CN111254291A - Large copper ingot purification method and device - Google Patents
Large copper ingot purification method and device Download PDFInfo
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- CN111254291A CN111254291A CN202010214716.7A CN202010214716A CN111254291A CN 111254291 A CN111254291 A CN 111254291A CN 202010214716 A CN202010214716 A CN 202010214716A CN 111254291 A CN111254291 A CN 111254291A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 70
- 239000010949 copper Substances 0.000 title claims abstract description 70
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000009413 insulation Methods 0.000 claims abstract description 90
- 239000002826 coolant Substances 0.000 claims abstract description 36
- 238000001816 cooling Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 42
- 229910002804 graphite Inorganic materials 0.000 claims description 41
- 239000010439 graphite Substances 0.000 claims description 41
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 3
- 230000006911 nucleation Effects 0.000 claims description 3
- 238000010899 nucleation Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 238000004321 preservation Methods 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 45
- 239000012535 impurity Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007670 refining Methods 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 3
- 235000017491 Bambusa tulda Nutrition 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 3
- 239000011425 bamboo Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004857 zone melting Methods 0.000 description 3
- 238000005349 anion exchange Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- 229910021592 Copper(II) chloride Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241000270295 Serpentes Species 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000002026 carminative effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000003280 down draw process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- NFFIWVVINABMKP-UHFFFAOYSA-N methylidynetantalum Chemical compound [Ta]#C NFFIWVVINABMKP-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910003468 tantalcarbide Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/006—Pyrometallurgy working up of molten copper, e.g. refining
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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)
Abstract
The invention discloses a method and a device for purifying a large copper ingot, belonging to the technical field of metal purification processes; the high-purity purification problem of the large copper ingot is solved, and the high-purity purification problem comprises a furnace body and a cooling system which are formed by buckling an upper furnace shell and a lower furnace shell, wherein the upper furnace shell and the lower furnace shell can be opened, a thermal field and a supporting system are arranged in the furnace body, and a thermal insulation cage, a bottom top heat preservation layer and a heating device form the thermal field; the supporting system is arranged in the thermal field, the other end of the supporting member penetrates through the bottom heat-insulating layer to be fixedly connected with the bottom of the furnace body, the cooling system is arranged in the supporting table, the heat-insulating cage is fixedly connected with the upper furnace shell, and the bottom heat-insulating layer is fixedly connected with the lower furnace shell through the supporting member; the cooling medium externally connected with the cooling system indirectly performs crystallization and purification on the copper ingot to be purified by cooling the supporting table; gaps are reserved among the bottom heat-insulating layer, the support table and the inner heat-insulating layer; the invention realizes the directional uniform growth of the copper ingot by establishing the controllable thermal field temperature gradient; the large-size preparation of the copper ingot is realized through the selection of crucible materials and the structural design.
Description
Technical Field
The invention belongs to the technical field of metal purification processes, and particularly relates to a large copper ingot purification method and device.
Background
High-purity copper (the purity of copper is 5N-6N, namely 99.999% -99.9999%) contains very few impurities, so that the copper has good electrical conductivity, thermal conductivity, ductility and excellent processability, and is widely applied to sputtering targets, fatigue-resistant cables, electronic industry, flexible cables, ultra-fine enameled wires and other aspects.
The conventional purification techniques for high-purity copper mainly include electrolytic refining, anion exchange and zone-melting refining. The electrolysis method removes impurity elements such As P, Bi, Sb, As, Fe, Ni, Pb, Sn, S, Zn, O and the like by repeatedly electrolyzing high-purity copper, but the electrolysis method has high energy consumption and complex production process, for example, the purification of 5N-6N high-purity copper needs 7-10 days, and the quality is unstable. Anion exchange method, removing impurity ions in copper solution by ion exchange, and evaporating the solution to obtain high-purity CuCl2And reducing the copper to obtain high-purity copper. The process is complex, not beneficial to environmental protection and unstable in quality.
The zone melting refining method is developed since 1955, and the purification principle is as follows: the impurities which can reduce the metal solidifying point move along with the advancing direction of the melting zone, and the impurities which can increase the metal solidifying point move along with the advancing direction of the melting zone, and after multiple times of zone melting, two kinds of impurities in the metal are respectively concentrated at two ends of the metal ingot, and the rest parts are purified. The current zone refining process is still used to produce high purity materials. However, the process has high energy consumption and is difficult to remove impurity elements with large solid-liquid distribution coefficients. In the prior art, a small-size phi 15.7 mm pure copper bar is produced by a process technology of vacuum melting and continuous directional solidification of the copper bar; and adopting a vacuum induction melting hydrogen protection directional solidification device to successfully prepare pure copper rods, tubes and plates by a down-drawing continuous directional solidification technology; however, the method has the defects that the temperature gradient control of the copper ingot purification crystallization is lack of fine control, the equipment and the process are complex, and the production requirement of large-size copper ingots cannot be met.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a method and a device for purifying a large copper ingot, which purify copper by utilizing different segregation coefficients and different saturated vapor pressures of impurities in the copper; the directional uniform growth of the copper ingot is realized by establishing a controllable thermal field temperature gradient; the problem of high-purity purification of large copper ingots is solved.
The invention is realized by the following technical scheme.
A large copper ingot purification device comprises a furnace body and a cooling system, wherein a thermal field and a supporting system are arranged in the furnace body, the thermal field comprises a heat insulation structure and a heating device arranged in the heat insulation structure, and the heat insulation structure comprises a heat insulation cage, a bottom heat insulation layer arranged at the bottom of the heat insulation cage and a top heat insulation layer arranged in the heat insulation cage; the supporting system comprises a supporting table, an inner heat-insulating layer arranged around the supporting table and a supporting member with one end fixedly connected to the bottom of the supporting table, the supporting system is arranged in the thermal field, the other end of the supporting member penetrates through the bottom heat-insulating layer to be fixedly connected with the bottom of the furnace body, the cooling system is arranged inside the supporting table, and a cooling medium externally connected with the cooling system indirectly performs crystallization purification on a copper ingot to be purified through cooling the supporting table; the furnace body comprises an upper furnace shell and a lower furnace shell which are buckled, the upper furnace shell or the lower furnace shell can be separated and opened along a vertical axis under the traction of an external action mechanism, the heat insulation cage is fixedly connected with the upper furnace shell, the bottom heat insulation layer is fixedly connected with the lower furnace shell through a supporting member, and gaps exist between the bottom heat insulation layer and the supporting platform as well as between the bottom heat insulation layer and the inner heat insulation layer.
Furthermore, the bottom heat-insulating layer is of an upper-lower double-layer structure, the heat-insulating structures at the upper part are grown at two ends of the heat-insulating structure at the lower part to form a stepped edge, and the bottoms at two sides of the heat-insulating cage are of a stepped shape matched with the bottom heat-insulating layer and are used for forming a sealing structure when the heat-insulating cage is buckled with the bottom heat-insulating layer.
Furthermore, the top heat-insulating layer is fixedly arranged in the heat-insulating cage and forms a gap with two side walls of the heat-insulating cage.
Further, the side wall of the heat insulation cage is provided with an inner layer heat insulation structure and an outer layer heat insulation structure, and the joint positions of the adjacent inner layer heat insulation structure and the adjacent outer layer heat insulation structure are staggered.
Further, the supporting platform is a graphite supporting platform which is of a convex structure with notches on two sides, and the upper part of the convex structure is used for feeding; and filling gaps on two sides of the graphite support platform by using graphite felt after feeding.
Furthermore, the supporting member comprises a plurality of bottom supports and hollow supporting columns fixedly arranged in the bottom supports, the bottom supports are fixedly connected with the bottom in the lower furnace shell, the bottom of the supporting platform is provided with a hole corresponding to the hollow supporting columns, and the upper portions of the hollow supporting columns extend into the holes and are connected with the supporting platform.
Furthermore, the cooling system comprises a cooling medium inlet pipe, a cooling medium outlet pipe and a cooling medium pump body, wherein the outlet end of the cooling medium inlet pipe sequentially penetrates through the bottoms of the lower furnace shell and the bottom support to extend into the hollow support column to the top of the hollow support column and form a gap with the inner side of the top of the hollow support column; the bottom of collet is provided with a plurality of through-holes, and the coolant exit tube is connected with the collet bottom.
Furthermore, a supporting graphite sheet is arranged at the joint of the hollow supporting column and the low heat insulation layer.
A method for purifying a large copper ingot by using the purification device comprises the following steps:
1) and (3) melting the copper material: putting the copper material into a crucible on a supporting table, and heating and melting the copper material by using a heater; 2) after the melting is finished, introducing a cooling medium into the supporting table to integrally cool the supporting table, so that the bottom of the crucible is cooled, and simultaneously moving the upper furnace shell or the lower furnace shell to clamp the furnace body according to the requirement of temperature gradient, so that the heat in the heat insulation cage is released from the bottom of the heat insulation cage, the temperature in the heat insulation cage is further reduced, and the copper material is gradually crystallized and purified from the bottom to the upper part;
3) after the initial nucleation is completed, the flow rate of the cooling medium is reduced until the cooling is finished.
Preferably, the cooling medium is liquid nitrogen.
Compared with the prior art, the invention has the beneficial effects that.
The invention overcomes the defects of the traditional thermal field, and purifies the copper by utilizing different segregation coefficients and different saturated vapor pressures of impurities in the copper; the directional uniform growth of the copper ingot is realized by establishing a controllable thermal field temperature gradient; the large-size preparation of the copper ingot is realized through crucible material selection and structural design; the high-purity metal directional solidification is realized by heating the inner side surface and the top of the heat insulation cage and performing forced cooling on the bottom, and the bottom supporting table heat insulation system forms an effective temperature gradient. The invention reduces the production time of the high-purity copper ingot to 3-4 days, reduces the production cost to below 30% of electrolytic copper, can produce the copper ingot with the cross section size of 1000mm x 1000mm, meets the multiple purposes of copper in different occasions, and provides a new technical route for the development of large-size high-purity copper target materials.
Drawings
Fig. 1 is a schematic structural diagram of a large copper ingot purification device according to an embodiment of the present invention when heating is turned off.
Fig. 2 is a schematic view of a partial structure of a large copper ingot purification device according to an embodiment of the present invention when the device is started to cool.
Fig. 3 is a schematic structural diagram of a large copper ingot purification device according to an embodiment of the present invention after the furnace shell is completely lifted.
Fig. 4 is a schematic view of a heat insulation cage and a bottom heat insulation layer of the large copper ingot purification device according to the embodiment of the invention.
Fig. 5 is a schematic structural diagram of a hollow support column and a cooling system according to an embodiment of the present invention.
In the figure, 1 is a graphite cylinder, 2 is an upper furnace shell, 3 is a top heat-insulating layer, 4 is a heat-insulating cage, 5 is a top heater, 6 is a crucible, 7 is a side heater, 8 is an inner heat-insulating layer, 9 is a lower furnace shell, 10 is a graphite supporting table, 11 is a bottom heat-insulating layer, 12 is a cooling medium inlet pipe, 13 is a bottom support, 14 is a hollow supporting column, 15 is a bottom heater, 16 is a heat-insulating strip, 17 is a cooling medium outlet pipe, 18 is an inner heat-insulating structure, 19 is an outer heat-insulating structure, and 20 is a supporting graphite sheet.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
As shown in fig. 1, the large copper ingot purification device comprises a furnace body and a cooling system, wherein a thermal field and a supporting system are arranged in the furnace body, the furnace body is formed by buckling an upper furnace shell 2 and a lower furnace shell 9, a hydraulic lifting device (not shown in the figure) is arranged outside the upper furnace shell, and the upper furnace shell 2 and the lower furnace shell 9 can be separated and opened along a vertical axis by the traction of the hydraulic lifting device.
The thermal field comprises a heat insulation structure and a heating device arranged in the heat insulation structure, the heating device comprises a top heater 5, a side heater 7 and a bottom heater 15 which are heat sources, and the heater can be made of graphite, platinum and the like without limitation; the shape of the heater can be selected from sheet, snake, plate and bar; as shown in fig. 4, the heat insulation structure comprises a heat insulation cage 4, a bottom heat insulation layer 11 arranged at the bottom of a bottom base 13, and a top heat insulation layer 3 arranged in the heat insulation cage 4; the heat insulation cage 4 is a heat insulation cage body with an opening at the bottom, the side wall of the heat insulation cage 4 is provided with a double-layer inner heat insulation structure 18 and a double-layer outer heat insulation structure 19, the positions of the joints of the inner heat insulation structure and the outer heat insulation structure are staggered, and meanwhile, a connecting seam formed by the inner heat insulation structure 18 is positioned close to the upper position of the heat insulation cage 4, so that the influence of the connecting seam on a hot-area temperature field is reduced; the inner side of the lower part of the inner heat insulation structure 18 is also provided with a heat insulation strip 16, the heat insulation strip 16 is a movable detachable component, and when the heat insulation cage 4 is lifted, the heat insulation strip plays a role in heat insulation for the side part of the processing material, and is beneficial to establishing a vertical temperature field. The bottom heat-insulating layer 11 is of an upper-lower double-layer structure, two ends of the heat-insulating structure at the lower part are extended out of the heat-insulating structure at the upper part to form a step-shaped edge, and the bottoms of the inner-layer heat-insulating structure and the outer-layer heat-insulating structure of the heat-insulating cage 4 are also step-shaped; the heat insulation cage 4 and the bottom heat insulation layer 11 are buckled to form a sealing structure, and when the heat insulation cage 4 is in a closed state, the heat insulation cage heat insulation layer and the bottom heat insulation layer are combined in a staggered mode, so that a closed space is formed in a hot area; the top heat preservation layer 3 is fixed in the heat insulation cage 4 and located below the top of the heat insulation cage 4, a gap is formed between the top heat preservation layer 3 and two side walls of the heat insulation cage 4, and the top heat preservation layer 3 is fixed when the heat insulation cage 4 is lifted. The whole heat insulation cage 4 is fixedly connected with the upper furnace shell 2 and can be lifted upwards along with the upper furnace shell 2. Go up the top of stove outer covering 2 and still install the carminative graphite section of thick bamboo 1 of heat extraction, graphite section of thick bamboo 1 passes thermal-insulated cage 4's top and top heat preservation 3 entering thermal field in proper order for carry out the emission of heat and gas on thermal field upper portion, graphite section of thick bamboo 1 and thermal-insulated cage 4's junction adopts H type support piece to support.
The supporting system comprises a graphite supporting platform 10, an inner insulating layer 8 wrapped around the graphite supporting platform 10, and a supporting member with one end fixedly connected to the bottom of the graphite supporting platform 10; the graphite support table 10 is a convex structure with notches on two sides, and the upper part of the convex structure is used for feeding; after feeding, filling gaps on two sides of the graphite support table 10 with graphite felts; the inner heat-insulating layer 8 plays a role in preventing the side part of the material to be processed from heat leakage; the supporting member comprises a plurality of groove-shaped stainless steel bottom supports 13 and hollow supporting columns 14 fixedly connected in the bottom supports 13 through bolts, the bottom supports 13 are welded with the inner bottom of the lower furnace shell 9, and the bottom supports 13 play a role in limiting the hollow supporting columns 14; the bottom of the graphite support platform 10 is provided with a pore canal corresponding to the number, shape and position of the hollow support columns 14, and the upper part of the hollow support columns 14 penetrates through the bottom insulating layer 11 and extends into the pore canal to contact with the graphite support platform 10. The hollow support columns 14 are provided with support graphite sheets 20 at the joints with the low thermal insulation layer 11.
As shown in fig. 5, the cooling system includes a cooling medium inlet pipe 12, a cooling medium outlet pipe 17 and a cooling medium pump body (not shown in the figure), wherein an outlet end of the cooling medium inlet pipe 12 sequentially passes through the bottoms of the lower furnace shell 9 and the bottom support 13, extends into the hollow support column 14 to the top of the hollow support column 14, and forms a gap with the inner side of the top of the hollow support column 14; the side surface of the bottom support 13 is provided with a small hole, so that a local negative pressure area or a local positive pressure area is prevented from being formed between the bottom support 13 and the hollow support 14 when the hollow support 14 is installed. The bottom of the bottom support 13 is provided with a plurality of through holes, a cooling medium outlet pipe 17 is communicated with the bottom support 13 and the lower furnace shell 9, a cooling system is externally connected with a liquid nitrogen storage tank, liquid nitrogen enters the graphite support table 10 from a cooling medium inlet pipe 12 to cool the graphite support table 10, and the liquid nitrogen taking heat away flows out of an interlayer of the hollow support column 14 and the cooling medium inlet pipe 12 to the cooling medium outlet pipe 17 at the bottom and is discharged; the crystallized copper ingot to be purified is crystallized and purified indirectly by cooling the graphite support table 10; the bottom heat-insulating layer 11 is fixedly connected with the lower furnace shell 9 through a hollow support column 14, and gaps exist between the bottom heat-insulating layer 11 and the graphite support platform 10 as well as between the bottom heat-insulating layer and the inner heat-insulating layer 8.
The above mentioned structural materials for thermal insulation can be selected from but not limited to graphite carbon felt, graphite hard felt, graphite soft felt, and a combination of graphite hard felt and graphite soft felt. Graphite paper, graphite fiber cloth and the like can be pasted in the heat-insulating layer; the coating such as silicon carbide, tantalum carbide and the like can be plated;
as shown in fig. 2 and fig. 3, after the thermal insulation cage 4 is opened along with the upper furnace shell 2, heat can be radiated from the bottom of the graphite support platform 10, and the hollow support column 14 realizes forced cooling of the graphite support platform 10 through the flow of the cooling medium therein, so as to construct a controllable temperature gradient.
The method for purifying the large copper ingot by adopting the device comprises the following steps:
1) and (3) melting the copper material: putting the copper material into a crucible 6 on a graphite support table 10, and starting a top heater 5, a side heater 7 and a bottom heater 15 to heat and melt the copper material;
2) after the melting is finished, liquid nitrogen is introduced into a cooling medium inlet pipe 12, then the liquid nitrogen is discharged into an interlayer between a hollow support column 14 and the cooling medium inlet pipe 12 through an outlet of the cooling medium inlet pipe 12, and then the liquid nitrogen flows to a cooling medium outlet pipe 17 through a through hole of a bottom support 13, in the process, the cooling medium passes through the inside of a graphite support platform 10 to integrally cool the graphite support platform 10, so that the bottom of a crucible 6 is cooled, then an upper furnace shell 2 is moved to clamp a furnace body according to the requirement of the crystallization temperature of a copper ingot, so that the heat in a heat insulation cage 4 is released from the bottom of the heat insulation cage 4, the temperature in the heat insulation cage 4 is further reduced, and the copper material is gradually crystallized and purified from the bottom to;
3) after the initial nucleation is completed, the flow rate of the cooling medium is reduced until the cooling is finished.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A large copper ingot purification device is characterized by comprising a furnace body and a cooling system, wherein a thermal field and a supporting system are arranged in the furnace body, the thermal field comprises a heat insulation structure and a heating device arranged in the heat insulation structure, and the heat insulation structure comprises a heat insulation cage, a bottom heat insulation layer arranged at the bottom of the heat insulation cage and a top heat insulation layer arranged in the heat insulation cage; the supporting system comprises a supporting table, an inner heat-insulating layer arranged around the supporting table and a supporting member with one end fixedly connected to the bottom of the supporting table, the supporting system is arranged in the thermal field, the other end of the supporting member penetrates through the bottom heat-insulating layer to be fixedly connected with the bottom of the furnace body, the cooling system is arranged inside the supporting table, and a cooling medium externally connected with the cooling system indirectly performs crystallization purification on a copper ingot to be purified through cooling the supporting table; the furnace body comprises an upper furnace shell and a lower furnace shell which are buckled, the upper furnace shell or the lower furnace shell can be separated and opened along a vertical axis under the traction of an external action mechanism, the heat insulation cage is fixedly connected with the upper furnace shell, the bottom heat insulation layer is fixedly connected with the lower furnace shell through a supporting member, and gaps exist between the bottom heat insulation layer and the supporting platform as well as between the bottom heat insulation layer and the inner heat insulation layer.
2. The large-scale copper ingot purification device according to claim 1, wherein the bottom insulating layer is of an upper and lower double-layer structure, the upper insulating structure is grown at two ends of the lower insulating structure to form a stepped edge, and the bottoms at two sides of the heat insulation cage are stepped to match the bottom insulating layer, so that a sealing structure is formed when the heat insulation cage is fastened with the bottom insulating layer.
3. The large copper ingot purification device according to claim 1, wherein the top insulating layer is fixedly arranged in the heat insulation cage and forms a gap with two side walls of the heat insulation cage.
4. The large-scale copper ingot purification device according to claim 1, wherein the side wall of the heat insulation cage is provided with an inner and outer multi-layer heat insulation structure, and the joint positions of the adjacent inner and outer heat insulation structures are staggered.
5. The large copper ingot purification device according to claim 1, wherein the support table is a graphite support table, the graphite support table is a convex structure with notches on two sides, and the upper part of the convex structure is used for feeding; and filling gaps on two sides of the graphite support platform by using graphite felt after feeding.
6. The large copper ingot purification device according to claim 1, wherein the support member comprises a plurality of bottom supports and hollow support columns fixedly arranged in the bottom supports, the bottom supports are fixedly connected with the bottom in the lower furnace shell, the bottom of the support table is provided with holes corresponding to the hollow support columns, and the upper parts of the hollow support columns extend into the holes and are connected with the support table.
7. The large copper ingot purification device according to claim 6, wherein the cooling system comprises a cooling medium inlet pipe, a cooling medium outlet pipe and a cooling medium pump body, wherein the outlet end of the cooling medium inlet pipe sequentially penetrates through the bottoms of the lower furnace shell and the bottom support to extend into the hollow support column to the top of the hollow support column and form a gap with the inner side of the top of the hollow support column; the bottom of collet is provided with a plurality of through-holes, and the coolant exit tube is connected with the collet bottom.
8. A large copper ingot purification device according to claim 6 or 7, wherein the hollow supporting columns are provided with supporting graphite sheets at the joints with the low thermal insulation layer.
9. A method for purifying a large copper ingot by using the purification apparatus as claimed in any one of claims 1 to 7, comprising the steps of:
1) and (3) melting the copper material: putting the copper material into a crucible on a supporting table, and heating and melting the copper material by using a heater; 2) after the melting is finished, introducing a cooling medium into the supporting table to integrally cool the supporting table, so that the bottom of the crucible is cooled, and simultaneously moving the upper furnace shell or the lower furnace shell to clamp the furnace body according to the requirement of temperature gradient, so that the heat in the heat insulation cage is released from the bottom of the heat insulation cage, the temperature in the heat insulation cage is further reduced, and the copper material is gradually crystallized and purified from the bottom to the upper part;
3) after the initial nucleation is completed, the flow rate of the cooling medium is reduced until the cooling is finished.
10. A method for purifying a large copper ingot according to claim 9, wherein the cooling medium is liquid nitrogen.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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