CA2747650A1 - Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof - Google Patents

Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof Download PDF

Info

Publication number
CA2747650A1
CA2747650A1 CA 2747650 CA2747650A CA2747650A1 CA 2747650 A1 CA2747650 A1 CA 2747650A1 CA 2747650 CA2747650 CA 2747650 CA 2747650 A CA2747650 A CA 2747650A CA 2747650 A1 CA2747650 A1 CA 2747650A1
Authority
CA
Canada
Prior art keywords
weight
nacl
particles
mgcl2
metal
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.)
Abandoned
Application number
CA 2747650
Other languages
French (fr)
Inventor
Sylvain Tremblay
Luc Desrosiers
Daniel Levesque
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.)
Pyrotek Inc
Original Assignee
Pyrotek Inc
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
Application filed by Pyrotek Inc filed Critical Pyrotek Inc
Priority to CA 2747650 priority Critical patent/CA2747650A1/en
Priority to PCT/CA2012/050507 priority patent/WO2013013321A1/en
Publication of CA2747650A1 publication Critical patent/CA2747650A1/en
Abandoned legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B21/00Obtaining aluminium
    • C22B21/06Obtaining aluminium refining
    • C22B21/062Obtaining aluminium refining using salt or fluxing agents

Landscapes

  • 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)

Abstract

A method and a use for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, wherein said metal is in a liquid phase and is contacted with a salt flux consisting of a selected tertiary mixture of NaCl, KCl, and MgCl2.

Description

USE OF A TERTIARY SALT FLUX OF NaCl, KCI, AND MgCI2 FOR THE
PURIFICATION OF ALUMINUM OR ALUMINUM ALLOYS, AND METHOD
THEREOF

Field of the invention [0001] The published US patent application No. US-2010-0307293 relates to the use of a binary salt flux comprising NaCl and MgCI2 for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, more particularly for the removal of alkali and alkaline-earth metals. This invention also relates to a method for the purification of said metal with said binary salt flux. Those NaCl/MgCI2 binary mixtures have shown unexpected economical advantages with respect to KCI/MgCI2 binary mixtures and few NaCl/KCI/MgCI2 tertiary mixtures that were also known, for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, more particularly for the removal of alkali and alkaline-earth metals.
[0002] Now the Applicant has discovered that some selected NaCI/KCI/MgCI2 tertiary mixtures, different from those already known, have shown unexpected technical and/or economical advantages for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, in view of existing NaCl/KCI/MgCI2 tertiary mixture and even in view of NaCI/MgCI2 binary mixtures.
[0003] Also, these selected tertiary mixtures according to the invention further show a low melting point.
[0004] The invention also relates to a method for the purification of said metal with said selected ternary salt flux.

Prior art [0005] The use of fluxes is well known in the field of metallurgy and these fluxes fulfill various functions.
[0006] Fluxes can be used to form a protecting layer at the surface of an alloy to prevent oxidation. When 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.
[0007] 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.
[0008] 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.
[0009] Also, the presence of hydrogen in too high concentration may lead to a too high porosity of the aluminum during its solidification. During the recycling of aluminum, the presence of non metallic inclusions is important.
[0010] Reactional kinetics for the withdrawal of calcium and sodium in an aluminum alloy have been well studied. Naturally, in these alloys, both impurities disappear according to a kinetic of order 1 for small concentrations and order 0 for high concentrations. Because of its high vapor tension, sodium oxidizes itself more rapidly than calcium, that is why calcium is used during cleaning tests. The addition of fluxes involves an increase of reactional constants and thereby a faster reduction of the content in impurities. Mixing also has a non negligible effect on the reduction of impurities. Mixing accelerates the withdrawal of impurities by increasing the contact between impurities and the salt flux.
[0011] MgCl2 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, MgCl2 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.
[0012] There are examples of fluxes that are based on magnesium chloride.
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.
[0013] The article entitled "Salt Fluxes for Alkali and Alkali and Alkaline Earth Element Removal from Molten Aluminum" by David H. DeYoung shows the use of a ternary salt based on magnesium chloride, sodium chloride and potassium chloride for the removal of sodium, calcium and lithium from aluminum alloys. However, the article entitled "The Treatment of Liquid Aluminum-Silicon Alloys" by Gruzleski et al., pp. 204-205 indicates that it is important to those skilled in the art, not to use fluxes containing sodium salts. Therefore, even if a ternary flux salts having low content in sodium salts may be tolerated, those skilled in the art are expressly invited to avoid using sodium salts.
[0014] Initially, the refining of aluminum was carried out by bubbling of chlorine and argon in the liquid metal. However, this created environmental problems due to emissions of chlorine, chlorhydric acid and particles in suspension. The use of salt fluxes was later adopted as a more ecologically-friendly solution.
[0015] 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.
[0016] Several methods can be used to incorporate salt fluxes in an alloy. US
patent no. 4,099,965 relates to a method where a flux of KCI and MgCl2 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.

5 [0017] Advantageously, the use of solid compounds obtained by melting of salts controls the granulometry. Particles may be used in batch processes or in continuous processes.

[0018] However, costs related to salt fluxes such as binary mixtures of magnesium chloride and potassium chloride, are high. Furthermore, 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. In fact, 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.

[0019] As already mentioned in co-pending published US patent application No. US-2010=0307293, during Applicant's search for a more effective solution to the purification problem, it was surprisingly noted that contrary to current apprehensions and beliefs of those skilled in the art, it is possible in a salt flux containing MgCl2, to replace expensive KCI by inexpensive NaCl. Such a substitution offers an economical solution for the treatment of aluminum or aluminum alloys with an efficiency of purification that is equivalent to methods presently used.
Indeed, contrary to apprehensions of those skilled in the art, there is no significant amount of sodium in the resulting aluminum or aluminum alloys when using the inventive purification method described herein.

[0020] Furthermore, during recent additional searches made by the Applicant, it was surprisingly noted that contrary to current apprehensions and beliefs of those skilled in the art, it is possible in a salt flux containing MgCI2, to replace only a portion of the expensive KCI by inexpensive NaCl, to form some selected tertiary salt fluxes of NaCl, KCI, and MgCi2, which contrary to existing NaCI/KCI/MgCI2 salt fluxes and even in view of NaCI/MgCI2 binary mixtures, show unexpected technical and/or economical advantages for the purification of a metal selected from the group consisting of aluminum and aluminum alloys. Also, these selected tertiary mixtures according to the invention further show a low melting point. Again, contrary to apprehensions of those skilled in the art, there is no significant amount of sodium in the resulting aluminum or aluminum alloys when using the inventive purification method described herein. Furthermore, these selected tertiary salt fluxes of NaCl, KCI, and MgCI2 also relates to a method for the purification of said metal with said selected ternary salt flux.

[0021] Embodiments of the selected tertiary salt fluxes of NaCl, KCI, and MgCI2 making the object of the present invention, show the following advantages:

- Economical advantages o Lower production costs because the melting point of the flux is lower.
o Lower costs of raw material.

- Efficiency equivalent to the purification methods using an existing well known salt flux sold under the trademark Promag (40 wt % KCI - 60 wt % MgCl2).

Economical alternative to existing product sold under the trademark Promag without creating any significant accumulation of sodium within aluminum or aluminum alloys.

[0022] A first preferred aspect of the published US patent application No. US-2010-0307293 is related to the use of a salt flux for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, said metal being in liquid phase and said salt flux being a binary mixture of NaCl and MgCI2.
[0023] A second preferred aspect of the published US patent application No.
US-2010-0307293 is related to a method for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, wherein said method comprises:

= heating the metal to a liquid phase; and = contacting the liquid metal with a salt flux consisting of a binary mixture of NaCl and MgCI2.

[0024] Another embodiment of the published US patent application No. US-2010-0307293 is related to a use or a method as defined hereinabove, wherein more than 22 % by weight of said binary mixture consists of NaCl.

[0025] Another embodiment of the published US patent application No. US-2010-0307293 is related to a use or a method as defined hereinabove, wherein the salt flux:

= is a binary mixture of particles of NaCl and particles of MgCI2; or = consists of particles resulting from the grinding of a fused salt of NaCl and MgCl2 in solid state; or = is a liquid mixture of NaCl and MgCl2.

[0026] Another embodiment of the published the US patent application No.
US-2010-0307293 is related to a use or 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 MgCl2. More particularly, this binary mixture comprises 45% by weight of NaCl and 55% by weight of MgCl2 to form an eutectic mixture having a melting point of about 439 C.

[0027] Another embodiment of the invention of the published US patent application No. US-2010-0307293 is related to a use or 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 pm and 3.35 mm. Preferably, said particles may have a particle size between 0.85 mm and 3.15 mm or between 100 pm and 1 mm.

[0028] Another embodiment of the published US patent application No. US-2010-0307293 is related to a use or 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 non limiting example of a gas injection equipment may consist of a rotary injector known under the tradename SNIF PHD-50 commercialized by the Applicant.

[0029] Another embodiment of the published US patent application No. US-2010-0307293 is related to a use or 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.

[0030] Another embodiment of the published US patent application No. US-2010-0307293 is related to a use or 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.

[0031] An embodiment of the present invention relates to a method for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, wherein said method comprises:

= heating the metal to a liquid phase; and = contacting the liquid metal with a salt flux consisting of a tertiary mixture of NaCl, KCI, and MgC12, said salt flux being selected in the group consisting of:

= salt fluxes in the form of a tertiary mixture of particles and comprising more than 22 % by weight of NaCl;

= salt fluxes in the form of particles obtained by grinding a fused salt of NaCI, KCI and MgCl2 and having the following formulations:

o 5-18 % by weight of NaCl, o 17-60 % by weight of KCI, o 35-65 % by weight of MgCl2 ;

= salt fluxes in the form of particles obtained by grinding a fused salt of NaCI, KCI and MgCl2 and having the following formulations:

o 22-55 % by weight of NaCl, o 13-43 % by weight of KCI, o 35-65 % by weight of MgCI2 ; and = salt fluxes in the form of a liquid tertiary mixture.

[0032] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is a ternary mixture of particles of NaCl, 5 KCI, and MgCI2, wherein more than 22 % by weight of said tertiary mixture consists of NaCl.

[0033] Another embodiment of the present invention relates to a method as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCI2, comprises:

10 a) from more than 22 to 30 % by weight of NaCl, b) from 5 to 43 % by weight of KCI, and c) from 35 to 65 % by weight of MgCI2.

[0034] Another embodiment of the present invention relates to a method as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCI2, comprises:

a) 25 % by weight of NaCl, b) 15_% by weight of KCI, and c) 60 % by weight of particles of MgCI2;

said tertiary mixture having a melting point of about 417 C.

[0035] Another embodiment of the present invention relates to a method as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCI2, have an average particle size comprised between 100 1m and 3.35mm, or comprised between 0.85 mm and 3.15 mm, or comprised between 100 pm and 1 mm.

[0036] Another embodiment of the present invention relates to a method as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCI2, are contacted with the liquid metal by injection with a gas injection equipment.
[0037] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCl2, having the following formulations:

o 5-18 % by weight of NaCl, o 17-60 % by weight of KCI, o 35-65 % by weight of MgCl2.

[0038] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCI, KCI and MgCl2, having the following formulations:

o 22-55 % by weight of NaCl, o 13-43 % by weight of KCI, and o 35-65 % by weight of MgCI2.

[0039] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCI2, having the following formulations:

o 25 % by weight of NaCl, o 15 % by weight of KCI, and o 60 % by weight Of M902;

said tertiary mixture having a melting point of about 417 C.

[0040] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCI2, have an average , particle size comprised between 100 m and 3.35mm, or comprised between 0.85 mm and 3.15 mm, or comprised between 100 m and 1 mm.

[0041] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCI2, are contacted with the liquid metal by injection with a gas injection equipment.

[0042] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is a liquid tertiary mixture of NaCl, KCI, and M902-[0043] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCi, KCI, and MgCI2 comprising:

= from 10 to 35 % by weight of NaCl, = from 5 to 45 % by weight of KCI, and = from 40 to 65 % by weight of MgCl2.

[0044] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCl2 comprising more than 22 % by weight of said liquid tertiary mixture consists of NaCl.

[0045] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCl2 comprising = from more than 22 to 35 % by weight of NaCl, = from 5 to 38 % by weight of KCI, and = from 40 to 65 % by weight of MgC12.

[0046] Another embodiment of the present invention relates to a method as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCI2 comprising:

= 25 % by weight of NaCl, = 15 % by weight of KCI, and = 60 % by weight of MgCl2.

[0047] Another embodiment of the present invention relates to a method as defined hereinabove, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.

[0048] Another embodiment of the present invention relates to a method as defined hereinabove, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.

[0049] An embodiment of the present invention relates to a use for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, wherein said use comprises:

= heating the metal to a liquid phase; and = contacting the liquid metal with a salt flux consisting of a tertiary mixture of NaCl, KCI, and MgCi2, said salt flux being selected in the group consisting of:

= salt fluxes in the form of a tertiary mixture of particles and comprising more than 22 % by weight of NaCl, = salt fluxes in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCi2 and having the following formulations:

o 5-18 % by weight of NaCl, o 17-60 % by weight of KCI, o 35-65 % by weight Of M902;

= salt fluxes in the form of particles obtained by grinding a fused salt of NaCl, KCI and Mg02 and having the following formulations:

o 22-55 % by weight of NaCl, o 13-43 % by weight of KCI, o 35-65 % by weight of MgCI2 ; and = salt fluxes in the form of a liquid tertiary mixture.

[0050] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is a ternary mixture of particles of NaCl, KCI, and MgCl2, wherein more than 22 % by weight of said tertiary mixture consists of NaCl.

5 [0051] Another embodiment of the present invention relates to a use as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCl2, comprises:

a) from more than 22 to 30 % by weight of NaCl, b) from 5 to 43 % by weight of KCI, and 10 c) from 35 to 65 % by weight of MgC12.

[0052] Another embodiment of the present invention relates to a use as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCl2, comprises:

a) 25 % by weight of NaCl, 15 b) 15 % by weight of KCI, and c) 60 % by weight of particles of MgCl2;

said tertiary mixture having a melting point of about 417 C.

[0053] Another embodiment of the present invention relates to a use as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCI2, have an average particle size comprised between 100 m and 3.35mm, or comprised between 0.85 mm and 3.15 mm, or comprised between 100 m and 1 mm.

1w [0054] Another embodiment of the present invention relates to a use as defined hereinabove, wherein the ternary mixture of particles of NaCl, KCI, and MgCl2, are contacted with the liquid metal by injection with a gas injection equipment.
[0055] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCI2, having the following formulations:

o 5-18 % by weight of NaCl, o 17-60 % by weight of KCI, o 35-65 % by weight of MgCI2.

[0056] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCI2, having the following formulations:

o 22-55 % by weight of NaCl, o 13-43 % by weight of KCI, and o 35-65 % by weight of MgCI2.

[0057] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCI2, having the following formulations:

o 25 % by weight of NaCl, o 15 % by weight of KCI, and o 60 % by weight of MgCI2;
said tertiary mixture having a melting point of about 417 C.

[0058] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCl2, have an average particle size comprised between 100 m and 3.35mm, or comprised between 0.85 mm and 3.15 mm, or comprised between 100 pm and 1 mm.

[0059] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCI and MgCl2, are contacted with the liquid metal by injection with a gas injection equipment.

[0060] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is a liquid tertiary mixture of NaCl, KCI, and MgCl2.

[0061] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCl2 comprising:

= from 10to35%byweightofNaCl, = from 5 to 45 % by weight of KCI, and = from 40 to 65 % by weight of MgCl2.

[0062] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCl2 comprising more than 22 % by weight of said liquid tertiary mixture consists of NaCl.
[0063] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCl2 comprising = from more than 22 to 35 % by weight of NaCI, = from 5 to 38 % by weight of KCI, and = from 40 to 65 % by weight of MgCl2.

[0064] Another embodiment of the present invention relates to a use as defined hereinabove, wherein said salt flux is in the form of a liquid tertiary mixture of NaCl, KCI, and MgCl2 comprising:

= 25 % by weight of NaCl, = 15 % by weight of KCI, and = 60 % by weight of MgCl2.

[0065] Another embodiment of the present invention relates to a use as defined hereinabove, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.

[0066] Another embodiment of the present invention relates to a used as defined hereinabove, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.

[0067] The present invention will be better understood with reference to the following drawings:

= Figure 1: a phase diagram of a fused salt KCI/NaCI/MgCl2;
= Figure 2: a phase diagram of a fused salt KCI/MgCI2;
= Figure 3: a phase diagram of a fused salt NaCI/MgCI2;

= Figure 4: a comparative graphic concerning examples 5 to 8; and = Figure 5: a comparative graphic concerning examples 9 to 12.

Phase diagrams of Figures 1 to 3 were extracted from factsage web site (http://factsage.com).

DESCRIPTION OF EMBODIMENTS OF THE INVENTION

[0068] As already mentioned in the published US patent application No. US-2010-0307293, especially in examples 1 to 8, which are reproduced hereinafter, the Applicant has noted, contrary to apprehensions of those skilled in the art, that formulations of salt fluxes comprising a binary mixture of NaCl and MgC12 do not involve an increase of the concentration of metallic sodium in an aluminum alloy having magnesium content. A non limiting example of such an aluminum alloy may consist of an aluminum alloy having a magnesium content of 5 % by weight.
Consequently, it appears that there is no counter-indication of using a binary salt flux comprising NaCl and MgCI2 for cleaning aluminum, especially in the case of an aluminum alloy with high magnesium content.

[0069] In the published US patent application No. US-2010-0307293, formulations which were based on NaCl and MgCI2, 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 % MgCI2), for equivalent amounts of MgCl2 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.

[0070] Furthermore, in said published US patent application No. US-2010-0307293, two fused salts were considered, that is (on a weight basis) the following binary system salt flux and ternary system salt flux:

= 45 % NaCl and 55 % MgCl2 with a melting point of 439 C; and 5 = 20 % NaCl, 20 % KCI and 60% MgCI2 with a melting point of 396 C.

[0071] Also, in said published US patent application No. US-2010-0307293, 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. Said example 1 is reproduced 10 hereinafter.

[0072] As mentioned in said published US patent application No. US-2010-0307293, preparation of 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 15 quickly, grinded and sifted to obtain a granulometry that was appropriate for the selected method. In example 7 hereinafter, the salt flux was made only by mixing the salts in an anhydrous solid phase.

[0073] 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) 20 commercialized by the Applicant (Pyrotek). Of course, other methods of addition well known to those skilled in the art and already mentioned for use in connection with prior art purification methods can be used to carry out the purification. The concentrations of salt fluxes required to carry out the purification may vary depending on the selected method.
Example 1 [0074] In a crucible made of graphite, one hundred grams (100 g) of NaCl in powder form and sold under the trademark SIFTO INDUSTRIAL were agitated in 1.5 kg of a liquid AA110 aluminum (sold under the trademark Alcan) in which 5 wt %
of solid magnesium were added. The crucible was maintained at 850 C during the whole test. Samples were taken every day during 7 days. According to these daily analyses, the sodium content of the resulting aluminum alloy was at a minimal level of 2 ppm during the whole test, showing that, contrary to apprehensions of those skilled in the art, an addition of NaCl does not involve an absorption of sodium in an aluminum alloy with high magnesium content.

Example 2 [0075] In a graphite crucible, fifteen grams (15 g) of a salt flux consisting of a binary mixture of 45 wt % NaCl and 55 wt % MgCI2 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 MgCI2 in flake form and sold under the trademark SKYLINE.

Example 3 [0076] In a graphite crucible, fifteen grams (15 g) of a salt flux consisting of a ternary mixture of 20 wt % NaCl, 20 wt % KCI and 60 wt % MgCI2 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 NaCI 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 MgCl2 in flake form and sold under the trademark SKYLINE.

Example 4:

[0077] 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. Then, three hundred and sixty grams (360g) of a salt flux made of 45 wt % NaCI and 55 wt % MgCl2 were added to the resulting alloy while agitating it in order to further purify it. The salt flux was prepared from NaCI in powder form and sold under the trademark SIFTO INDUSTRIAL and MgC12 in flake form and sold under the trademark SKYLINE.

[0078] 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.
Example 5 [0079] 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 MgCI2 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.

[0080] Two kg of AA1100 aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two grams of the flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. Samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

[0081] Analyses of samples have shown a reduction of the Ca level from 115 ppm to 3 ppm after the addition of the salt flux. Thirty minutes later, the calcium level was under 2 ppm. No increase in the sodium content was noted during the test.
The level of sodium in the alloy was in the order of 2 ppm.

Example 6 [0082] 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 MgCl2 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 microns was recovered.

[0083] Two kg of AM 100 aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two grams of the salt flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. The agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

[0084] 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.

Exemple 7 [0085] Fifty grams of a salt flux were prepared only by mixing 22.5 grams of NaCI 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 MgCl2 in flake form and sold under the trademark SKYLINE with a granulometry 90 % lower than 4.7 mm and 85 % higher to 1 mm.

[0086] Two kg of AM 100 aluminum alloy (sold under the trademark Alcan) 5 were melted and kept in liquid phase at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two 10 grams of the salt flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. Agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

[0087] Analyses of samples have shown a reduction of the Ca level from 15 77 ppm to 2 ppm after the addition of the salt flux. Thirty minutes later, the calcium level was under 1 ppm. No increase in the sodium content was noted during the test.
The sodium level was in the order of 2 ppm.

Example 8 (0088] Two kg of AM 100 aluminum alloy (sold under the trademark Alcan) 20 were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. Stirring was maintained during 2 minutes. A sample of the metal was taken for analysis. Two 25 grams of the PROMAG SI (trademark) formed of 40 wt % KCI and 60 wt % MgCI2, 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.

[0089] Analyses of samples have shown a reduction of the Ca level from 75 ppm to 7 ppm after the addition of the salt flux. Thirty minutes later the calcium level was under 5 ppm (see Figure 4). These analyses show that binary fluxes of NaCl and MgCI2 are more efficient than a ternary flux of NaCl, KCI and MgCI2 or a binary flux of KCI and MgCl2.
Ex.5 Ex.6 Ex. 7 Ex.8 Reference NaCI-MgCI2 NaCI-KCI-MgCI2 NaCI-MgCI2 Promag SI"` (no flux) (45-55) (20-20-60) (45-55) (KCI - MgCI2) Fused Fused Mix (40-60) Time After Ca 115 108 77 75 77 After salt 3 7 2 7 -30 min <1 2 <1 <5 58 60 min <1 <1 <1 <5 -90 min <1 <1 <1 <5 -120min - - - - 39 * trademark Example 9 [0090] Fifty grams of flux were prepared by mixing 12.5 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 7.5 grams of KCI in powder form (sold under the trademark IMC Kalium) and 30 grams of anhydrous MgCl2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 535 C until completely melt. 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.

[0091] Two kg of P1020A aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two grams of the salt flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. The agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

[0092] The analysis of samples shows a reduction of the Ca level from 62 ppm to 8 ppm after the addition of the salt flux. Thirty minutes later, the calcium level was lower than 5 ppm. No increase in sodium content was noted during the test. The sodium level was in the order of 5 ppm.

Example 10 [0093] Fifty grams of flux were prepared by mixing 10 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 10 grams of KCI in powder form (sold under the trademark IMC Kalium) and 30 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 535 C until completely melt. 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.
[0094] Two kg of P1020A aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two grams of the salt flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. The agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

[0095] The analysis of samples shows a reduction of the Ca level from 59 ppm to 15 ppm after the addition of the salt flux. Ninety minutes later, the calcium level was lower than 5 ppm. No increase in sodium content was noted during the test.
The sodium level was in the order of 5 ppm.

Example 11 [0096] Fifty grams of flux were prepared by mixing 12.5 grams of NaCI in powder form (sold under the trademark Sifto Industrial), 10 grams of KCI in powder form (sold under the trademark IMC Kalium) and 27.5 grams of anhydrous MgCl2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 535 C until completely melt. 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.

[0097] Two kg of P1020A aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two grams of the salt flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. The agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later.

[0098] The analysis of samples shows a reduction of the Ca level from 50 ppm to 12 ppm after the addition of the salt flux. Ninety minutes later, the calcium level was lower than 5 ppm. No increase in sodium content was noted during the test.
The sodium level was in the order of 5 ppm.

Example 12 [0099] Fifty grams of flux were prepared by mixing 5 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 22.5 grams of KCI in powder form (sold under the trademark IMC Kalium) and 22.5 grams of anhydrous MgCl2 in flake form (sold under the trademark Slyline), in a small alumina crucible. The mixture was exposed at a temperature of 535 C until completely melt. 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.

[0100] Two kg of P1020A aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. Two grams of the salt flux formed hereinabove were added to the liquid aluminum alloy doped with calcium while agitating for 2 minutes. The agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 5 90 minutes later.

[0101] The analysis of samples shows a reduction of the Ca level from 58 ppm to 8 ppm after the addition of the salt flux. Sixty minutes later, the calcium level was lower than 5 ppm. No increase in sodium content was noted during the test. The sodium level was in the order of 5 ppm.

10 Example 13 [0102] Two kg of P1020A aluminum alloy (sold under the trademark Alcan) were melted and kept in liquid state at 700 C in a graphite crucible. To this alloy, 2 grams of an aluminum alloy consisting of 90 wt % of aluminum and 10 wt % of calcium (sold under the trademark KB Alloys) were added in a vortex formed with an 15 agitator in the liquid metal, said agitator having straight blades. The agitation was maintained during 2 minutes. A sample of the metal was taken for analysis. The agitation was stopped and samples were taken immediately after the end of the agitation as well as 30, 60 and 90 minutes later. The analysis of samples shows the Ca level over time.

20 [0103] Data related to concentration of Ca in ppm and obtained from examples 9 to 13 are summarized in the following table and illustrated in Fig.
5:

Composition (MgCI2/KCI/NaCI) in weight %

Ex. 9 Ex. 10 Ex. 11 Ex. 12 Ex. 13 60/15/25 60/20/20 55/20/25. 45/45/10 No flux After addition of 61.80 58.53 49.97 58.27 57.77 Ca After addition of 8.07 14.70 11.90 8.17 52.63 flux (2 min) After addition of 4.93 9.10 7.87 5.07 43.90 flux (30 min) After addition of 4.63 6.50 5.90 5.00 31.93 flux (60 min) After addition of 4.50 4.87 4.83 3.90 22.43 flux (90 min) [0104] From the data contained in the above mentioned examples 9 to 13, it appears that exemplified ternary mixtures show that similarly to what was noted for MgCI2/KCI binary mixture and MgCI2/NaCI binary mixture, there was no increase of the residual level in sodium. In addition, with reference to data contained in the above mentioned table, the efficiency of the reduction of the Ca level in aluminum is very important with respect to what was noted in example 13 and surprisingly faster than what was noted in example 10. The efficiency in Ca level reduction after minutes is similar to what was noted with binary mixtures of MgCI2/KCI and MgCI2/NaCI.

MELTING POINTS DETERMINATION
Exemple 14 [0105] Sixty grams of flux were prepared by mixing 26.40 grams of KCI in powder form (sold under the trademark IMC Kalium) and 33.60 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 550 C for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 486 C.

Exemple 15 [0106] Seventy five grams of flux were prepared by mixing 32.14 grams of NaCI in powder form (sold under the trademark Sifto Industrial), and 42.86 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible. The mixture was exposed at a temperature of 580 C for 30 minutes.
The crucible was then removed from the oven and isolated in wool for the cooling.
The temperature of the mixture was recorded until being stable. The melting point was of 443 C.

Example 16 [0107] Seventy grams of flux were prepared by mixing 17.129 grams of NaCI
in powder form (sold under the trademark Sifto Industrial), 13.923 grams of KCI in powder form (sold under the trademark IMC Kalium) and 38.948 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible.

The mixture was exposed at a temperature of 535 C for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 390 C.

Example 17 [0108] Seventy grams of flux were prepared by mixing 7.7 grams of NaCI in powder form (sold under the trademark Sifto Industrial), 31.01 grams of KCI in powder form (sold under the trademark IMC Kalium) and 31.29 grams of anhydrous MgCl2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 535 C for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 403 C.

Example 18 [0109] Seventy grams of flux were prepared by mixing 10.024 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 19.173 grams of KCI in powder form (sold under the trademark IMC Kalium) and 40.803 grams of anhydrous MgCIZ in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 560 C for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 430 C.

Example 19 [0110] Seventy grams of flux were prepared by mixing 15.379 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 13.720 grams of KCI in powder form (sold under the trademark IMC Kalium) and 40.901 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 560 C for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 398 C.

Example 20 [0111] Seventy grams of flux were prepared by mixing 22.288 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 5.012 grams of KCI
in powder form (sold under the trademark IMC Kalium) and 42.7 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 560 C 'for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 442 C.

Example 21 [0112] Seventy grams of flux were prepared by mixing 17.5 grams of NaCl in powder form (sold under the trademark Sifto Industrial), 10.5 grams of KCI in powder form (sold under the trademark IMC Kalium) and 42 grams of anhydrous MgCI2 in flake form (sold under the trademark Slyline), in a small alumina crucible.
The mixture was exposed at a temperature of 560 C for 30 minutes. The crucible was then removed from the oven and isolated in wool for the cooling. The temperature of the mixture was recorded until being stable. The melting point was of 417 C.

[0113] Data related to melting points obtained from examples 14 to 21 are summarized in the following table:

Compositions (wt. %) Approx. Melting point Examples MgCl2 KCI NaCl C
14 56.00 44.00 0.00 486 15 57.14 0.00 42.86 443 16 55.64 19.89 24.47 390 17 44.70 44.30 11.00 403 18 58.29 14.32 27.39 430 19 58.43 19.60 21.97 398 20 61.00 7.16 31.84 442 21 60.00 15.00 25.00 417 [0114] It appears from the above table that a ternary mixture always have a melting point lower that is lower that the one of the binary mixture MgCI2/KCI
or the binary mixture MgCI2/NaCI. In this regard, it is to be noted that a lowering in the 5 melting point of MgCI2/KCI/NaCl tertiary mixtures allows an economical reduction of costs concerning energy and raw material. Indeed, there will be a substantial economy of energy for the preparation of fused and liquid ternary mixtures, and an economical reduction of costs in raw material, sodium chloride being 6 to 8 times cheaper than KCI.

10 [0115] In view of the foregoing, it appears that tertiary mixtures of MgCI2/KCI/NaCI having low melting points provide an efficient and fast reduction of the calcium level in liquid aluminum, and that tertiary mixtures of examples 9, 11 and 12 surprisingly show a faster reduction of the calcium level in liquid aluminum.

[0116] The present invention has been described with respect to its preferred embodiments. The description and the drawings are only intended to aid to the understanding of the invention and are not intended to limit its scope. It will be clear to those skilled in the art that numerous variations and modifications can be made to the implementation of the invention without being outside the scope of the invention.
Such variations and modifications are covered by the present invention. The invention will be now described in the following claims:

Claims (84)

1 A method for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, wherein said method comprises:

.cndot. heating the metal to a liquid phase; and .cndot. contacting the liquid metal with a salt flux consisting of a tertiary mixture of NaCl, KCl, and MgCl2, said salt flux being selected in the group consisting of:

.cndot. salt fluxes in the form of a tertiary mixture of particles and comprising more than 22 % by weight of NaCl;

.cndot. salt fluxes in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 and having the following formulations:

.circle. 5-18 % by weight of NaCl, .circle. 17-60 % by weight of KCl, .circle. 35-65 % by weight of MgCl2 ;

.cndot. salt fluxes in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 and having the following formulations:

.circle. more than 22 to 55 % by weight of NaCl, .circle. 13-43 % by weight of KCl, .circle. 35-65 % by weight of MgCl2 ; and .cndot. salt fluxes in the form of a liquid tertiary mixture.
2. The method of claim 1, wherein said salt flux is a ternary mixture of particles of NaCl, KCl, and MgCl2, wherein more than 22 % by weight of said tertiary mixture consists of NaCl.
3. The method of claim 2, wherein particles have an average particle size comprised between 100 µm and 3.35mm.
4. The method of claim 2, wherein said particles have an average size particle comprised between 0.85 mm and 3.15 mm.
5. The method of claim 2, wherein said particles have an average particle size comprised between 100 µm and 1 mm.
6. The method of claim 2, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
7. The method of claim 2, wherein said tertiary mixture comprises:
a) from more than 22 to 30 % by weight of NaCl, b) from 5 to 43 % by weight of KCl, and c) from 35 to 65 % by weight of MgCl2.
8. The method of claim 2, wherein said tertiary mixture comprises :
a) 25 % by weight of NaCl, b) 15 % by weight of KCl, and c) 60 % by weight of particles of MgCl2;

said tertiary mixture having a melting point of about 417°C.
9. The method of claim 8, wherein particles have an average particle size comprised between 100 µm and 3.35 mm.
10. The method of claim 8, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
11. The method of claim 8, wherein said particles have an average particle size between 100 µm and 1 mm.
12. The method of claim 8, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
13. The method of claim 1, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 having the following formulations:

.circle. 5-18 % by weight of NaCl, .circle. 17-60 % by weight of KCl, .circle. 35-65 % by weight of MgCl2.
14. The method of claim 13, wherein said particles have an average particle size between 100 µm and 3.35mm.
15. The method of claim 13, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
16. The method of claim 13, wherein said particles have an average particle size between 100 µm and 1 mm.
17. The method of claim 13, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
18. The method of claim 1, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 having the following formulations:

.circle. more than 22 to 55 % by weight of NaCl, .circle. 13-43 % by weight of KCl, .circle. 35-65 % by weight of MgCl2.
19. The method of claim 18, wherein said particles have an average particle size between 100 µm and 3.35mm.
20. The method of claim 18, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
21. The method of claim 18, wherein said particles have an average particle size between 100 µm and 1 mm.
22. The method of claim 18, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
23. The method according to claim 18, wherein said tertiary mixture comprises:

a) 25 % by weight of NaCl, b) 15 % by weight of KCl, and c) 60 % by weight of MgCl2;

said tertiary mixture having a melting point of about 417°C.
24. The method of claim 23, wherein said particles have an average particle size between 100 µm and 3.35 mm.
25. The method of claim 23, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
26. The method of claim 23, wherein said particles have an average particle size between 100 µm and 1 mm.
27. The method of claim 23, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
28. The method of claim 1, wherein said salt flux is a liquid tertiary mixture of NaCl, KCl, and MgCl2.
29. The method of claim 28, wherein said liquid tertiary mixture comprises:
a) from 10 to 35 % by weight of NaCl, b) from 5 to 45 % by weight of KCl, and c) from 40 to 65 % by weight of MgCl2.
30. The method according to claim 28, wherein more than 22 % by weight of said liquid tertiary mixture consists of NaCl.
31. The method according to claim 28, wherein said liquid tertiary mixture comprises:

a) from more than 22 to 35 % by weight of NaCl, b) from 5 to 38 % by weight of KCl, and c) from 40 to 65 % by weight of MgCl2.
32. The method according to claim 28, wherein said tertiary mixture comprises:

a) 25 % by weight of NaCl, b) 15 % by weight of KCl, and c) 60 % by weight of MgCl2.
33. The method according to claim 1, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
34. The method according to claim 2, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
35. The method according to claim 13, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
36. The method according to claim 18, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
37. The method according to claim 28, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
38. The method according to claim 1, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
39. The method according to claim 2, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
40. The method according to claim 13, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
41. The method according to claim 18, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
42. The method according to claim 28, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
43. Use of a salt flux consisting of a tertiary mixture of NaCl, KCl, and MgCl2 for the purification of a metal selected from the group consisting of aluminum and aluminum alloys, wherein said method comprises:

.cndot. heating the metal to a liquid phase; and .cndot. contacting the liquid metal with a salt flux consisting of a tertiary mixture of NaCl, KCl, and MgCl2, said salt flux being selected in the group consisting of:

.cndot. salt fluxes in the form of a tertiary mixture of particles and comprising more than 22 % by weight of NaCl;

.cndot. salt fluxes in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 and having the following formulations:

.circle. 5-18 % by weight of NaCl, .circle. 17-60 % by weight of KCl, .circle. 35-65 % by weight of MgCl2 ;

.cndot. salt fluxes in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 and having the following formulations:

.circle. more than 22 to 55 % by weight of NaCl, .circle. 13-43 % by weight of KCl, .circle. 35-65 % by weight of MgCl2 ; and .cndot. salt fluxes in the form of a liquid tertiary mixture.
44. The use of claim 43, wherein said salt flux is a ternary mixture of particles of NaCl, KCl, and MgCl2, wherein more than 22 % by weight of said tertiary mixture consists of NaCl.
45. The use of claim 44, wherein particles have an average particle size comprised between 100 µm and 3.35mm.
46. The use of claim 44, wherein said particles have an average size particle comprised between 0.85 mm and 3.15 mm.
47. The use of claim 44, wherein said particles have an average particle size comprised between 100 µm and 1 mm.
48. The use of claim 44, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
49. The use of claim 44, wherein said tertiary mixture comprises:
a) from more than 22 to 30 % by weight of NaCl, b) from 5 to 43 % by weight of KCl, and c) from 35 to 65 % by weight of MgCl2.
50. The use of claim 44, wherein said tertiary mixture comprises :
a) 25 % by weight of NaCl, b) 15 % by weight of KCl, and c) 60 % by weight of particles Of MgCl2;

said tertiary mixture having a melting point of about 417°C.
51. The use of claim 50, wherein particles have an average particle size comprised between 100 µm and 3.35 mm.
52. The use of claim 50, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
53. The use of claim 50, wherein said particles have an average particle size between 100 µm and 1 mm.
54. The use of claim 50, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
55. The use, of claim 43, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 having the following formulations:

.circle. 5-18 % by weight of NaCl, .circle. 17-60 % by weight of KCl, .circle. 35-65 % by weight of MgCl2.
56. The use of claim 55, wherein said particles have an average particle size between 100 µm and 3.35mm.
57. The use of claim 55, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
58. The use of claim 55, wherein said particles have an average particle size between 100 µm and 1 mm.
59. The use of claim 55, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
60. The use of claim 43, wherein said salt flux is in the form of particles obtained by grinding a fused salt of NaCl, KCl and MgCl2 having the following formulations:

.circle. more than 22 to 55 % by weight of NaCl, .circle. 13-43 % by weight of KCl, .circle. 35-65 % by weight of MgCl2.
61. The use of claim 60, wherein said particles have an average particle size between 100 µm and 3.35mm.
62. The use of claim 60, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
63. The use of claim 60, wherein said particles have an average particle size between 100 µm and 1 mm.
64. The use of claim 60, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
65. The use according to claim 60, wherein said tertiary mixture comprises:
a) 25 % by weight of NaCl, b) 15 % by weight of KCl, and c) 60 % by weight of MgCl2;

said tertiary mixture having a melting point of about 417°C.
66. The use of claim 65, wherein said particles have an average particle size between 100 µm and 3.35 mm.
67. The use of claim 65, wherein said particles have an average size particle between 0.85 mm and 3.15 mm.
68. The use of claim 65, wherein said particles have an average particle size between 100 µm and 1 mm.
69. The use of claim 65, wherein said particles are contacted with the liquid metal by injection with a gas injection equipment.
70. The use of claim 43, wherein said salt flux is a liquid tertiary mixture of NaCl, KCl, and MgCl2.
71. The use of claim 70, wherein said liquid tertiary mixture comprises:
a) from 10 to 35 % by weight of NaCl, b) from 5 to 45 % by weight of KCl, and c) from 40 to 65 % by weight of MgCl2.
72. The use according to claim 70, wherein more than 22 % by weight of said liquid tertiary mixture consists of NaCl.
73. The use according to claim 70, wherein said liquid tertiary mixture comprises:
a) from more than 22 to 35 % by weight of NaCl, b) from 5 to 38 % by weight of KCl, and c) from 40 to 65 % by weight of MgCl2.
74. The use according to claim 70, wherein said tertiary mixture comprises:
a) 25 % by weight of NaCl, b) 15 % by weight of KCl, and c) 60 % by weight of MgCl2.
75. The use according to claim 43, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
76. The use according to claim 44, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
77. The use according to claim 55, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
78. The use according to claim 60, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
79. The use according to claim 70, wherein the metal is an aluminum alloy having a magnesium content higher than 3 % by weight.
80. The use according to claim 43, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
81. The use according to claim 44, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
82. The use according to claim 55, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
83. The use according to claim 60, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
84. The use according to claim 70, wherein the metal is an aluminum alloy having a silicon content higher than 10 % by weight.
CA 2747650 2011-07-28 2011-07-28 Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof Abandoned CA2747650A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CA 2747650 CA2747650A1 (en) 2011-07-28 2011-07-28 Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof
PCT/CA2012/050507 WO2013013321A1 (en) 2011-07-28 2012-07-26 Use of a tertiary salt flux of nac1, kcl, and mgc12 for the purification of aluminum or aluminum alloys, and method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CA 2747650 CA2747650A1 (en) 2011-07-28 2011-07-28 Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof

Publications (1)

Publication Number Publication Date
CA2747650A1 true CA2747650A1 (en) 2013-01-28

Family

ID=47625536

Family Applications (1)

Application Number Title Priority Date Filing Date
CA 2747650 Abandoned CA2747650A1 (en) 2011-07-28 2011-07-28 Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof

Country Status (1)

Country Link
CA (1) CA2747650A1 (en)

Similar Documents

Publication Publication Date Title
AU2010258042B2 (en) Use of a binary salt flux of NaCl and MgCl2 for the purification of aluminum or aluminum alloys, and method thereof
Utigard The properties and uses of fluxes in molten aluminum processing
CN104328299A (en) Flux for aluminum and aluminum alloy melt refining and preparation method of flux
RU2417266C2 (en) Melted salts for purification of strontium containing magnesium alloys
US10988830B2 (en) Scandium master alloy production
CN101643855B (en) Method for refining aluminum and aluminum alloy melt through in-situ reduction
US20120017726A1 (en) Use of a tertiary salt flux of nacl, kci and mgcl2 for the purification of aluminium or aluminium alloys, and method thereof
JP2004523660A (en) Method for preparing silicon and optionally aluminum and silumin (aluminum silicon alloy)
KR20150033675A (en) Flux composition useful in directional solidification for purifying silicon
US7988763B2 (en) Use of a binary salt flux of NaCl and MgCl2 for the purification of aluminium or aluminium alloys, and method thereof
CN1142301C (en) Flux for removing iron from Mg alloy and its preparing process
WO2013013321A1 (en) Use of a tertiary salt flux of nac1, kcl, and mgc12 for the purification of aluminum or aluminum alloys, and method thereof
CN101942578A (en) Magnesium alloy composite flux, preparation thereof and use thereof
CA2747650A1 (en) Use of tertiary salt flux of naci, kci, and mgci2 for the purification of aluminum or aluminum alloys, and method thereof
TWI488807B (en) Addition of alkali magnesium halide to a solvent metal
Baek et al. Removal of Ca from magnesium melt by flux refining
CN100393912C (en) Magnesium-zirconium alloying
EP4192992A1 (en) Multi-component flux
CN1275628A (en) Aluminium alloy covering slag-cleaning agent
JP4599521B2 (en) Method for removing lead in copper alloys
JP2002371376A (en) Method of recycling sludge, and slag-removing agent for molten aluminum alloy
JP5950103B2 (en) Separation of precious metals and sulfate impurities
JP5673776B1 (en) Ash draw flux
RU2150523C1 (en) Method of aluminothermic refining of dust-like zinc dross fraction
JP2020007630A (en) Flux for dephosphorylation

Legal Events

Date Code Title Description
FZDE Dead

Effective date: 20140916