CN104145033A - Aluminum refining apparatus and aluminum refining method - Google Patents

Aluminum refining apparatus and aluminum refining method Download PDF

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Publication number
CN104145033A
CN104145033A CN201280069220.9A CN201280069220A CN104145033A CN 104145033 A CN104145033 A CN 104145033A CN 201280069220 A CN201280069220 A CN 201280069220A CN 104145033 A CN104145033 A CN 104145033A
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CN
China
Prior art keywords
cooling
gas
container
stream
aluminium
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CN201280069220.9A
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Chinese (zh)
Inventor
金森照己
与津岳志
林雅章
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Nippon Light Metal Co Ltd
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Nippon Light Metal Co Ltd
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Publication of CN104145033A publication Critical patent/CN104145033A/en
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    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22DCASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D1/00Treatment of fused masses in the ladle or the supply runners before casting
    • B22D1/002Treatment with gases

Abstract

The present invention addresses the problem of providing an aluminum refining apparatus that enables a reduction in refining time and an increase in yield. This aluminum refining apparatus (1) is provided with: a vessel (10) with a bottom that accommodates molten raw aluminum; a heating means (20) for heating the vessel (10); a cooling means (30) for cooling part of the vessel (10); and a primary crystal detaching means (40) for detaching primary crystal particles (PAl) that have crystallized on the inner surface of the vessel (10). The aluminum refining apparatus (1) is characterized in that: the cooling means (30) has a gas flow passage (3a) disposed in such a manner as to surround the vessel; and the gas flow passage (3a) is partitioned into a plurality of divided passages aligned in the vertical direction, and the direction of flow of a cooling gas reverses in the odd-numbered stages of the divided passages from the top, and the even-numbered stages of the divided passages from the top.

Description

Aluminium refining plant and aluminium process for purification
Technical field
The present invention relates to a kind of aluminium refining plant and aluminium process for purification.
Background technology
In patent documentation 1 grade, the aluminium process for purification that utilizes segregated solidification method is disclosed.The disclosed process for purification of patent documentation 1 is (following as the aluminum or aluminum alloy of impurity to containing Fe, Si, peritectic system element and other element unavoidably containing, be called " raw material aluminium ") carry out refining method, it comprises: Local cooling process, in this Local cooling process, separate out containing near the top of container of liquation the cooling primary crystal particle that makes aluminium partly; Crystalline growth process, in this crystalline growth process, peels off to make it to deposit to container bottom on the primary crystal particle of separating out on inner surface of container, and the stores compacting of post-depositional primary crystal particle is made to the crystal growth of aluminium; And molten metal discharge process, in this molten metal discharge process, the liquation that contains impurity is discharged from the container.
In addition, disclose following refining plant in patent documentation 1, using the refining plant as carrying out above-mentioned process for purification, wherein, above-mentioned refining plant comprises: have the container at the end, this has the container at the end to accommodate the liquation of raw material aluminium; Heating unit, this heating unit heats container; Cooling element, a part (following, to be called " crystallization face ") for the internal surface of this cooling element to container is carried out cooling; And primary crystal scraper element, this primary crystal scraper element is peeled off the primary crystal particle of separating out on crystallization face.Cooling element comprises the pipeline contacting with the outside surface of container and make cooling flow with gas cooling with equipment (gas blower etc.) in pipeline, by utilize the cooling heat of capturing tube wall with gas flowing in pipeline, come a part for container cooling.
Prior art document
Patent documentation
Patent documentation 1: Japanese Patent Laid-Open 2002-155322 communique
Summary of the invention
Invent technical problem to be solved
In the refining plant of patent documentation 1, because the cooling temperature with gas is along with rising towards the downstream side of gas flow path, therefore, cooling efficiency can produce difference in upstream side and the downstream side of gas flow path, has the possibility of crystallization amount generation segregation.
Based on such viewpoint, technical problem of the present invention is to provide a kind of crystallization amount to be not easy to occur aluminium refining plant and the aluminium process for purification of segregation.
The technical scheme that technical solution problem adopts
The aluminium refining plant of the present invention that solves such technical problem comprises: have the container at the end, this has the container at the end to accommodate the liquation of raw material aluminium; Heating unit, this heating unit heats said vesse; Cooling element, this cooling element carries out cooling to a part for said vesse; And primary crystal scraper element, this primary crystal scraper element is peeled off the primary crystal particle of separating out on the internal surface of said vesse, it is characterized in that, above-mentioned cooling element has to surround the gas flow path that the mode of said vesse configures, above-mentioned gas stream is divided into multiple streams of cutting apart of arranging on above-below direction, and at least one is above-mentioned cuts apart stream and remaining above-mentioned to cut apart the cooling flow direction with gas in stream contrary.
Although the cooling temperature with gas flowing in respectively cutting apart stream is along with rising towards downstream side from upstream side, but dispose remaining downstream side of cutting apart stream (high temperature side) owing to cutting apart the upstream side (low temperature side) of stream at least one, and the downstream side (high temperature side) of cutting apart stream at least one disposes remaining upstream side of cutting apart stream (low temperature side), therefore, with only make cooling with gas along compared with the mobile situation of direction, the deviation of the height (width) of crystallization face (utilizing cooling element to be cooled to the belt-like zone of the internal surface of the following container of primary crystal point) diminishes, and then the deviation of temperature on crystallization face also diminishes.That is to say, according to aluminium refining plant of the present invention, crystallization amount is not easy to occur segregation.
In the present invention, preferably make at the above-mentioned flow direction of cutting apart the cooling use gas in stream of cutting apart stream and even level from starting from odd-level above-mentioned starting contrary.If like this, the height of crystallization face and temperature are not easy to produce deviation.
The aluminium process for purification of the present invention of technical solution problem comprises: molten metal injection process, in this molten metal injection process, is injected with the liquation of raw material aluminium in the container at the end; Local cooling process, in this Local cooling process, cooling mobile in the multiple gas flow paths that configure in the mode of surrounding said vesse with gas by making, a part for the internal surface of said vesse is cooled to the temperature lower than primary crystal point; Crystal growth process, in this crystal growth process, peels off to make it to deposit to the bottom of said vesse on the primary crystal particle of separating out on the internal surface of said vesse, and the stores compacting of post-depositional primary crystal particle is made to the crystal growth of aluminium; And molten metal discharge process, in this molten metal discharge process, above-mentioned liquation is discharged from the container, it is characterized in that, in above-mentioned Local cooling process, make at least one above-mentionedly cut apart stream above-mentioned to cut apart the cooling flow direction with gas in stream contrary with remaining.
According to the process for purification of aluminium of the present invention, because the height (width) of crystallization face and the deviation of temperature diminish, therefore, crystallization amount is not easy to occur segregation.
In Local cooling process, preferably make at the above-mentioned flow direction of cutting apart the cooling use gas in stream of cutting apart stream and even level from starting from odd-level above-mentioned starting contrary.If like this, further make the segregation of crystallization amount be not easy to produce.
In above-mentioned liquation discharge process, comparatively it is desirable to, by making spinning upside down of said vesse, above-mentioned liquation is discharged from said vesse.If like this, liquation residual in container promptly can be discharged, and can be easily by liquation and crystal separation.
In addition, if pressure when compacting stores lower than 4.0 × 10 4(Pa), there is the inadequate situation of extruding of the liquation that is present in the gap between the interparticle gap of primary crystal or crystallization, and if exceed 1.1 × 10 5(Pa), exist and make the impaired possibility of aluminium refining plant, therefore, in above-mentioned crystal growth process, comparatively it is desirable to, with 4.0 × 10 4~1.1 × 10 5(Pa) pressure, by above-mentioned stores compacting.
In the situation that containing peritectic system element as impurity, carry out the sepn process of peritectic system element: in this peritectic system element sepn process, at least one party in boron and boron-containing compound is added in the liquation of raw material aluminium, and be blown into the gas that contains oxidizing gas, and the peritectic system element floating on the surface of above-mentioned liquation or peritectic system element compound are removed, in above-mentioned molten metal injection process, the liquation obtaining is injected to said vesse in the sepn process of above-mentioned peritectic system element.If can reduce like this, the amount of the peritectic system element in liquation.
Invention effect
According to the present invention, make crystallization amount be not easy to occur segregation.
Brief description of the drawings
Fig. 1 is the sectional view that represents the aluminium refining plant of embodiment of the present invention.
Fig. 2 is the X1-X1 sectional view of Fig. 1.
Fig. 3 is the partial enlarged drawing of Fig. 1.
Fig. 4 (a) is the partial enlarged drawing of ring-type stream portion, and Fig. 4 (b) is the side-view of ring-type stream portion.
Fig. 5 (a) is the Y1-Y1 sectional view of Fig. 2, and Fig. 4 (b) is the Y2-Y2 sectional view of Fig. 2, and Fig. 4 (c) is the Y3-Y3 sectional view of Fig. 2.
Fig. 6 is the X2-X2 sectional view of Fig. 1.
Fig. 7 is the sectional view that represents pretreating device.
Fig. 8 is the sectional view that represents the crystalline condition of primary crystal particle.
Fig. 9 is the sectional view that represents the aluminium refining plant of comparative example.
Embodiment
The aluminium process for purification of embodiments of the present invention is implemented in order to obtain raffinal from the raw material aluminium liquation of (containing Fe, Si, peritectic system element and other element unavoidably the containing raw material aluminium as impurity).The aluminium process for purification of present embodiment is to utilize the pretreating device 2 shown in the aluminium refining plant 1 shown in Fig. 1 and Fig. 7 to carry out.
First, the structure of aluminium refining plant 1 is elaborated.
Aluminium refining plant 1 is the device that the Steppecd crystallization by utilizing segregation phenomena makes the crystal growth of aluminium, and as shown in Figure 1, it comprises: container 10, the liquation of this container 10 to raw material aluminium (is called " raw material liquation M below, 1") accommodate; Heating unit 20, this heating unit 20 heats container 10; Cooling element 30, a part (crystallization face) for the internal surface of this cooling element 30 to container 10 is carried out cooling; Primary crystal scraper element 40, this primary crystal scraper element 40 makes the primary crystal particle P separating out on the internal surface of container 10 alpeel off and thermal insulation barriers 50, this thermal insulation barriers 50 covers container 10.
Container 10 includes the inner side container 11 of round-ended cylinder shape and covers the outside container 12 that has round-ended cylinder shape of inner side container 11.Inner side container 11 is made up of heat-stable materials such as graphite, and outside container 12 is made up of stainless steel and other metal materials.The internal surface of outside container 12 contacts with the outside surface of inner side container 11.In addition, lid (not shown) is installed on the opening end of outside container 12.
Heating unit 20 is configured in container 10 around.The heating unit 20 of present embodiment comprises: lower heater 21, and this lower heater 21 heats the bottom of container 10; The middle part well heater 22,22 of multistage (being in the present embodiment four sections) ..., these middle part well heaters 22,22 ... bottom from container 10 to the region at the middle part of short transverse is heated; And upper portion heater 23, this upper portion heater 23 heats the top of container 10.Lower heater 21, multiple middle parts well heater 22,22 ... and upper portion heater 23 is independent mutually, and can carry out respectively temperature control.
Lower heater 21 configures in the mode of covering container 10 bottoms.Middle part well heater 22,22 ... the mode of container 10 being surrounded with the region between lower heater 21 and cooling element 30 configures.The mode that upper portion heater 23 surrounds container 10 with the region of the upside at cooling element 30 configures.
Cooling element 30 comprises: gas flow path 3a, and the cooling gas of using can flow in above-mentioned gas stream 3a; And not shown cooling such as, with equipment (gas blower etc.), this is cooling is used for making coolingly flowing at gas flow path 3a with gas with equipment.
As shown in Figure 2, the cooling element 30 of present embodiment comprises: ring-type stream portion 31, and this ring-type stream portion 31 is along the outside surface configuration of container 10; The first gas supply part 32 and the second gas supply part 33, above-mentioned the first gas supply part 32 and the second gas supply part 33 never illustrated suction opening extend to ring-type stream portion 31; And exhaust portion 34, this exhaust portion 34 extends to not shown venting port from ring-type stream portion 31.Gas flow path 3a (with reference to Fig. 1) is formed on the inner side (internal space) of ring-type stream portion 31, the first gas supply part 32, the second gas supply part 33 and exhaust portion 34.
Ring-type stream portion 31 configures in the mode of surrounding container 10.Ring-type stream portion 31 is made up of stainless material.
As shown in Figure 3, ring-type stream portion 31 comprises the partition wall 315 that separate up and down on the rectangular shell in cross section (internal perisporium 311, periphery wall 312, upper wall 313 and lower wall 314) and the edge, internal space by above-mentioned shell.,, in ring-type stream portion 31, gas flow path is divided on above-below direction multiple stream 31a~31f of cutting apart side by side.In addition, in the present embodiment, show and cut apart the situation that the cross-sectional shape of stream 31a~31f is rectangle, but be not intended to limit the cross-sectional shape of cutting apart stream.Though not shown, the cross-sectional shape of cutting apart stream can be also circular.In this case, respectively cut apart stream as long as utilize the rounded stainless steel tube in cross section to form.
Internal perisporium 311 be with the periphery (outside container 12) of container 10 across relative with gap position, periphery wall 312 is across relative position, compartment of terrain with internal perisporium 311.Upper wall 313 is positions that the top of internal perisporium 311 is connected with the top of periphery wall 312, and lower wall 314 is positions that the bottom of internal perisporium 311 is connected with the bottom of periphery wall 312.In addition also can make, the periphery butt of internal perisporium 311 and container 10.
Partition wall 315 is for gas flow path (internal space of=ring-type stream portion 31) is divided into multiple partition walls of cutting apart stream 31a~31f, and they are multiple along being arranged side by side across compartment of terrain up and down.The quantity of partition wall 315 does not limit, but comparatively it is desirable to, and the quantity of partition wall 315 is set as to odd number, so that the Segmentation Number of gas flow path is even number.
In ring-type stream portion 31, be formed with relative with the outside surface of container 10 multiple direct cooling with opening 3b, 3b ...
Direct cooling be that it is made up of the circular hole of running through internal perisporium 311 in order directly to blow to the outside surface of container 10 and the member that forms by cooling with gas with opening 3b.The direct cooling opening end by container 10 1 sides with opening 3b is relative across compartment of terrain with the outside surface of container 10.Direct cooling opening diameter while being made as circular hole with opening 3b is for example preferably set as to 1~7mm left and right.In addition the direct cooling shape with opening 3b is not limited.Though not shown, also can will be polygonal hole or slotted hole as the direct cooling opening 3b that uses, can also using the week at container 10 upwards continuous slit as the direct cooling opening 3b that uses.
Direct cooling with opening 3b and the superiors cut apart stream 31a and the undermost stream 31b~31e of cutting apart of cutting apart outside stream 31f is communicated with., be coolingly communicated with opening 3b with direct respectively at the stream 31b~31e of cutting apart in stage casing, the superiors cut apart stream 31a and the undermost stream 31f of cutting apart is not coolingly communicated with opening 3b with direct.
As shown in Fig. 4 (a), in cutting apart in stream 31b of stage casing, along cooling flow direction with gas (container 10 circumferentially) across compartment of terrain and multiple direct cooling use opening 3b, 3b ... be communicated with.In addition,, though not shown, other the stream 31c~31e of cutting apart is also like this.
The ring-type stream portion 31 of present embodiment have along the cooling flow direction with gas (container 10 circumferentially) across equal intervals arrange multiple direct cooled region 3c, 3c ..., multiple direct cooled region 3c, 3c ... be formed with respectively at least one direct cooling opening 3b that uses.As shown in Fig. 4 (b), in the present embodiment, show the direct cooling situation with opening 3b in each direct cooled region 3c configuration eight (cutting apart each two of stream 31b~31e), but be not intended to limit direct cooling number and configuration with opening 3b.In addition, the arrow shown in Fig. 4 (b) represents the cooling flow direction with gas.
The direct cooling port area with opening 3b and the direct cooling quantity with opening 3b can suitably be set, but in order heating unit 20 (with reference to Fig. 1) not to be caused to unnecessary load, comparatively it is desirable to, the surface-area of internal perisporium 311 area of the face relative with container 10 (in the ring-type stream portion 31) is made as P, by direct cooling with opening 3b, 3b ... the aggregate value of port area while being made as Q, the value that makes Q/ (P+Q) is below 0.1.Particularly, be below 0.02 if make the value of Q/ (P+Q), owing to can heating unit 20 not being caused to unnecessary load in the cooling efficiency that improves crystallization face, therefore comparatively desirable.In addition, in the case of being formed by circular tubing ring-type stream portion 31, in the perisporium of tubing, to be positioned at than the vertical surface of the kernel of section through tubing be more internal perisporium by the part (being the part cylindraceous after being divided into two) of container 10 1 sides.
As shown in Fig. 5 (a), the first gas supply part 32 has: the first air supply header 32a, and this first air supply header 32a extends from suction opening (not shown); The first air feed collector 32b, this first air feed collector 32b is connected with the downstream end of the first air supply header 32a; And multiple (being in the present embodiment three) first gas manifold 32c, 32c, 32c, these first gas manifolds 32a, 32a, 32a extend to ring-type stream portion 31 from the first air feed collector 32b.The first air feed collector 32b is the hollow member that is configured in the fork position of gas flow path 3a.Cut apart stream 31a, 31c, the 31e (the superiors cut apart stream 31a, from the 3rd layer of upper beginning cut apart stream 31c and cut apart stream 31e from the layer 5 of upper beginning) of the internal space of the first gas manifold 32c, 32c, 32c and the odd-level from upper beginning are communicated with.That is, the gas flow path 3a in the first gas supply part 32 is bifurcated into after three, with cut apart stream 31a, 31c, 31e is communicated with.In addition, the arrow in Fig. 5 represents the cooling flow direction with gas.
As shown in Figure 6, be provided with guide wall 316 in the connection portion of ring-type stream portion 31 and the first gas supply part 32.Guide wall 316 is that it is arranged on the inside of ring-type stream portion 31 for making the cooling gas of using that imports ring-type stream portion 31 from the first gas supply part 32 along the mobile partition wall of a direction (in the counter clockwise direction of Fig. 5).
As shown in Fig. 5 (b), the second gas supply part 33 comprises: the second air supply header 33a, and this second air supply header 33a extends from suction opening (not shown); The second air feed collector 33b, this second air feed collector 33b is connected with the downstream end of the second air supply header 33a; And multiple (being in the present embodiment three) second gas manifold 33c, 33c, 33c extend to ring-type stream portion 31 from the second air feed collector 33b.The second air feed collector 32b is the hollow member that is configured in the fork position of gas flow path 3a.The internal space of the second gas manifold 33c, 33c, 33c and the even level from upper beginning cut apart stream 31b, 31d, 31f (from the second layer of upper beginning cut apart stream 31b, from the 4th layer of upper beginning cut apart stream 31d and cut apart stream 31f from the layer 6 (orlop) of upper beginning) be communicated with.That is, the gas flow path 3a in the second gas supply part 33 is bifurcated into after three, with cut apart stream 31b, 31d, 31f is communicated with.
Though not shown, be provided with guide wall in the connection portion of ring-type stream portion 31 and the second gas supply part 33.This guide wall is that it is arranged on the inside of ring-type stream portion 31 for making the cooling gas of using that imports ring-type stream portion 31 from the second gas supply part 33 along a partition wall that direction is mobile.In addition, in the present embodiment, so that cooling with gas the odd-level from starting cut apart stream 31a, 31c, 31e with and the above-mentioned mode that flow direction in stream 31b, 31d, 31f is contrary of cutting apart of cutting apart stream 31a, 31c, even level that 31e is adjacent guide wall is set.
As shown in Fig. 5 (c), exhaust portion 34 comprises: exhaust branch pipe 34a, 34a ..., this exhaust branch pipe 34a, 34a ... extend from ring-type stream portion 31; Exhaust header 34b, this exhaust header 34b and exhaust branch pipe 34a, 34a ... downstream end connect; And exhaust-gas receiver 34c, this exhaust-gas receiver 34c extends to not shown venting port from exhaust header 34b.Exhaust header 34b be configured in exhaust branch pipe 34a, 34a ... the hollow member at the position of confluxing.Exhaust branch pipe 34a, 34a ... internal space with cut apart stream 31a~31f and be communicated with.
As shown in Figure 1, primary crystal scraper element 40 comprises: support rod 41; The discoideus press section 42 of peeling off, this peels off press section 42 and is arranged on the lower end of support rod 41; And not shown propulsion source, this propulsion source makes support rod 41 and peels off press section 42 to move up and down.Support rod 41 and peel off press section 42 and made by heat-stable materials such as graphite.
Peel off press section 42 and there is the external diameter identical with the internal diameter of container 10, and slide on the inner peripheral surface of container 10.On press section 42, be formed with liquid-through hole 42a peeling off.Liquid-through hole 42a is along running through up and down the through hole of peeling off press section 42.
Thermal insulation barriers 50 is the members that improve the heat insulation effect of container 10, and it configures in the mode of surrounding heating unit 20 and ring-type stream portion 31.Thermal insulation barriers 50 is made up of the material with resistivity against fire and thermal insulation.
Then,, with reference to Fig. 7, the structure of pretreating device 2 is elaborated.
Pretreating device 2 is (below, to be called " raw material liquation M to containing peritectic system element as the liquation of the raw material aluminium of impurity 0") device of processing that the amount of peritectic system element is reduced, it comprises: crucible 60, this crucible 60 is to raw material liquation M 0keep; Boron adds element 70, and this boron adds element 70 and adds at least one party in boron and boron-containing compound to raw material liquation M in crucible 60 0in; And gas is blown into element 80, this gas is blown into element 80 gas that contains oxidizing gas is blown into the raw material liquation M in crucible 60 0in.
Crucible 60 is the containers that have round-ended cylinder shape.The internal surface of crucible 60 is covered by heat-stable materials such as graphite, unsetting refractory body, refractory brick.
Boron adds element 70 and comprises: storage vessel 71, in this storage vessel 71, at least one party in boron and boron-containing compound is stored; Drop into pipe 72, this input pipe 72 extends towards crucible 60 from the bottom of storage vessel 71; And open and close valve 73, this open and close valve 73 is opened input pipe 72, close.
Gas is blown into element 80 and comprises: swivel bearing pipe 81; Agitating vane 82, this agitating vane 82 is arranged on the lower end of swivel bearing pipe 81; Propulsion source 83, this propulsion source 83 is connected with the upper end of swivel bearing pipe 81; Swivel joint 84, this swivel joint 84 is folded between propulsion source 83 and swivel bearing pipe 81; Gas supply source 85, this gas supply source 85 is accumulated the gas that contains oxidizing gas (atmosphere and carbonic acid gas etc.); Gas supply pipe 86, this gas supply pipe 86 extends to swivel joint 84 from gas supply source 85; And pressure regulator valve 87, this pressure regulator valve 87 is arranged at gas supply pipe 86.
Swivel bearing pipe 81 and agitating vane 82 are made up of heat-stable materials such as graphite.On agitating vane 82, be formed with the gas discharge outlet 82a being communicated with swivel bearing pipe 81.
Propulsion source 83 is made up of electric motor of the forward and reverse rotation of speed of rotation that can turn with per minute 0~1200 etc.The output shaft of propulsion source 83 is connected with the upper end of swivel bearing pipe 81 via swivel joint 84.In addition, in the time making swivel bearing pipe 81 and agitating vane 82 carry out forward and reverse rotation, can be not to raw material liquation M 0surface carry out in the situation of significantly disturbance, to raw material liquation M 0stir.
Gas supply source 85 is via swivel joint 84 and gas supply pipe 86 and be communicated with swivel bearing pipe 81.The gas that contains oxidizing gas process gas supply pipe 86, swivel joint 84 and swivel bearing pipe 81 in gas supply source 85, and be blown into raw material liquation M from gas discharge outlet 82a 0in.The bubble of the gas that contains oxidizing gas spreads in being stirred blade 82 miniaturizations.
Then, the aluminium process for purification that utilizes aluminium refining plant 1 (with reference to Fig. 1) and pretreating device 2 (with reference to Fig. 7) is described.In addition, in the present embodiment, show and carry out refining situation to containing Fe, Si, peritectic system element and other element unavoidably containing as the raw material aluminium of impurity.
In the aluminium process for purification of present embodiment, comprise the sepn process of peritectic system element, molten metal injection process, Local cooling process, crystal growth process and molten metal discharge process.In addition, the sepn process of peritectic system element is carried out in pretreating device 2, and Local cooling process, crystal growth process and molten metal discharge process are carried out in aluminium refining plant 1.
As shown in Figure 7, the sepn process of peritectic system element is to add at least one party in boron and boron-containing compound to raw material liquation M 0in (containing Fe, Si, peritectic system element and other element unavoidably the containing liquation as the raw material aluminium of impurity), and be blown into the gas that contains oxidizing gas, and will be at raw material liquation M 0surface on the process removed of the peritectic system element that floats or peritectic system element compound.
In the sepn process of peritectic system element, first, by the raw material liquation M of specified amount 0inject crucible 60.Then, utilize boron to add element 70 and add at least one party in boron and boron-containing compound to raw material liquation M in crucible 60 0in, then with regulation speed of rotation (for example per minute 400 turns) make the forward and reverse rotation of agitating vane 82 in, from gas discharge outlet 82a to raw material liquation M 0be blown into the gas that contains oxidizing gas.Continuing to be blown into the gas that contains oxidizing gas after the specified time, stop being blown into the gas that contains oxidizing gas, then, will be at raw material liquation M 0surface on the peritectic system element boron compound absorption slag that floats pick up, separate and discharge.After the sepn process of peritectic system element, just can obtain the raw material liquation M containing peritectic system element hardly 1.
Be that 800 (mm), internal height are in the crucible 60 of 1000 (mm), to inject the raw material liquation 1.0 (t) of the V (vanadium) of the Ti (titanium), the 50 quality ppm that contain 30 quality ppm at internal diameter, and add after the boron mother alloy of 1.3 (kg), be blown into the flow of 80 (l/min) gas that contains oxidizing gas and reach 20 minutes, thereby make the Ti in aluminum melt become 1 quality ppm, V becomes 1 quality ppm.Incidentally, carrying out being blown into argon gas to replace after the comparative experiments of the gas that contains oxidizing gas, the Ti in aluminum melt becomes 7 quality ppm, and V becomes 23 quality ppm.
In addition, the removal speed of the Ti in above-mentioned test and V is represented by the primary first-order equation speed type shown in following formula 1, removes velocity coefficient k as shown in table 1 below.
C=C 0e -ktformula 1
Wherein:
C: the concentration (quality ppm) after time t minute
C 0: starting point concentration (quality ppm)
K: remove velocity coefficient
T: reaction times (min)
Table 1
Be blown into gaseous species The removal velocity coefficient k of Ti The removal velocity coefficient k of V
The gas that contains oxidizing gas 0.18 0.22
Argon gas 0.07 0.04
As shown in Table 1, the removal velocity coefficient k of the Ti while being blown into the gas that contains oxidizing gas is 2.6 times while being blown into argon gas, and the removal velocity coefficient k of the V while being blown into the gas that contains oxidizing gas is 5.5 times while being blown into argon gas.No matter be Ti or V, the removal velocity coefficient k while being blown into the gas that contains oxidizing gas is all large when being blown into argon gas, and therefore, for example, Ti concentration and V concentration after (20 minutes) becomes low-down value at the appointed time.
Obtaining the raw material liquation M containing peritectic system element hardly 1afterwards, by raw material liquation M 1the container 10 (molten metal injection process) that injects aluminium refining plant 1 carries out Local cooling process, crystal growth process and molten metal discharge process in the aluminium refining plant 1 shown in Fig. 1.
In addition, molten metal injection process is carried out under the state that primary crystal scraper element 40 is pulled down.Raw material liquation M1 is being injected the rear installation of container 10 by primary crystal scraper element 40.In addition, container 10 heats by heating unit 20.Local cooling process and crystal growth process are carried out under argon gas atmosphere.
Local cooling process is cooling mobile in gas flow path 3a with gas by making, and a part for the internal surface of container 10 (following, to be called " crystallization face ") is cooled to the process lower than the temperature of primary crystal point.In Local cooling process, as shown in Figure 3, cut apart in stream 3b~3e cooling at least a portion with gas of flowing via direct cooling with opening 3b, 3b ... and directly contact with the outside surface of container 10.
As shown in Figures 5 and 6, cooling being supplied to via the first gas supply part 32 and the second gas supply part 33 with gas cut apart stream 31a~31f in ring-type stream portion 31, cutting apart in stream 31a~31f after circulation, discharges via exhaust portion 34.When making coolingly to cut apart in stream 31a~31f while flowing with gas, indirectly container 10 is carried out via the internal perisporium 311 (with reference to Fig. 3) of ring-type stream portion 31 cooling, utilize simultaneously from direct cooling with opening 3b, 3b ... the cooling of periphery that blows to container 10 directly carries out cooling to container 10 with gas.
In addition, interior mobile cooling being bifurcated into gas after three strands of the first gas supply part 32, be supplied to and cut apart stream 31a, 31c, 31e (with reference to Fig. 5 (a)), circulate along left-handed rotation (counterclockwise) cutting apart in stream 31a, 31c, 31e, and interior mobile cooling being bifurcated into gas after three strands of the second gas supply part 33, be supplied to and cut apart stream 31b, 31d, 31f (with reference to Fig. 5 (b)), circulate cutting apart in stream 31b, 31d, 31f along dextrad rotation (clockwise).; one cut apart stream (from the odd-level of upper beginning cut apart stream 31a, 31c, 31e) with and this cut apart the cutting apart in stream (from the even level of upper beginning cut apart stream 31b, 31d, 31f) of adjacent other of stream, the cooling flow direction with gas is contrary.(with reference to Fig. 4 (b)).If like this, cutting apart in stream 31a~31f, cut apart stream 31a, 31c, upstream side (low temperature side) and remaining of 31e are cut apart stream 31b, 31d, the downstream side (high temperature side) of 31f is adjacent, cut apart stream 31a, 31c, downstream side (high temperature side) and remaining of 31e are cut apart stream 31b, 31d, the upstream side (low temperature side) of 31f is adjacent, therefore, with make cooling with gas only along compared with the mobile situation of direction, crystallization face is (in container 10, be cooled to the following belt-like zone of primary crystal point) the deviation of height (width) diminish, and then the deviation of temperature in crystallization face diminishes., in the all-round scope of crystallization face, temperature can become even.
Then, make if continue cooling with gas flow, the belt-like zone (crystallization face) of the internal surface of the container 10 corresponding with ring-type stream portion 31 just temperature can maintain the temperature range between eutectic point and primary crystal point.If the temperature of crystallization face lower than primary crystal point, is separated out the primary crystal particle P of aluminium on crystallization face al.In addition, use heating unit 20 suitably to heat container 10, to avoid raw material liquation M 1solidify at position outside crystallization face.
On crystallization face, separate out primary crystal particle P alafterwards, carry out crystal growth process.
As shown in Figure 1, crystal growth process is the primary crystal particle P separating out on crystallization face (internal surface of container 10) alpeel off to make it to be deposited on the bottom of container 10, and by post-depositional primary crystal particle P alstores C alcompacting makes the process of the crystal growth of aluminium.Repeatedly carry out crystal growth process, until stores C alapproach the lower edge of crystallization face.During carrying out crystal growth process, also continue to use cooling gas to carry out cooling to crystallization face.
By primary crystal particle P alwhile peeling off, as long as the press section 42 of peeling off of primary crystal scraper element 40 is moved up and down periodically near crystallization face.Make to peel off press section 42 from the upside of crystallization face (ring-type stream portion 31) down side shifting or make peel off press section 42 from the downside of crystallization face upward when side shifting, primary crystal particle P aljust can be stripped from, and be deposited on the bottom of container 10.In the time making to peel off press section 42 and move up and down, because crystallization face can be upgraded periodically, therefore, crystallization velocity can not reduce.In addition, the primary crystal particle P after being stripped from ala part floating on raw material liquation M 1in process in carry out crystal growth, be then deposited on the bottom of container 10.Owing to peeling off being communicated with via liquid-through hole 42a up and down of press section 42, therefore, make to peel off press section 42 towards below while moving, peel off the raw material liquation M of the downside of press section 42 1can flow into and peel off the upside of press section 42 via liquid-through hole 42a, make to peel off press section 42 towards above while moving, peel off the raw material liquation M of the upside of press section 42 1can flow into the downside of peeling off press section 42 via liquid-through hole 42a.
After peeling off press section 42 and starting to move up and down through the specified time (for example, about 3~30 minutes) afterwards, make to peel off press section 42 and move towards below, to being deposited on the stores C of primary crystal particle of container 10 bottoms al(aluminium crystal) pushes, with by stores C alcompacting.Use peel off press section 42 from above to stores C alwhen extruding, raw material liquation M 1can ooze out from the gap between the interparticle gap of primary crystal or crystal, and be discharged to via liquid-through hole 42a the raw material liquation M that peels off press section 42 upsides 1.
By stores C alwhen compacting, lower heater 21 and middle part well heater 22,22 ... in, be positioned at part (crush-zone) after new accumulation well heater around and suitably heat.Like this, from stores C allower layer part towards upper layer part or from stores C alperipheral part can carry out dissolving again, the crystallization again of aluminium crystal towards center position.In addition, utilize and peel off the extruding of press section 42 and the heating from the peripheral part of container 10, the impure liquid that contains impurity is moved towards top from bottom, and move towards central part from peripheral part.
In addition, if to stores C alpressure while carrying out compacting is lower than 4.0 × 10 4(Pa), there is the raw material liquation M that is present in the interparticle gap of primary crystal or the gap of crystal 1extrude inadequate possibility, on the other hand, if exceed 1.1 × 10 5(Pa), there is the possibility that makes aluminium refining plant 1 impaired, and have the possibility on the liquid-through hole 42a that crystal is cemented in peel off press section 42, therefore, comparatively it is desirable to, with 4.0 × 10 4~1.1 × 10 5(Pa) pressure, by stores C alcompacting.
At crystal (the stores C of aluminium al) upper surface arrive near the lower edge of crystallization face after, stop coolingly with the flowing of gas, and by support rod 41 and peel off press section 42 and extract from container 10, and be transferred to molten metal and discharge operation.
Molten metal discharge process is by residual raw material liquation M 1the process of discharging from container 10.Though not shown, in the present embodiment, by the element that fascinates, container 10 is fascinated, and make spinning upside down of container 10, thereby by raw material liquation M 1discharge from container 10.At stores C alcentral part and upper layer part in, at stores C alinner side (gap between crystal) also can residually contain the raw material liquation M of impurity 1if maintain the state spinning upside down of container 10, except remaining in stores C althe raw material liquation M in outside 1outside, remain in stores C althe raw material liquation M of inner side (gap of crystal) 1also can under the effect of gravity, promptly discharge from container 10, consequently, make the raw material liquation M of the impurity that contains high density 1crystal (stores C with highly purified aluminium al) separate.Due to stores C alwith the close contact such as the bottom surface of container 10, therefore, even if make the container 10 not landing at once of overturning also, if but upset exceedes 5 minutes, there is stores C althe situation of landing, therefore, comparatively it is desirable to, and is set in the flip-flop transition of container 10 in 5 minutes, then makes it promptly be returned to original position.
Container 10 is returned to behind original position, just complete the solid-liquid separation of aluminium.In addition also can pass through the raw material liquation M in container 10, 1aspirate, by stores C alwith raw material liquation M 1separate.
Then, by stores C alplace cooling number hour, and by stores C altake out from container 10, be used as product and store in a warehouse.
If aluminium is refined according to above-mentioned steps, although at stores C alcentral part or its top near remain slightly again the impure liquid after dissolving, but at other parts place, can obtain Fe, Si etc. are suppressed to the raffinal of not enough number quality ppm.
As mentioned above, according to aluminium refining plant 1, because utilization is peeled off press section 42 to raw material liquation M 1stir, and be accompanied by stores C alextruding (compacting), and the impurity between crystal is extruded from liquid-through hole 42a towards top, therefore, the purity of aluminium also becomes high purity.In addition, due to the raw material liquation M that contains impurity 1can be raised stores C althe gap on top, therefore, can discharge simply.In addition, according to aluminium refining plant 1, carry out primary crystal particle P owing to peeling off press section 42 with one alpeel off and stores C alcompacting, therefore, it is very simple that structure and operation become, the risk of fault also reduces.
In addition,, according to aluminium refining plant 1, because the outside surface of container 10 is exposed to gas flow path 3a (cutting apart stream 31b~31e), therefore, coolingly directly contact with the outside surface of container 10 with gas.; according to aluminium refining plant 1; due to can via direct cooling with opening 3b, 3b ... directly capture the heat of container 10; therefore; with do not arrange direct cooling with opening 3b, 3b ... situation compare; can improve cooling efficiency, and then shorten crystallization face is cooled to and (is cooled to primary crystal particle P lower than the needed time of temperature of primary crystal point altime before separating out).In addition, if cooling efficiency improves, even if the in the situation that of heating near to crystallization face, also can obtain larger crystallization face, and the temperature of crystallization face is also not easy to rise (as being not easy to narrow lower than the region of primary crystal point), therefore crystallization amount is not easy to reduce.
At the container 10 that uses internal diameter 560mm, high 1300mm, after confirming the test of the direct cooling effect with opening 3b, not arranging in the direct cooling example with opening 3b, in Local cooling process from beginning to cool down the primary crystal particle P of aluminium alstarting to separate out needs 2 hours, in contrast, be provided with direct cooling with being 0.6 hour in the example of opening 3b.In addition, not arranging in the direct cooling example with opening 3b, after beginning to cool down in Local cooling process, in 12 hours, can make 55% of raw material liquation solidify, but being provided with in the direct cooling example with opening 3b, after beginning to cool down, in 9 hours, just can make 60% of raw material liquation solidify, and in 12 hours, can make 70% of raw material liquation solidify.In addition, direct cooling be the circular hole of diameter 5mm with opening 3b, directly coolingly cut apart stream 31b~31e with opening 3b uniformly distributing in stage casing by 100.In addition, in each section, direct cooling with the circumferentially roughly equally spaced configuration of opening 3b edge by 25.The surface-area of the internal perisporium 311 of ring-type stream portion 31 is being made as to P, by direct cooling with opening 3b, 3b ... the aggregate value of port area be made as in the situation of Q, the value of Q/ (P+Q) is 0.006 (0.6%).
Like this, if the direct cooling opening 3b that uses is set, can shortens cycle time and improve yield rate.
In addition, according to aluminium refining plant 1, owing to the gas flow path 3a in ring-type stream portion 31 being divided into multiple stream 31a~31f of cutting apart, make cooling with gas cut apart stream 31a, 31c, 31e and and cut apart adjacent other of stream 31a, 31c, 31e and cut apart stream 31b, 31d, the flow direction in 31f is contrary, therefore, the deviation of the temperature of crystallization face diminishes, and consequently, is not easy to occur the segregation (with reference to Fig. 8) of crystallization amount.
Particularly, in the present embodiment, what gas flow path 3a was divided into even level cuts apart stream 31a~31f, and make cooling with gas the odd-level from starting cut apart stream 31a, 31c, 31e and even level from beginning to cut apart flow direction in stream 31b, 31d, 31f contrary, therefore, can be by balancedly cooling the all-round scope of crystallization face, thus can make the segregation of crystallization amount further reduce.In addition, in the present embodiment, cut apart stream 31b~31e and the direct cooling opening 3b that uses, 3b, be communicated with, therefore, cutting apart stream 31c, the upstream side (low temperature side) of 31e is located, from cutting apart stream 31c, the low temperature that 31e blows out cooling with gas with from cutting apart stream 31b, the cooling of the high temperature that 31d blows out mixes in the space between container 10 and ring-type stream portion 31 with gas, on the other hand, cutting apart stream 31b, the upstream side (low temperature side) of 31d is located, from cutting apart stream 31c, the high temperature that 31e blows out cooling with gas with from cutting apart stream 31b, the cooling of the low temperature that 31d blows out mixes in the space between container 10 and ring-type stream portion 31 with gas, thereby, temperature distribution is not easy to produce deflection, and then can make the segregation of crystallization amount less.
According to aluminium refining plant 1, due to make the superiors cut apart stream 31a and undermost cut apart outside stream 31f cut apart stream 31b~31e and direct cooling with opening 3b, 3b ... be communicated with, therefore, the temperature that can be suppressed in the upper and lower region of crystallization face declines, consequently, can reduce the suffered load of heating unit 20.
According to aluminium refining plant 1, set along the cooling flow direction with gas across equal intervals arrange multiple direct cooled region 3c, 3c ..., directly cooled region 3c, 3c ... form respectively at least one direct cooling opening 3b that uses.If like this, due to direct cooling with opening 3b, 3b ... configuration regularly, therefore, the deviation of the temperature of crystallization face diminishes, and consequently, is not easy to occur the segregation of crystallization amount.
In addition, in the present embodiment, show make the superiors cut apart stream 31a and cut apart stream 31b~31e and direct cooling situation about with opening 3b being communicated with outside stream 31f undermost cutting apart, but also can make the superiors cut apart stream 31a and the undermost stream 31f of cutting apart is coolingly communicated with opening 3b with direct.If like this, although there is the possibility that the suffered load of heating unit 20 is increased, also can improve cooling efficiency in rising wood and the lower edge of crystallization face.
In addition, in the present embodiment, show the gas flow path 3a in ring-type stream portion 31 is divided into multiple stream 31a~31f of cutting apart, and make cooling with gas cut apart stream 31a, 31c, 31e with and cut apart the situation that flow direction in stream 31b, 31d, 31f is contrary of cutting apart of adjacent other of stream 31a, 31c, 31e, but do not need to make the reverse quantity of cutting apart stream identical.Though not shown, as long as to cut apart flow direction in stream contrary with remaining to make at least one cut apart stream, with make cooling with gas only along compared with the mobile situation of direction, the deviation of the height (width) of crystallization face diminishes, and then the deviation of temperature on crystallization face also diminishes.In addition, in the present embodiment, show make the cooling flow direction with gas be along left-handed rotation cut apart stream with for along the right handed situation of cutting apart stream alternately configured, but may not need alternately configured.For example also gas flow path 3a can be divided into four, make cooling with gas be along left-handed rotation (along dextrad rotation) at the superiors and the undermost flow direction of cutting apart in stream, and make cooling with gas be to rotate (along left-handed rotation) along dextrad at the flow direction of cutting apart in stream of middle two sections.
Embodiment
Use the container 10 of internal diameter 560mm, height 1300mm to make the cooling test of cutting apart the effect confirmation when contrary of flow direction in stream 31b, 31d, 31f of cutting apart stream 31a, 31c, 31e and even level from beginning at the odd-level from starting with gas.In addition, the direct cooling opening 3b that uses is not set.
In comparative example, use the aluminium refining plant 1 ' shown in Fig. 9, be a direction by the cooling flow direction unification with gas.In addition, the cooling gas of using, via gas supply part 32 ', is supplied to the multiple streams of cutting apart in ring-type stream portion 31, respectively cutting apart stream after equidirectional circulation, discharges via exhaust portion 34 '.
In addition, embodiment's cuts apart in stream 31a~31f, by cooling with gas being made as along left-handed rotation from the flow direction of cutting apart in stream 31a, 31c, 31e of odd-level starting, be made as along dextrad and rotate at the flow direction in stream 31b, 31d, 31f cut apart of the even level from beginning with gas cooling.The cooling flow with gas of the time per unit of embodiment and comparative example does not have difference.Incidentally, being supplied to the cooling temperature with gas of cutting apart stream 31a~31f is about 25 DEG C.
Be that 250 (ppm), Si concentration are raw material liquation 580 (kg) the injection container 10 of 200 (ppm) by Fe concentration, and carry out Local cooling process under argon gas atmosphere after, from starting the primary crystal particle P of Local cooling process to aluminium alstart to separate out the needed time, in embodiment, comparative example, be 2 hours.
In embodiment, comparative example, all carry out crystal growth process, after 6 hours solidify 35% of liquation, repeatedly move up and down peeling off in the raw material liquation of press section 42 above ring-type stream 31, and make cooling gas flow 1 hour of using, and continue crystallization face to carry out cooling.Then, the raw material liquation that impurity is concentrated is removed, and observes primary crystal particle P alcrystalline state.Fig. 8 is the primary crystal particle P representing in embodiment althe figure of crystalline state, Fig. 9 is the primary crystal particle P representing in comparative example althe figure of crystalline state.
As shown in Figure 8, in an embodiment, primary crystal particle P in the all-round scope of the inner peripheral surface of container 10 alseparate out equably.That is to say, in an embodiment, be not easy to occur the segregation of crystallization amount.
On the other hand, in comparative example, as shown in Figure 9, present crystallization amount along with from gas supply part 32 ' towards exhaust portion 34 ' and reduce result.In comparative example, exist along with refining carrying out and make the upper level (height of freezing interface) of stores become inhomogeneous possibility.In addition, if the highly significant of freezing interface ground is inhomogeneous, exists and when stores is pushed, make the impaired possibilities such as support rod 41.
(nomenclature)
10 containers
20 heating units
30 cooling elements
31 flow passage structure parts
3a gas flow path
31a~31f is cut apart stream
3b is the cooling opening of using directly
The direct cooled region of 3c
40 primary crystal scraper elements
50 thermal insulation barriers

Claims (7)

1. an aluminium refining plant, comprising:
Have the container at the end, this has the container at the end to accommodate the liquation of raw material aluminium;
Heating unit, this heating unit heats described container;
Cooling element, this cooling element carries out cooling to a part for described container; And
Primary crystal scraper element, this primary crystal scraper element is peeled off the primary crystal particle of separating out on the internal surface of described container,
It is characterized in that,
Described cooling element has to surround the gas flow path that the mode of described container configures,
Described gas flow path is divided into multiple streams of cutting apart of arranging on above-below direction,
Described at least one, cut apart stream contrary with the flow direction of cutting apart the cooling use gas in stream described in remaining.
2. aluminium refining plant as claimed in claim 1, is characterized in that,
From cutting apart stream described in the odd-level of upper beginning and to cut apart the cooling flow direction with gas in stream described in even level from upper beginning contrary.
3. an aluminium process for purification, comprising:
Molten metal injection process, in this molten metal injection process, is injected with the liquation of raw material aluminium in the container at the end;
Local cooling process, in this Local cooling process, cooling mobile in the multiple gas flow paths that configure in the mode of surrounding described container with gas by making, a part for the internal surface of described container is cooled to the temperature lower than primary crystal point;
Crystal growth process, in this crystal growth process, peels off to make it to deposit to the bottom of described container on the primary crystal particle of separating out on the internal surface of described container, and the stores compacting of post-depositional primary crystal particle is made to the crystal growth of aluminium; And
Molten metal discharge process, in this molten metal discharge process, is discharged from the container described liquation,
Described aluminium process for purification is characterised in that,
In described Local cooling process, make to cut apart described at least one stream and described in remaining, to cut apart the cooling flow direction with gas in stream contrary.
4. aluminium process for purification as claimed in claim 3, is characterized in that,
In described Local cooling process, make from cutting apart stream described in the odd-level of upper beginning and to cut apart the cooling flow direction with gas in stream described in even level from upper beginning contrary.
5. the aluminium process for purification as described in claim 3 or 4, is characterized in that,
In described molten metal discharge process, by described container is spun upside down, described liquation is discharged from described container.
6. the aluminium process for purification as described in claim 3 or 4, is characterized in that,
In described crystal growth process, with 4.0 × 10 4~1.1 × 10 5(Pa) pressure, by described stores compacting.
7. the aluminium process for purification as described in claim 3 or 4, is characterized in that,
Carry out the sepn process of peritectic system element, in this peritectic system element sepn process, at least one party in boron and boron-containing compound is added to and contains peritectic system element in the liquation of the raw material aluminium of impurity, and be blown into the gas that contains oxidizing gas, and the peritectic system element floating on the surface of described liquation or peritectic system element compound are removed
In described molten metal injection process, the liquation obtaining is injected to described container in the sepn process of described peritectic system element.
CN201280069220.9A 2012-05-07 2012-05-07 Aluminum refining apparatus and aluminum refining method Pending CN104145033A (en)

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Application publication date: 20141112