CA1095732A - Process for refining molten metal - Google Patents
Process for refining molten metalInfo
- Publication number
- CA1095732A CA1095732A CA280,820A CA280820A CA1095732A CA 1095732 A CA1095732 A CA 1095732A CA 280820 A CA280820 A CA 280820A CA 1095732 A CA1095732 A CA 1095732A
- Authority
- CA
- Canada
- Prior art keywords
- gas
- refining
- molten metal
- melt
- 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.)
- Expired
Links
Classifications
-
- 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
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
- C22B9/055—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ while the metal is circulating, e.g. combined with filtration
-
- 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
- C22B9/05—Refining by treating with gases, e.g. gas flushing also refining by means of a material generating gas in situ
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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)
- Treatment Of Steel In Its Molten State (AREA)
Abstract
PROCESS FOR REFINING MOLTEN METAL
ABSTRACT
A process for refining molten metal selected from the group consisting of magnesium, copper, zinc, tin, and lead comprising the steps of:
1. feeding the molten metal into a refining zone;
2. maintaining a protective atmosphere above the surface of said molten metal at a greater than atmospheric pressure, thereby preventing contact of the melt with air or atmospheric moisture;
3. providing a gas injection device submerged in said molten metal comprising (a) a shaft fixedly attached to a vaned rotor at its lower end, (b) a stationary sleeve surrounding said shaft, and (c) a passageway for conveying and discharging refining gas into the molten metal running the length of said gas injection device;
4. introducing refining gas into the upper end of said passageway under sufficient pressure to be injected into the melt;
5. preheating the refining gas by contact thereof with the hot walls of the passageway, whereby the gas is expanded, before being sub-divided into gas bubbles, to the point where thermal growth of said bubbles in the melt is substantially prevented;
6. directing the preheated refining gas to the vanes of said rotor of said gas injection device;
7. sub-dividing the refining gas into discrete gas bubbles by rotating said vaned rotor at a speed sufficient to create a circulation pattern in the molten metal such that the gas bubbles are transported substantially radially outward with a downward component relative to their points of entry into the melt thereby coming into intimate contact with substantially the entire mass of molten metal in said refining zone, resulting in the removal of dissolved gases and sub-stantially all non-metallic impurities from said melt;
8. withdrawing the spent refining gas and the dissolved gases released by the metal while collect-ing other non-metallic impurities in a slag layer on the surface of the molten metal; and 9. withdrawing the refined molten metal from said refining zone.
ABSTRACT
A process for refining molten metal selected from the group consisting of magnesium, copper, zinc, tin, and lead comprising the steps of:
1. feeding the molten metal into a refining zone;
2. maintaining a protective atmosphere above the surface of said molten metal at a greater than atmospheric pressure, thereby preventing contact of the melt with air or atmospheric moisture;
3. providing a gas injection device submerged in said molten metal comprising (a) a shaft fixedly attached to a vaned rotor at its lower end, (b) a stationary sleeve surrounding said shaft, and (c) a passageway for conveying and discharging refining gas into the molten metal running the length of said gas injection device;
4. introducing refining gas into the upper end of said passageway under sufficient pressure to be injected into the melt;
5. preheating the refining gas by contact thereof with the hot walls of the passageway, whereby the gas is expanded, before being sub-divided into gas bubbles, to the point where thermal growth of said bubbles in the melt is substantially prevented;
6. directing the preheated refining gas to the vanes of said rotor of said gas injection device;
7. sub-dividing the refining gas into discrete gas bubbles by rotating said vaned rotor at a speed sufficient to create a circulation pattern in the molten metal such that the gas bubbles are transported substantially radially outward with a downward component relative to their points of entry into the melt thereby coming into intimate contact with substantially the entire mass of molten metal in said refining zone, resulting in the removal of dissolved gases and sub-stantially all non-metallic impurities from said melt;
8. withdrawing the spent refining gas and the dissolved gases released by the metal while collect-ing other non-metallic impurities in a slag layer on the surface of the molten metal; and 9. withdrawing the refined molten metal from said refining zone.
Description
~95'~3Z
This invention relates in general to refining of molten metal, and more particularly, to a method for removing dissolved gases and non-metallic impurities from molten metal wîthout the emission of corrosive or environmentally harmful gases and fumes.
Molten metal, prior to casting, contains many impurities which, if not removed, cause high scrap loss in casting, or otherwise cause poor metal quality in products fabricated therefrom. The principal object-ionable impurities are dissolved gases and suspendednon-metallic particles such as metal oxides and refractory particles, ~ t is an ob;ect of this invention to provide a process for refining metal with refining gas which efficiently removes dissolved gases and other non-metallic impurities from the metal in a continuous process at high metal throughput rates.
The above object and others, which will be apparent to those skilled in the art, are achieved by a process for removing dissolved gases and non-metallic impurities from a molten metal selected from the group consisting of magnesium, copper, zinc, tin and lead comprising the steps of:
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1~35'73Z
(1~ feeding the molten metal into a refining zone;
. (2) maintaining a protective a~mosphere above the surface of the molten metal at a positive pressure relative to the ambient pressure, thereby preventing infusion of air and moisture into said zone and contact of the molten metal therewith;
(3) introducing a refining gas in the form of discrete bubbles into the molten metal beneath the surface of the melt;
(4) stirring the molten metal in the refining zone to create a circulation pattern in the molten metal relative to the points of entry of the gas bubbles in the melt such that the gas bubbles introduced into the melt are transported substantially radially ou~ard, relative to said points of entry of the bubbles, thereby prolonging the residence time of the gas bubbles in the melt and causing the gas bubbles to come into întimate content with substantially the entire mass of molten metal in said refining zone;
(5) withdrawing the spent refining gas and the dissolved gases released by the metal while collect-ing and separating the other non-metallic impurities in a slag layer on the surface of ~he molten metal; and , (6) withdrawing the refined molten metal from said refining zone.
~9573Z
The term "refining gas" as used herein is meant to include gases which are conventionally used in the refining of magnesium, copper, zinc, tin, and lead.
The com~on characteristic of these refining gases is that they are inert towards the molten metal being refined. Argon and nitrogen or mixtures thereof are preferred although other inert gases of the periodic table are suitable for the present invention. Other useful refining gases are hydrogen and carbon monoxide or mixtures thereof with each other or the inert gases o the periodic table. It will be noted that hydrogen and carbon monoxide may be used in instances where they will not react with the molten metal, but will react with gaseous impurities such as oxygen. Other reactive gases with similar characteristics can also be used such as sulfur hexafluoride, chlorine, and halogenated hydrocarbons. Selection of a particular refining gas is generally made in accordance with the characteristics of the particular metal being refined.
The ter~l "metal" as used throughout the speci~ication and claims is meant to include pure metal as well as alloys of the metal.
DRAWINGS
Figure 1 is a perspective view of a gas injection devlce for use in the present invention;
Figure 2 is a cros~-sectional view of the device shown in Figure l;
1~95732 /;
Figure 3 is a schematic diagram in cross-section illustrating a preferred system for refining a metal stream in a continuous process in accordance with the present invention;
Figures 4 and 5 are a cross-sectional and a top view, respectively, of another preferred embodiment of apparatus suitable for refining molten metal in accord-ance with the present invention.
Detailed Description -The gas injection device suggested for use in the present invention is characterized by its ability to inject gas at high flow rates into molten metal in the form ~ dis.crete gas bubbles and to achieve a high degree of gas dispersion throughout the melt. The device, when in operation, induces flow patterns in the metal in the vicinity of the device such that the gas bubbles which are formed, are transported along a resultant flow yector which is radially outward with a downward component relative to the vertical axis of the injection device. These flow patterns have several advantageous effects. First, essentially vertical stirring is provid-ed for the en~ire body of the melt, whereby a downwardly directed flow along the device, in combination with the rotating vanes, causes subdivision of the gas into 1~95732 small discrete gas bubbles. Second, the rapid conveyance of the gas bubbles away from the point of introduction into the melt prevents bubble coalescence in the zone where the gas bubble concentration is the highest.
Third, the g2S residence time of the well dispersed gas bubbles in the melt is prolonged, because the gas bubbles do not immediately, upon formation, rise to the surface under the influence of gravity.
Another factor which contributes to maximization of the subdivision of the gas into small bubbles, and -hence leading to a large metal-gas interfacial area, is the preheating of the gas before it enters the melt.
Such preheating is provided in the present invention by conducting the gas through a passageway running the length of the device which is submerged in the hot molten metal. Thus, the initially cold gas is preheated by contact with the hot, heat conducting walls of the gas passageway, whereby the gas is expanded before being subdivided into gas bubbles. Consequently, the number of bubbles generated from a given volume of gas is increased substantially, and thermal growth of the small bubbles in the melt is substantially prevented.
When used for injecting refining gas into molten metal, the injection device produces an unanticipated improve~ent in the efficiency of the refining operation.
In addition to being able to degas the metal at a high 1~9~73;~: /
throughput rate, the vigorous stirring action produced by the device, coupled with the large gas/metal contact area of the well distributed gas bubbles, assure efficient removal of solid particulate impurities suspended in the melt.
As shown in Figures l and 2, the gas injection device consists of rotor 1, equipped with vertical vanes 2, and rotated by means of a motor, such as an air motor or electric motor (not shown) through shaft 3.
Shaft 3 which does not contact the melt during normal ~
operation, may be constructed of steel, while the remainder of the equipment is preferably constructed from a refractory material, such as commercially avail-able graphite or silicon carbide, materials which are inert toward the metal at the operating temperatures involved. Shaft 3 is shielded from the molten metal by sleeve 4, which is fixedly attached to stator 5.
The abutting inner surfaces 6 and 7 respectively, of sleeve 4 and stator 5, and the abutting outer surfaces 8 and 9 respectively, of shaft 3 and rotor 1, form an annular axial passageway 10 for the gas to be injected.
A plurality of vertical channels 11 are machined into stator 5. The combination of stator 5 and rotor 1, when in operation, induce an upper and lower flow pattern of ~olten metal around the injec~ion device as indicated generally by the arrows 13 and 12, respectively.
_g_ lC~95732 Specifically, the upper flow pattern 13 has a main velocity vector pointing essentially downward, i.e. it is coaxial with the axis of rotation of the rotor 1, thereby forcing the molten metal through the channels 11 of stator 5; the lower, more localized flow pattern indicated by arrows 12, develops beneath the rotor l and is poin~ed essentiall~ upward and perpendicular to the axis of rotation of the rotor 1. The resultant i flow of these components is indicated by arrows 14, which show that the molten metal is forcefully dis-charged by the rotating vanes 2 radially and do-wnwardly away from rotor l. The resultant flow pattern causes a well distributed and uniform gas dispersion and a thorough agitation of the molten metal within the treating vessel.
A refining gas (indicated by arrow 15) is introduced into the annular passageway 10 at a predetermined pres-sure and flow rate. The gas fills the bell shaped pocket 16 which is a continuation of passageway 10 surrounding neck 17 of rotor l. Since the gas is supplied at a pressure greater than the pressure pre-vailing in the molten ~etal at a height indicated by arrow 18, the gas pocket 16 prevents molten ~etal from running baclc through the gas passage and from coming in contact with the metal shaft 3 of the gas injec~or.
Neck 17 surrounds shaft 3 and is constructed from a 1~9573Z
material resistant to the molten metal in order to protect shaft 3 from attack by the molten metal. As shown in Figure 2, the torque from shaft 3 is transferred to rotor 1 by means of winged cross-piece 21 which is threaded to shaft 3. Cross-piece 21 is placed during assembly into cavity 23 of rotor 1, the cavity 23 having a shape corresponding to that of cross-piece 21. There-after, cavity 23 is sealed by threading and cementing neck 17 into thread 24 in rotor 1, The introdu~tion of refining gas 15 into annular passageway 10 need not necessarily be the sole means of providing the gas to be injected, An alternate embodiment of the invention may include a hollow shaft, wherein a passageway 19 extends axially through shaft 3 and is provided with a plurality of drillings 20 which provide communication with passageway 10 and gas pocket 15. Thus, gas (indicated by arrows 15 and 25) may be provided through either passageway 10 or passage-way 19 or both.
It is important that the cold gas (indicated by arrows 15 and 25) entering the injec~or be preheated during its passage thr~ugh passageway 10 or passageway 19, and gas pocket 16 by contacting the sleeve 4 and shaft 3 which are essentially at the temperature of the melt. The preheated gas is forced between the ~anes of the rotor 1 where it is broken up int~ small discrete bubbles by collision with the vanes 2 and by the metal flow sweeping pas~ the vanes. The forced circulation of the metal around the injector device rapidly disperses the gas bubbles as they are formed in a direction essentially along the main flow velocity vector, indicated by arrows 14. The initial trajectory of the gas bubbles follows the direction of the arrows 14 until the buoyancy force prevails and causes the gas bubbles to rise to the surface of the melt.
The beneficial effects of the forced circulation pattern of the metal around the in~ection device include the following: (1) the provision of an efficient mechanism for small gas bubble formation, (2) the prevention of bubble coalescence by aispersing the small gas bubbles almost simultaneously with their formation, (3) the provision of efficient circulation of the metal, and (4) prolonged residence time of the gas bubbles in the ~elt beyond the time they would remain in the melt if gravity were the sole force acting upon them.
The process of the invention can be carried out in a batch-type operation, or in a continuous operation by using a refining system such as shown in Figure 3. The refining system comprises a cast iron shell 31 which is maintained at its operating temperature by conventional heating means which may be located in well 32, and is insula~ed against heat loss by an outer refractory shell 5732 ,' 33. The inner surface of shell 31 is lined with graphite 34 or with other refractory materials which are inert to the molten metal and non-metallic impurities likely to be present. Shell 31 is provided with a cover 36 which rests up~n flanges 39. A gas-tight seal is provided between flanges 39 and cover 36 which may be bolted or otherwise f~stened thereto, thereby allowing the system to be operated without the infiltration of air. A gas injection device 35, such as that shown in Figure 1, is fastened to cover 36 and supported therefrom.
Refining gas (indicated by arrow 37) is injected into molten metal 38 by gas injector 35. The gas after passing through the molten metal, collects in head space 43 to form an inert gas blanket over the melt and leaves through metal inlet port 40 counter-current to the incoming flow of metal. The free cross-sectional area of the gas passage, and hence the pressure in the system, is regulated by damper 49 located in port 40.
The slightly pressurized inert gas in head space 43 prevents air leakage into the vessel.
Entry of the metal 38 into the refining system is through metal inlet port 40. Inside the vessel, metal 38 is sparged by the ùniformly distributed small bubbles of inert gas and is agitated by the action provided by the rotating gas injector 35. Gases dissolved in the melt diffuse into and are carried away by the bubbles 7`32 of inert ga.s as they rise through the melt to the melt surface 42. The large surface area of the finely dispersed gas bubbles also serves as an efficient transport means for suspended non-metallic particles to slag layer 48 at the melt surface 42 from where they can be removed by skimming. The major overall circulation pattern developed in the molten metal are schematically shown by arrows 50. It is this induced flow pattern of metal in the vessel which continues to bring fresh metal into contact with the gas bubbles which are being discharged from the space between the rotor and stator of the injection device.
The refined molten metal l.eaves the refining vessel through discharge port 44 situated below the metal surface 42 in wall 45. The metal then passes through well 46 and leaves the system through exit trough 47 to a casting station. Well 46 may contain a conventional filtering medium, such as, graphite or solid refractory chips.
Skimming of the metal surface 42 may be accomplished by the mode of construction of the refining vessel or by stopping the inlet flow.of metal to the refining vessel while maintaining the flow of inert gas 37 through gas injector 35 so as to push the slag layer 48 into inlet trough 40 from where it may be removed by mechanical means. Alternatively, metal surface 42 can be skimmed by means of a hand tool-inserted into shell ~ ~95732 31 through inlet trough 40 or through an opening (not shown) in cover 36.
j The refinlng operation is not restricted to being carried out in a single refining zone as shown in ~igure 3; rather, the vessel may contain a plurality of individual refining compartments or zones through which the molten metal passes in series. Figures 4 and 5 illustrate such an alternate arrangement.
The refining vessel 55, shown in Figures 4 and 5, is constructed fro~ a refractory which is inert to the~
molten metal, and is insulated against heat losses with high temperature insulating materials. If necessary, the vessel may also be provided with electric heating elements (not shown) to compensate for heat losses.
Refining vessél 55 is provided with a cover 56 which is attached to vessel 55 gas-tight leaving only the ~etal inlet trough 57 unsealed. Gas injectors 59 and 60 which are of the type described in Figure 1, and their respective drives 61 and 62 are supported by cover 56.
Arrows 75 indicate inert gas entering gas injectors 59 and 60 through their respective inlet ports.
The refining vessel 55 is intended to be used in continuous operation, i.e., molten metal is continuously supplied through inlet trough 57 into the vessel 55, the metal is refined by continuous agitation and gas injection through injectors 59 and 60, and the refined -lS-` 8630-3 1~9~i73Z
metal is continuously withdrawn from the vessel via exit trough 58. Reference to Figure 5 shows that refining vessel 55 is provided with two refining zones 63 and 64 separated by a baffle plate 65. The metal first enters refining zone 63 where it is agitated and sparged with an inert gas provided by gas injector 59. The metal leaves the refining zone 63, in part by overflow over the top of baffle plate 65, and partly by underflow through ports 66 provided in baffle plate 65. The metal is further refined in the second refining zone 64 where it is similarly agitated and sparged with inert gas provided by gas injector 60. The metal leaves refining zone 64 by overflowing the bottom baffle plate 67 and entering exit pipe 68. Exit pipe 68 is fabricated from a re:Eractory material, such as graphite or silicon carbide and serves to conduct the refined molten metal from refining zone 64 to exit well 69 where it leaves the refining vessel through exit trough 58.
The refining gas introduced into the system passes `through the molten metal, collects in head space 74 above the metal and leaves the refining vessel 55 through inlet trough 57 above and in counter-current flow to the entering molten metal. The pressure in the refining vessel 55 may be adjusted by a hinged damper 73, located in inlet trough 57, by regulating the free cross-sectional area of the gas passage in inlet trough : 57. Thus, it is possible to provide, in addition to the static seal provide~3 by cover 56, a dynamic gas seal 9~i732 for the refining vessel by operating vessel 55 slightly above the ambient pressure so as to prevent air from entering the vessel.
A distinct advantage of the system of the present invention is that it can be readily adjusted to supply the refining gas requirements for different metals and the speed of refining can be matched to a wide range of casting rates. The specific refining gas requirement, generally expressed as volume of gas at norm~l temperat-ure and pressure per unit weight of metal to be treated, is a function of the composition of the alloy and the degree of purity required in the finished product. The flow rate of metal through the refining system may be governed by the speed of casting, i.e., by the type of casting machines used and by the number of -ngots cast simultaneously from the refined metal.
The following illustrates a convenient way by which operating conditions in the system may be adjusted ~epending upon the particular alloy to be refined and the desired rate of refining in accordance with the present invention.
Initially, the flow rate of the refining gas per gas injection device is calculated from the following formula:
~95~32 V c W C/N (1) where: V = the flow rate of the refining gas through the device, normal cu.ft./min;
W = the metal flow rate or refining rate, lbs~min;
C c the specific refining gas requirement, normal cu.ft./lb. metal;
N = the number of gas injection devices in the system.
The specific refining gas requirement, "C'', is determined by experimentation or, for purposes of start-up, it can be estimated based on the amount of refining gases used for refining the particular metal in conventional practice.
After having determined the necessary gas flow rate through the injection device, the speed of rotation of the rotor is adjusted in accordance with the following formula.
R = (300 ~ 750V + 83r )/d (2) where: R = the speed of rotation of the rotor, (RPM~;
V = the gas flow rate through the device as calculated from formula (1), normal cu.ft /min;
r = the ratio of the least cross-sectional dimension of the refining zone around the rotor to the diameter of the rotor , ? 86~0-3 ~q~gS73;~
(calculated with consistent units); for exa~ple, in tne refining system shown in Figure 5, the least cross-sectional dimension of refining zone 63 is the smaller of the two dimensions indicated by arrows 7Q and 71;
d = the diameter of the rotor, inches.
This formula yields an approximate RPM
for the rotor which ensures a satisfactory dispersion of the refining gas and a good stirring of the metal -bath under most operating conditions, From the formula it can be seen that the speed of the rotor must be increased with increasing refining gas flow rates.
It should be noted, however, that it is possible to operate the device at significantly lower speeds than predicted by this formula, the optimum speed being dictated primarily by the desired degree of refining.
This invention relates in general to refining of molten metal, and more particularly, to a method for removing dissolved gases and non-metallic impurities from molten metal wîthout the emission of corrosive or environmentally harmful gases and fumes.
Molten metal, prior to casting, contains many impurities which, if not removed, cause high scrap loss in casting, or otherwise cause poor metal quality in products fabricated therefrom. The principal object-ionable impurities are dissolved gases and suspendednon-metallic particles such as metal oxides and refractory particles, ~ t is an ob;ect of this invention to provide a process for refining metal with refining gas which efficiently removes dissolved gases and other non-metallic impurities from the metal in a continuous process at high metal throughput rates.
The above object and others, which will be apparent to those skilled in the art, are achieved by a process for removing dissolved gases and non-metallic impurities from a molten metal selected from the group consisting of magnesium, copper, zinc, tin and lead comprising the steps of:
~' t ~b~U_ ~
1~35'73Z
(1~ feeding the molten metal into a refining zone;
. (2) maintaining a protective a~mosphere above the surface of the molten metal at a positive pressure relative to the ambient pressure, thereby preventing infusion of air and moisture into said zone and contact of the molten metal therewith;
(3) introducing a refining gas in the form of discrete bubbles into the molten metal beneath the surface of the melt;
(4) stirring the molten metal in the refining zone to create a circulation pattern in the molten metal relative to the points of entry of the gas bubbles in the melt such that the gas bubbles introduced into the melt are transported substantially radially ou~ard, relative to said points of entry of the bubbles, thereby prolonging the residence time of the gas bubbles in the melt and causing the gas bubbles to come into întimate content with substantially the entire mass of molten metal in said refining zone;
(5) withdrawing the spent refining gas and the dissolved gases released by the metal while collect-ing and separating the other non-metallic impurities in a slag layer on the surface of ~he molten metal; and , (6) withdrawing the refined molten metal from said refining zone.
~9573Z
The term "refining gas" as used herein is meant to include gases which are conventionally used in the refining of magnesium, copper, zinc, tin, and lead.
The com~on characteristic of these refining gases is that they are inert towards the molten metal being refined. Argon and nitrogen or mixtures thereof are preferred although other inert gases of the periodic table are suitable for the present invention. Other useful refining gases are hydrogen and carbon monoxide or mixtures thereof with each other or the inert gases o the periodic table. It will be noted that hydrogen and carbon monoxide may be used in instances where they will not react with the molten metal, but will react with gaseous impurities such as oxygen. Other reactive gases with similar characteristics can also be used such as sulfur hexafluoride, chlorine, and halogenated hydrocarbons. Selection of a particular refining gas is generally made in accordance with the characteristics of the particular metal being refined.
The ter~l "metal" as used throughout the speci~ication and claims is meant to include pure metal as well as alloys of the metal.
DRAWINGS
Figure 1 is a perspective view of a gas injection devlce for use in the present invention;
Figure 2 is a cros~-sectional view of the device shown in Figure l;
1~95732 /;
Figure 3 is a schematic diagram in cross-section illustrating a preferred system for refining a metal stream in a continuous process in accordance with the present invention;
Figures 4 and 5 are a cross-sectional and a top view, respectively, of another preferred embodiment of apparatus suitable for refining molten metal in accord-ance with the present invention.
Detailed Description -The gas injection device suggested for use in the present invention is characterized by its ability to inject gas at high flow rates into molten metal in the form ~ dis.crete gas bubbles and to achieve a high degree of gas dispersion throughout the melt. The device, when in operation, induces flow patterns in the metal in the vicinity of the device such that the gas bubbles which are formed, are transported along a resultant flow yector which is radially outward with a downward component relative to the vertical axis of the injection device. These flow patterns have several advantageous effects. First, essentially vertical stirring is provid-ed for the en~ire body of the melt, whereby a downwardly directed flow along the device, in combination with the rotating vanes, causes subdivision of the gas into 1~95732 small discrete gas bubbles. Second, the rapid conveyance of the gas bubbles away from the point of introduction into the melt prevents bubble coalescence in the zone where the gas bubble concentration is the highest.
Third, the g2S residence time of the well dispersed gas bubbles in the melt is prolonged, because the gas bubbles do not immediately, upon formation, rise to the surface under the influence of gravity.
Another factor which contributes to maximization of the subdivision of the gas into small bubbles, and -hence leading to a large metal-gas interfacial area, is the preheating of the gas before it enters the melt.
Such preheating is provided in the present invention by conducting the gas through a passageway running the length of the device which is submerged in the hot molten metal. Thus, the initially cold gas is preheated by contact with the hot, heat conducting walls of the gas passageway, whereby the gas is expanded before being subdivided into gas bubbles. Consequently, the number of bubbles generated from a given volume of gas is increased substantially, and thermal growth of the small bubbles in the melt is substantially prevented.
When used for injecting refining gas into molten metal, the injection device produces an unanticipated improve~ent in the efficiency of the refining operation.
In addition to being able to degas the metal at a high 1~9~73;~: /
throughput rate, the vigorous stirring action produced by the device, coupled with the large gas/metal contact area of the well distributed gas bubbles, assure efficient removal of solid particulate impurities suspended in the melt.
As shown in Figures l and 2, the gas injection device consists of rotor 1, equipped with vertical vanes 2, and rotated by means of a motor, such as an air motor or electric motor (not shown) through shaft 3.
Shaft 3 which does not contact the melt during normal ~
operation, may be constructed of steel, while the remainder of the equipment is preferably constructed from a refractory material, such as commercially avail-able graphite or silicon carbide, materials which are inert toward the metal at the operating temperatures involved. Shaft 3 is shielded from the molten metal by sleeve 4, which is fixedly attached to stator 5.
The abutting inner surfaces 6 and 7 respectively, of sleeve 4 and stator 5, and the abutting outer surfaces 8 and 9 respectively, of shaft 3 and rotor 1, form an annular axial passageway 10 for the gas to be injected.
A plurality of vertical channels 11 are machined into stator 5. The combination of stator 5 and rotor 1, when in operation, induce an upper and lower flow pattern of ~olten metal around the injec~ion device as indicated generally by the arrows 13 and 12, respectively.
_g_ lC~95732 Specifically, the upper flow pattern 13 has a main velocity vector pointing essentially downward, i.e. it is coaxial with the axis of rotation of the rotor 1, thereby forcing the molten metal through the channels 11 of stator 5; the lower, more localized flow pattern indicated by arrows 12, develops beneath the rotor l and is poin~ed essentiall~ upward and perpendicular to the axis of rotation of the rotor 1. The resultant i flow of these components is indicated by arrows 14, which show that the molten metal is forcefully dis-charged by the rotating vanes 2 radially and do-wnwardly away from rotor l. The resultant flow pattern causes a well distributed and uniform gas dispersion and a thorough agitation of the molten metal within the treating vessel.
A refining gas (indicated by arrow 15) is introduced into the annular passageway 10 at a predetermined pres-sure and flow rate. The gas fills the bell shaped pocket 16 which is a continuation of passageway 10 surrounding neck 17 of rotor l. Since the gas is supplied at a pressure greater than the pressure pre-vailing in the molten ~etal at a height indicated by arrow 18, the gas pocket 16 prevents molten ~etal from running baclc through the gas passage and from coming in contact with the metal shaft 3 of the gas injec~or.
Neck 17 surrounds shaft 3 and is constructed from a 1~9573Z
material resistant to the molten metal in order to protect shaft 3 from attack by the molten metal. As shown in Figure 2, the torque from shaft 3 is transferred to rotor 1 by means of winged cross-piece 21 which is threaded to shaft 3. Cross-piece 21 is placed during assembly into cavity 23 of rotor 1, the cavity 23 having a shape corresponding to that of cross-piece 21. There-after, cavity 23 is sealed by threading and cementing neck 17 into thread 24 in rotor 1, The introdu~tion of refining gas 15 into annular passageway 10 need not necessarily be the sole means of providing the gas to be injected, An alternate embodiment of the invention may include a hollow shaft, wherein a passageway 19 extends axially through shaft 3 and is provided with a plurality of drillings 20 which provide communication with passageway 10 and gas pocket 15. Thus, gas (indicated by arrows 15 and 25) may be provided through either passageway 10 or passage-way 19 or both.
It is important that the cold gas (indicated by arrows 15 and 25) entering the injec~or be preheated during its passage thr~ugh passageway 10 or passageway 19, and gas pocket 16 by contacting the sleeve 4 and shaft 3 which are essentially at the temperature of the melt. The preheated gas is forced between the ~anes of the rotor 1 where it is broken up int~ small discrete bubbles by collision with the vanes 2 and by the metal flow sweeping pas~ the vanes. The forced circulation of the metal around the injector device rapidly disperses the gas bubbles as they are formed in a direction essentially along the main flow velocity vector, indicated by arrows 14. The initial trajectory of the gas bubbles follows the direction of the arrows 14 until the buoyancy force prevails and causes the gas bubbles to rise to the surface of the melt.
The beneficial effects of the forced circulation pattern of the metal around the in~ection device include the following: (1) the provision of an efficient mechanism for small gas bubble formation, (2) the prevention of bubble coalescence by aispersing the small gas bubbles almost simultaneously with their formation, (3) the provision of efficient circulation of the metal, and (4) prolonged residence time of the gas bubbles in the ~elt beyond the time they would remain in the melt if gravity were the sole force acting upon them.
The process of the invention can be carried out in a batch-type operation, or in a continuous operation by using a refining system such as shown in Figure 3. The refining system comprises a cast iron shell 31 which is maintained at its operating temperature by conventional heating means which may be located in well 32, and is insula~ed against heat loss by an outer refractory shell 5732 ,' 33. The inner surface of shell 31 is lined with graphite 34 or with other refractory materials which are inert to the molten metal and non-metallic impurities likely to be present. Shell 31 is provided with a cover 36 which rests up~n flanges 39. A gas-tight seal is provided between flanges 39 and cover 36 which may be bolted or otherwise f~stened thereto, thereby allowing the system to be operated without the infiltration of air. A gas injection device 35, such as that shown in Figure 1, is fastened to cover 36 and supported therefrom.
Refining gas (indicated by arrow 37) is injected into molten metal 38 by gas injector 35. The gas after passing through the molten metal, collects in head space 43 to form an inert gas blanket over the melt and leaves through metal inlet port 40 counter-current to the incoming flow of metal. The free cross-sectional area of the gas passage, and hence the pressure in the system, is regulated by damper 49 located in port 40.
The slightly pressurized inert gas in head space 43 prevents air leakage into the vessel.
Entry of the metal 38 into the refining system is through metal inlet port 40. Inside the vessel, metal 38 is sparged by the ùniformly distributed small bubbles of inert gas and is agitated by the action provided by the rotating gas injector 35. Gases dissolved in the melt diffuse into and are carried away by the bubbles 7`32 of inert ga.s as they rise through the melt to the melt surface 42. The large surface area of the finely dispersed gas bubbles also serves as an efficient transport means for suspended non-metallic particles to slag layer 48 at the melt surface 42 from where they can be removed by skimming. The major overall circulation pattern developed in the molten metal are schematically shown by arrows 50. It is this induced flow pattern of metal in the vessel which continues to bring fresh metal into contact with the gas bubbles which are being discharged from the space between the rotor and stator of the injection device.
The refined molten metal l.eaves the refining vessel through discharge port 44 situated below the metal surface 42 in wall 45. The metal then passes through well 46 and leaves the system through exit trough 47 to a casting station. Well 46 may contain a conventional filtering medium, such as, graphite or solid refractory chips.
Skimming of the metal surface 42 may be accomplished by the mode of construction of the refining vessel or by stopping the inlet flow.of metal to the refining vessel while maintaining the flow of inert gas 37 through gas injector 35 so as to push the slag layer 48 into inlet trough 40 from where it may be removed by mechanical means. Alternatively, metal surface 42 can be skimmed by means of a hand tool-inserted into shell ~ ~95732 31 through inlet trough 40 or through an opening (not shown) in cover 36.
j The refinlng operation is not restricted to being carried out in a single refining zone as shown in ~igure 3; rather, the vessel may contain a plurality of individual refining compartments or zones through which the molten metal passes in series. Figures 4 and 5 illustrate such an alternate arrangement.
The refining vessel 55, shown in Figures 4 and 5, is constructed fro~ a refractory which is inert to the~
molten metal, and is insulated against heat losses with high temperature insulating materials. If necessary, the vessel may also be provided with electric heating elements (not shown) to compensate for heat losses.
Refining vessél 55 is provided with a cover 56 which is attached to vessel 55 gas-tight leaving only the ~etal inlet trough 57 unsealed. Gas injectors 59 and 60 which are of the type described in Figure 1, and their respective drives 61 and 62 are supported by cover 56.
Arrows 75 indicate inert gas entering gas injectors 59 and 60 through their respective inlet ports.
The refining vessel 55 is intended to be used in continuous operation, i.e., molten metal is continuously supplied through inlet trough 57 into the vessel 55, the metal is refined by continuous agitation and gas injection through injectors 59 and 60, and the refined -lS-` 8630-3 1~9~i73Z
metal is continuously withdrawn from the vessel via exit trough 58. Reference to Figure 5 shows that refining vessel 55 is provided with two refining zones 63 and 64 separated by a baffle plate 65. The metal first enters refining zone 63 where it is agitated and sparged with an inert gas provided by gas injector 59. The metal leaves the refining zone 63, in part by overflow over the top of baffle plate 65, and partly by underflow through ports 66 provided in baffle plate 65. The metal is further refined in the second refining zone 64 where it is similarly agitated and sparged with inert gas provided by gas injector 60. The metal leaves refining zone 64 by overflowing the bottom baffle plate 67 and entering exit pipe 68. Exit pipe 68 is fabricated from a re:Eractory material, such as graphite or silicon carbide and serves to conduct the refined molten metal from refining zone 64 to exit well 69 where it leaves the refining vessel through exit trough 58.
The refining gas introduced into the system passes `through the molten metal, collects in head space 74 above the metal and leaves the refining vessel 55 through inlet trough 57 above and in counter-current flow to the entering molten metal. The pressure in the refining vessel 55 may be adjusted by a hinged damper 73, located in inlet trough 57, by regulating the free cross-sectional area of the gas passage in inlet trough : 57. Thus, it is possible to provide, in addition to the static seal provide~3 by cover 56, a dynamic gas seal 9~i732 for the refining vessel by operating vessel 55 slightly above the ambient pressure so as to prevent air from entering the vessel.
A distinct advantage of the system of the present invention is that it can be readily adjusted to supply the refining gas requirements for different metals and the speed of refining can be matched to a wide range of casting rates. The specific refining gas requirement, generally expressed as volume of gas at norm~l temperat-ure and pressure per unit weight of metal to be treated, is a function of the composition of the alloy and the degree of purity required in the finished product. The flow rate of metal through the refining system may be governed by the speed of casting, i.e., by the type of casting machines used and by the number of -ngots cast simultaneously from the refined metal.
The following illustrates a convenient way by which operating conditions in the system may be adjusted ~epending upon the particular alloy to be refined and the desired rate of refining in accordance with the present invention.
Initially, the flow rate of the refining gas per gas injection device is calculated from the following formula:
~95~32 V c W C/N (1) where: V = the flow rate of the refining gas through the device, normal cu.ft./min;
W = the metal flow rate or refining rate, lbs~min;
C c the specific refining gas requirement, normal cu.ft./lb. metal;
N = the number of gas injection devices in the system.
The specific refining gas requirement, "C'', is determined by experimentation or, for purposes of start-up, it can be estimated based on the amount of refining gases used for refining the particular metal in conventional practice.
After having determined the necessary gas flow rate through the injection device, the speed of rotation of the rotor is adjusted in accordance with the following formula.
R = (300 ~ 750V + 83r )/d (2) where: R = the speed of rotation of the rotor, (RPM~;
V = the gas flow rate through the device as calculated from formula (1), normal cu.ft /min;
r = the ratio of the least cross-sectional dimension of the refining zone around the rotor to the diameter of the rotor , ? 86~0-3 ~q~gS73;~
(calculated with consistent units); for exa~ple, in tne refining system shown in Figure 5, the least cross-sectional dimension of refining zone 63 is the smaller of the two dimensions indicated by arrows 7Q and 71;
d = the diameter of the rotor, inches.
This formula yields an approximate RPM
for the rotor which ensures a satisfactory dispersion of the refining gas and a good stirring of the metal -bath under most operating conditions, From the formula it can be seen that the speed of the rotor must be increased with increasing refining gas flow rates.
It should be noted, however, that it is possible to operate the device at significantly lower speeds than predicted by this formula, the optimum speed being dictated primarily by the desired degree of refining.
Claims (12)
1. A process for refining a molten metal selected from the group consisting of magnesium, copper, zinc, tin and lead comprising the steps of:
1. feeding the molten metal into a refining zone;
2. maintaining a protective atmosphere above the surface of said molten metal at a greater than atmospheric pressure, thereby preventing contact of the melt with air or atmospheric moisture;
3. providing a gas injection device submerged in said molten metal comprising (a) a shaft fixedly attached to a vaned rotor at its lower end, (b) a stationary sleeve surrounding said shaft, and (c) a passageway for conveying and discharging refining gas into the molten metal running the length of said gas injection device;
4. introducing a refining gas into the upper end of said passageway under sufficient pressure to be injected into the melt;
5. preheating the refining gas by contact thereof with the hot walls of the passageway, whereby the gas is expanded, before being sub-divided into gas bubbles, to the point where thermal growth of said bubbles in the melt is substantially prevented;
6. directing the preheated refining gas to the vanes of said rotor of said gas injection device;
7. sub-dividing the refining gas into discrete gas bubbles by rotating said vaned rotor at a speed sufficient to create a circulation pattern in the molten metal such that the gas bubbles are transported substantially radially outward with a downward component relative to their points of entry into the melt thereby coming into intimate contact with substantially the entire mass of molten metal in said refining zone, resulting in the removal of dissolved gases and sub-stantially all non-metallic impurities from said melt;
8. withdrawing the spent refining gas and the dissolved gases released by the metal while collect-ing other non-metallic impurities in a slag layer on the surface of the molten metal; and 9. withdrawing the refined molten metal from said refining zone.
2. The process of claim 1 wherein said refining gas is argon.
3. The process of claim 1 wherein said refining gas is nitrogen.
4. The process of claim 1 wherein said refining gas is a mixture of argon and nitrogen.
5. The process of claim 1 wherein said passageway is formed by the outer surface of said shaft and the inner surface of said stationary sleeve.
6 The process of claim 1 wherein said passageway extends axially through said shaft.
7. A process for refining a molten metal selected from the group consisting of magnesium, copper, zinc, tin, and lead comprising the steps of:
1. providing a refining vessel for containing molten metal, said vessel containing at least one refining zone;
2. feeding molten metal into the refining vessel;
3. maintaining a protective atmosphere above the surface of the molten metal at a greater than atmospheric pressure, thereby preventing contact of the molten metal with air or atmosphere moisture;
4. providing at least one gas injection device in said refining vessel submerged in said molten metal comprising (a) a shaft fixedly attached to a vaned rotor at its lower end, (b) a stationary sleeve surrounding said shaft, and (c) a passageway for conveying and discharging refining gas into molten metal running the length of said gas injection device;
5. introducing refining gas into the upper end of said passageway under sufficient pressure to be injected into the melt, the flow rate of said gas being defined by the following formula:
V = W C/N
where:
V = flow rate of gas through each injection device, normal cu.ft./min.
W = the feed rate of molten metal into said refining vessel, lbs/min.
C = the specific refining gas requirement in normal cubic feet/pound metal N = the number of gas injection devices in said refining vessel;
V = W C/N
where:
V = flow rate of gas through each injection device, normal cu.ft./min.
W = the feed rate of molten metal into said refining vessel, lbs/min.
C = the specific refining gas requirement in normal cubic feet/pound metal N = the number of gas injection devices in said refining vessel;
6. sub-dividing the refining gas into discrete gas bubbles by rotating said vaned rotor at a speed sufficient to create a circulation pattern in the molten metal such that the gas bubbles are transported substantially radially outward with a downward component relative to their points of entry into the melt, result-ing in the removal of dissolved gases and substantially all non-metallic impurities from the melt;
7. withdrawing the spent refining gas and the dissolved gases released by the metal while collect-ing other non-metallic impurities in a slag layer on the surface of the molten metal; and 8. withdrawing the refined molten metal from said refining vessel.
8. The process of claim 7 wherein said gas injection device is operated at a speed approximately as defined by the following formula:
R = (300 + 750V + 83r2) /d where:
R = rotational speed of the rotor, RPM;
V = gas flow rate through the injection device, normal cu.ft./min.
r = the ratio of the least cross-sectional dimension of the refining zone to the diameter of the rotor (dimensionless); and d = diameter of the rotor, inches.
R = (300 + 750V + 83r2) /d where:
R = rotational speed of the rotor, RPM;
V = gas flow rate through the injection device, normal cu.ft./min.
r = the ratio of the least cross-sectional dimension of the refining zone to the diameter of the rotor (dimensionless); and d = diameter of the rotor, inches.
9. The process of claim 7 wherein said refining gas is argon.
10, The process of claim 7 wherein said gas inert with respect to the metal is nitrogen.
11. A process for refining molten metal selected from the group consisting of magnesium, copper, zinc, tin, and lead comprising the steps of:
1. feeding molten metal into a refining zone;
2. maintaining a protective atmosphere above the surface of said molten metal at a greater than atmospheric pressure, thereby preventing contact of the melt with air or atmospheric moisture;
3. introducing a refining gas into said melt beneath the surface thereof;
4. preheating said refining gas before being sub-divided into gas bubbles by expanding the gas to the point where thermal growth of said bubbles in the melt is substantially prevented;
5. sub-dividing the refining gas into discrete gas bubbles;
6. creating a circulation pattern in the molten metal such that the bubbles of said refining gas are transported substantially radially outward with a downward component relative to their points of entry into the melt, whereby said gas bubbles come into intimate contact with substantially the entire mass of molten metal in said refining zone, resulting in the removal of dissolved gases and substantially all non-metallic impurities from said melt;
7. withdrawing the spent refining gas containing the dissolved gases released by the metal, while collecting other non-metallic impurities in a a slag layer on the surface of the molten metal; and 8. withdrawing the refined molten metal from said refining zone.
1. feeding molten metal into a refining zone;
2. maintaining a protective atmosphere above the surface of said molten metal at a greater than atmospheric pressure, thereby preventing contact of the melt with air or atmospheric moisture;
3. introducing a refining gas into said melt beneath the surface thereof;
4. preheating said refining gas before being sub-divided into gas bubbles by expanding the gas to the point where thermal growth of said bubbles in the melt is substantially prevented;
5. sub-dividing the refining gas into discrete gas bubbles;
6. creating a circulation pattern in the molten metal such that the bubbles of said refining gas are transported substantially radially outward with a downward component relative to their points of entry into the melt, whereby said gas bubbles come into intimate contact with substantially the entire mass of molten metal in said refining zone, resulting in the removal of dissolved gases and substantially all non-metallic impurities from said melt;
7. withdrawing the spent refining gas containing the dissolved gases released by the metal, while collecting other non-metallic impurities in a a slag layer on the surface of the molten metal; and 8. withdrawing the refined molten metal from said refining zone.
12. The process of claim 11 wherein said re-fining gas with respect to the metal is selected from the group consisting of argon, nitrogen and mixtures thereof.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US05/697,466 US4047938A (en) | 1974-12-23 | 1976-06-18 | Process for refining molten metal |
| US697,466 | 1976-06-18 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1095732A true CA1095732A (en) | 1981-02-17 |
Family
ID=24801232
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA280,820A Expired CA1095732A (en) | 1976-06-18 | 1977-06-17 | Process for refining molten metal |
Country Status (17)
| Country | Link |
|---|---|
| JP (1) | JPS52156105A (en) |
| AU (1) | AU506332B2 (en) |
| BR (1) | BR7703792A (en) |
| CA (1) | CA1095732A (en) |
| CH (1) | CH621365A5 (en) |
| CS (1) | CS212305B2 (en) |
| DE (1) | DE2727142A1 (en) |
| ES (1) | ES459881A1 (en) |
| FR (1) | FR2355079A1 (en) |
| GB (1) | GB1587662A (en) |
| IN (1) | IN146956B (en) |
| IT (1) | IT1078941B (en) |
| MX (1) | MX146591A (en) |
| NO (1) | NO772138L (en) |
| RO (1) | RO75207A (en) |
| SE (1) | SE7706137L (en) |
| YU (1) | YU148677A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3468275D1 (en) * | 1983-08-04 | 1988-02-04 | Alusuisse | Process and device for the introduction of metal to a metal melt |
| BRMU8402794U8 (en) * | 2004-08-27 | 2021-10-26 | Magnesita Insider Refratarios Ltda | Configuration applied to a device for injecting gas and/or gas and powders into liquid metals through a rotating refractory lance |
| RU2619534C2 (en) * | 2015-11-19 | 2017-05-16 | Виталий Евгеньевич Дьяков | Vacuum apparatus for separation tin alloy |
| CN117604311B (en) * | 2024-01-24 | 2024-04-19 | 北京航空航天大学 | Aluminum alloy rotary blowing refining method based on three-channel rotor |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3743263A (en) * | 1971-12-27 | 1973-07-03 | Union Carbide Corp | Apparatus for refining molten aluminum |
-
1977
- 1977-05-25 SE SE7706137A patent/SE7706137L/en unknown
- 1977-06-15 YU YU01486/77A patent/YU148677A/en unknown
- 1977-06-16 DE DE19772727142 patent/DE2727142A1/en active Pending
- 1977-06-16 RO RO7790725A patent/RO75207A/en unknown
- 1977-06-17 CS CS774027A patent/CS212305B2/en unknown
- 1977-06-17 AU AU26185/77A patent/AU506332B2/en not_active Expired
- 1977-06-17 CH CH747477A patent/CH621365A5/en not_active IP Right Cessation
- 1977-06-17 GB GB25357/77A patent/GB1587662A/en not_active Expired
- 1977-06-17 FR FR7718706A patent/FR2355079A1/en active Granted
- 1977-06-17 ES ES459881A patent/ES459881A1/en not_active Expired
- 1977-06-17 JP JP7120577A patent/JPS52156105A/en active Pending
- 1977-06-17 IN IN913/CAL/77A patent/IN146956B/en unknown
- 1977-06-17 BR BR7703792A patent/BR7703792A/en unknown
- 1977-06-17 IT IT49880/77A patent/IT1078941B/en active
- 1977-06-17 NO NO772138A patent/NO772138L/en unknown
- 1977-06-17 MX MX169525A patent/MX146591A/en unknown
- 1977-06-17 CA CA280,820A patent/CA1095732A/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| AU506332B2 (en) | 1979-12-20 |
| YU148677A (en) | 1984-08-31 |
| ES459881A1 (en) | 1978-04-16 |
| GB1587662A (en) | 1981-04-08 |
| JPS52156105A (en) | 1977-12-26 |
| MX146591A (en) | 1982-07-12 |
| IT1078941B (en) | 1985-05-08 |
| IN146956B (en) | 1979-10-20 |
| NO772138L (en) | 1977-12-20 |
| FR2355079A1 (en) | 1978-01-13 |
| BR7703792A (en) | 1978-03-28 |
| SE7706137L (en) | 1977-12-19 |
| DE2727142A1 (en) | 1977-12-22 |
| RO75207A (en) | 1981-04-30 |
| AU2618577A (en) | 1978-12-21 |
| FR2355079B1 (en) | 1983-12-30 |
| CH621365A5 (en) | 1981-01-30 |
| CS212305B2 (en) | 1982-03-26 |
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