crucible was left without agitation for 5 hours. During this time, the calcium content of the resulting aluminum alloy was reduced from 350 ppm to 150 ppm.
  • salt flux made of 45 wt % NaCl and 55 wt % MgCl 2 were added to the resulting alloy while agitating it in order to further purify it.
  • the salt flux was prepared from NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL and MgCl 2 in flake form and sold under the trademark SKYLINE.
  • Analyses made on the purified aluminum alloy have shown a reduction of the Ca content from 150 ppm to 70 ppm, that is a reduction of 53 %, immediately after the addition of the salt flux, and this Ca content drops to 25 ppm 3 hours after the addition. Also, analyses have shown that the sodium content was in the order of 2 ppm.
  • Fifty grams of a flux were prepared in a small alumina crucible by mixing 22.5 grams of NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL, and 27.5 grams of MgCl 2 in flake form and sold under the trademark SKYLINE. The mixture was subjected to a temperature of 550°C during 45 minutes. The liquid mixture obtained was then poured into an enamelled-coated bowl for quick solidification. The salt flux obtained was then grinded with in a mortar and sifted. The fraction having a particle size lower than 3150 microns and higher than 105 microns was recovered.
  • a salt flux Fifty grams of a salt flux were prepared in a small alumina crucible by mixing 10 grams of NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL, 10 grams of KCI in powder form and sold under the trademark IMC KALIUM, and 30 grams of MgCl 2 in flake form and sold under the trademark SKYLINE. The mixture was subjected to a temperature of 550°C during 45 minutes. The liquid mixture obtained was then poured into an enamelled-coated bowl for quick solidification. The salt flux obtained was then grinded in a mortar and sifted. The fraction having a particle size lower than 3150 microns and higher than 105 microns was recovered.
  • the analysis of samples shows a reduction of the Ca level from 108 ppm to 7 ppm after the addition of the salt flux. Thirty minutes later, the calcium level was at 2 ppm and after 60 minutes the calcium level was under 1 ppm. No increase in sodium content was noted during the test. The sodium level was in the order of 2 ppm. This example shows that a ternary flux having a low content in NaCl does not increase the level of sodium in the alloy.
  • Fifty grams of a salt flux were prepared only by mixing 22.5 grams of NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL with a granulometry 95% lower than 840 microns and 95 % higher than 300 microns, and 27.5 grams of MgCl 2 in flake form and sold under the trademark SKYLINE with a granulometry 90 % lower than 4.7 mm and 85 % higher to 1 mm.
  • PROMAG SI (trademark) formed of 40 wt % KCl and 60 wt % MgCl 2 , with a granulometry 99% lower than 3150 microns and 95 % higher than 850 microns, were added to the alloy doped with calcium while agitating for 2 minutes. The agitation was stopped and samples were later taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Claims (5)

  1. Procédé pour la purification d'un métal avec un flux salin binaire, le métal étant choisi dans le groupe constitué par des alliages d'aluminium, pour l'élimination de métaux alcalins et alcalino-terreux, ledit procédé comprenant :
    • le chauffage du métal en une phase liquide ; et
    la mise en contact du métal liquide avec le flux salin constitué d'un mélange binaire de NaCl et MgCl2,
    dans lequel ledit flux salin est constitué de particules résultant du broyage d'un sel fondu de NaCl et de MgCl2 à l'état solide, ledit mélange binaire comprenant de 40 à 50 % en poids de NaCl et de 50 à 60 % en poids de MgCl2.
  2. Procédé selon la revendication 1, dans lequel lesdites particules ont une taille moyenne de particule comprise entre 100 µm et 3,35 mm, en particulier entre 0,85 mm et 3,15 mm et plus particulièrement entre 100 µm et 1 mm.
  3. Procédé selon l'une quelconque des revendications 1 ou 2, dans lequel lesdites particules sont mises en contact avec le métal liquide par injection avec un appareillage d'injection de gaz.
  4. Procédé selon l'une quelconque des revendications 1 à 3, dans lequel le métal est un alliage d'aluminium ayant une teneur en magnésium supérieure à 3 % en poids.
  5. Procédé selon l'une quelconque des revendications 1 à 4, dans lequel le métal est un alliage d'aluminium ayant une teneur en silicium supérieure à 10 % en poids.
EP10785623.9A 2009-06-08 2010-06-08 Utilisation d'un flux salin binaire de nacl et de mgcl2 pour la purification d'aluminium ou d'alliages d'aluminium et procédé correspondant Active EP2446065B2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA2668473A CA2668473C (fr) 2009-06-08 2009-06-08 Utilisation d'un flux binaire de nacl et de mgcl2 pour la purification de l'aluminium ou des alliages d'aluminium, et methode d'utilisation de ce flux
PCT/CA2010/000866 WO2010142025A1 (fr) 2009-06-08 2010-06-08 Utilisation d'un flux salin binaire de nacl et de mgcl2 pour la purification d'aluminium ou d'alliages d'aluminium et procédé correspondant

Publications (4)

Publication Number Publication Date
EP2446065A1 EP2446065A1 (fr) 2012-05-02
EP2446065A4 EP2446065A4 (fr) 2017-03-15
EP2446065B1 EP2446065B1 (fr) 2020-12-16
EP2446065B2 true EP2446065B2 (fr) 2024-02-21

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Country Status (9)

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EP (1) EP2446065B2 (fr)
JP (1) JP2012529565A (fr)
CN (1) CN102459663A (fr)
AU (1) AU2010258042B2 (fr)
BR (1) BRPI1015440A2 (fr)
CA (1) CA2668473C (fr)
ES (1) ES2862528T5 (fr)
RU (1) RU2011147513A (fr)
WO (1) WO2010142025A1 (fr)

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2013013321A1 (fr) * 2011-07-28 2013-01-31 Pyrotek Inc. Utilisation d'un flux de sel tertiaire de nacl, kcl et mgcl2 pour la purification d'aluminium et d'alliages d'aluminium, et procédé correspondant
CN104831079B (zh) * 2015-05-13 2016-08-31 上海交通大学 偏析法精铝提纯中有效去除钒的方法
CN104862496A (zh) * 2015-05-13 2015-08-26 上海交通大学 用于偏析法精铝提纯的熔体复合处理剂及其制备方法
CN105177311A (zh) * 2015-09-15 2015-12-23 沈阳航空航天大学 一种用于铝熔体处理的含钠氯盐熔合物及其制造方法
CN105177335B (zh) * 2015-09-15 2017-03-22 沈阳航空航天大学 一种用于铝合金生产的合金元素添加剂及其制备方法
IT201700074924A1 (it) * 2017-07-04 2019-01-04 Foundry Ecocer S R L Flusso fondente per la scorifica del metallo fuso.
US10513753B1 (en) * 2019-01-03 2019-12-24 2498890 Ontario Inc. Systems, methods, and cored wires for treating a molten metal
WO2022031721A1 (fr) * 2020-08-05 2022-02-10 Pyrotek, Inc. Flux à constituants multiples
JP7713325B2 (ja) * 2021-07-13 2025-07-25 株式会社豊田中央研究所 Ｍｇ除去剤およびアルミニウム合金の製造方法
CN115198106B (zh) * 2022-07-08 2023-08-29 中国铝业股份有限公司 一种铝灰用提铝精炼剂及其制备方法和使用方法
CN117403069A (zh) * 2023-10-17 2024-01-16 郑州西盛铝业有限公司 一种铝及铝合金用精炼剂及其制备方法、使用方法

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WO2005049875A1 (fr) † 2003-11-19 2005-06-02 Corus Technology Bv Procede servant a refroidir du metal en fusion pendant la cristallisation fractionnaire

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WO2005049875A1 (fr) † 2003-11-19 2005-06-02 Corus Technology Bv Procede servant a refroidir du metal en fusion pendant la cristallisation fractionnaire

Also Published As

Publication number Publication date
EP2446065A1 (fr) 2012-05-02
AU2010258042A1 (en) 2011-12-22
WO2010142025A1 (fr) 2010-12-16
ES2862528T5 (es) 2024-09-18
CA2668473A1 (fr) 2010-12-08
CN102459663A (zh) 2012-05-16
CA2668473C (fr) 2014-08-19
ES2862528T3 (es) 2021-10-07
BRPI1015440A2 (pt) 2018-07-17
RU2011147513A (ru) 2013-07-20
JP2012529565A (ja) 2012-11-22
EP2446065B1 (fr) 2020-12-16
AU2010258042B2 (en) 2014-01-23
EP2446065A4 (fr) 2017-03-15

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