CN103898338A - Method and apparatus for separation and purification of high-purity aluminum - Google Patents
Method and apparatus for separation and purification of high-purity aluminum Download PDFInfo
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- CN103898338A CN103898338A CN201310737750.2A CN201310737750A CN103898338A CN 103898338 A CN103898338 A CN 103898338A CN 201310737750 A CN201310737750 A CN 201310737750A CN 103898338 A CN103898338 A CN 103898338A
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Abstract
The invention provides a method for separation and purification of high-purity aluminum. According to the method, the high-purity aluminum is prepared from primary aluminum by virtue of a smelting method, a segregation method and a batch ultrasonic separation method, wherein the purity of the produced qualified high-purity aluminum can be 99.99-99.9999%. Specifically, the method comprises the following steps: loading the raw material in a smelting furnace, and heating to 680-750 DEG C so that the raw material is melted into molten aluminum; adding a refining agent and smelting, and then discharging 1-10% of molten aluminum at the bottom; transferring the rest molten aluminum into a segregation furnace; adjusting the flow rate of cooling gas and cooling the wall of the furnace at 558-665 DEG C, and then carrying out segregation and crystallization; vibrating the segregated crystals by use of ultrasonic waves, and when the segregated crystals are separated from the wall of the segregation furnace until 15-35% of alumium liquid is left in a crystallization furnace, pouring out the residual liquid; cooling a crystallized alumium ingot and then taking out; and removing 3-15% of the weight of the ingot from the head and the tail parts of the crystallized ingot respectively, thus obtaining the high-purity aluminum product.
Description
Technical field
The present invention relates to method of purification and the equipment of the method for purification of metallic aluminium, particularly rafifinal.
Background technology
Along with the continuous progress of science and technology, rafifinal has purposes widely in fields such as electronics, Aeronautics and Astronautics and national defense industry, and its consumption increases year by year.At present, countries in the world great majority adopt three layers of liquid electrolytic refining process, segregation method of purification, organic solution electrolytic process etc. to prepare the high-purity or ultra-pure aluminum of various purity.Three layers of liquid electrolytic refining process extracted the purity of aluminium between 4N to 5.5N, but power consumption is generally more than 13000kwh/t, is 4 to 5 times of left and right of segregation method, and energy consumption is high; The obnoxious flavour serious environment pollutions such as the fluorochloride meanwhile, producing in electrolytic process.Organic solution electrolytic process owing to yielding poorly, complex process, general only for the producing on a small quantity of the above purity ultra-pure aluminum of 7N, be not suitable for suitability for industrialized production.Segregation principle method of purification belongs to physical purification method, can be used to prepare the rafifinal of 3.5N to 6N purity according to the difference of raw material, technology and equipment, and has that energy consumption is low, labour intensity is little, free of contamination feature, uses more and more extensive.
The segregation method of purification of aluminium mainly contains directional solidification method, zone melting method, Steppecd crystallization.Zone melting method can obtain the rafifinal of 5.5N to 6N, is mainly used in three layers of liquid electrolytic refining process or other segregation method rafifinals further to purify, and equipment complexity, inefficiency, energy consumption are higher, are not suitable for suitability for industrialized production.Directional solidification method can obtain the rafifinal of 4N to 6N, but its complex process, size little, yield poorly, be difficult to realize scale of mass production.Steppecd crystallization is industrialization use in a large number at home and abroad, refining effect depends on the purity of primary aluminum, the aluminum feedstock of the general 99.5-99.95% of use can obtain the rafifinal of 3.5N to 6N through purifying, but the shortcomings such as existing technique is high to ingredient requirement, production efficiency is low, consumable quantity is large, need further optimize, improve.At present, the key problem that uses Steppecd crystallization to produce rafifinal is improvement, optimizes crystallization mode, keeps good refining effect and higher production efficiency when improving the quality of products.
Summary of the invention
Technical problem to be solved by this invention is, for prior art deficiency, provide a kind of technique flexibly, simple, and energy-saving and environmental protection, high yield, high-quality rafifinal method of purification.
A technical scheme of the present invention provides a kind of separating and purifying method of rafifinal, comprises following steps:
1), by industrial aluminum raw material, surface is cleared up and is dried;
2) step 1) gained raw material is put into smelting furnace, heating is incubated after fusing completely;
3) to step 2) add refining agent master alloy in gained fused solution, start to stir, after stirring reaction, leave standstill insulation, the aluminium liquid of bottom 1-10% is discharged;
4) step 3) residual Al liquid is proceeded to segregation stove, after 558-665 DEG C of insulation, cooling and compacting crystal, simultaneously brilliant by the stripping of intermittent type ultrasonic wave, during to aluminium liquid residue 15-35%, stop, and upper strata residual Al liquid is poured out;
5) be cooled to normal temperature, take out aluminium ingot, the head of crystallization ingot and afterbody are removed respectively to crystallization ingot weight
3-15%, obtains rafifinal product.
The method providing according to technique scheme, iterative process step, can obtain more highly purified rafifinal.
In some embodiments, industrial aluminum material purity of the present invention is more than or equal to 99.7%.
In some embodiments, gained rafifinal product purity of the present invention is 99.99-99.9999%.
In some embodiments, step 2 of the present invention) described in be heated to be and be heated to 680-750 DEG C
In some embodiments, step 2) described soaking time is 0.5-2 hour, and the stirring reaction time is 0.5-2 hour described in step 3), and soaking time is 0.5-2 hour described in step 4).
A kind of segregation stove of the method providing for technique scheme is provided another technical scheme of the present invention, comprise interval type ultrasonic wave and shell brilliant device 3, compaction apparatus 4, annular gas cooling duct 5, heating unit 6, plumbago crucible 2 and Stainless Steel Crucible 7, and plumbago crucible is placed in Stainless Steel Crucible, heating unit from top to bottom interval is fixedly installed in Stainless Steel Crucible and furnace shell takes between interlayer; Annular gas cooling duct directly contacts with Stainless Steel Crucible, and is placed in its outside; The brilliant device of the ultrasonic stripping of intermittent type and annular gas cooling duct horizontal positioned, and directly contact, ultrasonic source is placed in outside furnace shell.
In some embodiments, smelting furnace adopts gas heating to make raw materials melt, adopts resistive heating insulation.In some embodiments, adopt heat accumulating type smelting furnace, in the time of the molten aluminium of a stove eye, other stove eyes can be distinguished preheating, to save molten aluminium cost.
Technique scheme of the present invention has been improved segregation furnace accretion crystalline substance and primary crystal scrapes mode, crystallisation process carries out in crystal growing furnace, crucible rotates counterclockwise at stove inner-spiral type, compaction apparatus clockwise rotates at crucible inner-spiral type, fully stirred melt, well heater keeps the interior homo(io)thermism of crystal growing furnace at 558-665 DEG C; Cooling gas carries out Local cooling by furnace wall cooling air pipe to molten aluminium in crystal growing furnace crucible, makes melt produce tiny primary crystal; Adopt intermittent type vibration of ultrasonic wave source to shake the first crystal of crucible inwall, first crystal is shaken off and is settled down to crucible bottom; By crystal compaction apparatus, first crystal is pushed, by the extruding of intergranular melt, primary crystal surface layer is anti-molten simultaneously, to improve purification efficiency; Can control crystallization rate interval time by control cooling gas flow, pressure, compaction apparatus elevation rate, intermittent type vibration of ultrasonic wave; Can measure residual Al liquid measure by compaction apparatus stroke; By controlling residual Al liquid measure control rafifinal product purity; Adopt intermittent type vibration of ultrasonic wave to separate just crystal, can save primary crystal scraper plate, reduce the consumption of graphite material and reduced its pollution to product.
Beneficial effect of the present invention is:
(1) the present invention, by fusion process, can remove the impurity element of segregation coefficient >=0.9, comprises Ti, V, Cr, Zr etc., has expanded raw material sources scope, has reduced raw materials cost;
(2) segregation stove provided by the invention can fully stir melt; Can make primary crystal surface layer anti-molten by crystal compaction apparatus, intermittent type vibration of ultrasonic wave source and refrigerating unit acting in conjunction, improve purification efficiency; Adopt intermittent type vibration of ultrasonic wave to separate just crystal, can save primary crystal scraper plate, reduce the consumption of graphite material and reduced its pollution to product;
(3) current conventional rafifinal production technology, melt raw material and stirred crystallization are in same stove, and the time generally could finish more than 15 hours in crystallization, the present invention by comparison, efficiency can promote approximately 3 times, if same size is produced continuously, gross investment can reduce nearly half;
(4), according to the purity difference of raw material, can obtain the rafifinal of different purity; Iterative process step, can obtain more highly purified rafifinal.
Brief description of the drawings
Fig. 1 is segregation furnace structure schematic diagram of the present invention.
In figure: 1 is high-purity aluminium ingot; 2 is plumbago crucible and base, and 3 shell brilliant device for interval type ultrasonic wave, and 4 is compaction apparatus, and 5 is annular gas cooling duct, and 6 is heating unit, and 7 is Stainless Steel Crucible.
Embodiment
The following stated be the preferred embodiment of the present invention, what the present invention protected is not limited to following preferred implementation.It should be pointed out that on the basis of conceiving in these innovation and creation for a person skilled in the art, some distortion and the improvement made, all belong to protection scope of the present invention.
1) selecting 27.5Kg purity is that 99.7% Raw Aluminium is raw material, and its surface is cleared up and dried;
2) raw material of getting ready is put into smelting furnace, be heated to 750 DEG C to being incubated 1 hour after fusing completely;
3) add refining agent master alloy (aluminum-boron alloy), turn on agitator stirring reaction, leaves standstill insulation, opens lower part outlet, and the aluminium liquid of bottom 2.5Kg is emitted, and the aluminium liquid of upper strata 25Kg is proceeded to segregation stove;
4) segregation crystallization, segregation stove resistive heating to 660 DEG C insulation 1 hour, opens annular gas cooling pipeline, opens compaction apparatus, opens intermittent type ultrasonic wave and shells brilliant device, and after 4 hours, aluminium liquid stops while remaining 25%, and upper strata aluminium liquid is poured out;
5) Stainless Steel Crucible is proposed to be cooled to normal temperature, take out aluminium ingot, head, the afterbody of crystallization ingot are removed respectively to 3%, 10% of quality, middle portion is the rafifinal of required purity, heavy 17Kg.
After testing, meet GB/T8644-2000 remelting refined aluminium ingot 4.3N standard.
1) selecting 30Kg purity is that 99.996% Raw Aluminium is raw material, and its surface is cleared up and dried;
2) raw material of getting ready is put into smelting furnace, be heated to 680 DEG C to being incubated 1.5 hours after fusing completely;
3) add refining agent master alloy (aluminum-boron alloy), turn on agitator stirring reaction, leaves standstill insulation, opens lower part outlet, and the aluminium liquid of bottom 3Kg is emitted, and the aluminium liquid of upper strata 27Kg is proceeded to segregation stove;
4) segregation crystallization, segregation stove resistive heating to 665 DEG C insulation 2 hours, opens annular gas cooling pipeline, opens compaction apparatus, opens intermittent type ultrasonic wave and shells brilliant device, and after 4 hours, aluminium liquid stops while remaining 35%, and upper strata aluminium liquid is poured out;
5) Stainless Steel Crucible is proposed to be cooled to normal temperature, take out aluminium ingot, head, the afterbody of crystallization ingot are removed respectively to 5%, 15% of quality, middle portion is the rafifinal of required purity, heavy 14Kg.
After testing, meet GB/T8644-2000 remelting refined aluminium ingot 5.5N standard.
1) selecting 27.5Kg purity is that 99.7% Raw Aluminium is raw material, and its surface is cleared up and dried;
2) raw material of getting ready is put into smelting furnace, be heated to 720 DEG C to being incubated 0.5 hour after fusing completely;
3) add refining agent master alloy (aluminum-boron alloy), turn on agitator stirring reaction, leaves standstill insulation, opens lower part outlet, and the aluminium liquid of bottom 2.5Kg is emitted, and the aluminium liquid of upper strata 25Kg is proceeded to segregation stove;
4) segregation crystallization, segregation stove resistive heating to 560 DEG C insulation 1.5 hours, opens annular gas cooling pipeline, opens compaction apparatus, opens intermittent type ultrasonic wave and shells brilliant device, and after 4 hours, aluminium liquid stops while remaining 25%, upper strata aluminium liquid is poured out,
5) Stainless Steel Crucible is proposed to be cooled to normal temperature, take out aluminium ingot, head, the afterbody of crystallization ingot are removed respectively to 5%, 10% of quality, middle portion is the rafifinal of required purity, heavy 17Kg;
6) repeating step 2)-5), obtain the about 10Kg of rafifinal.
After testing, meet GB/T8644-2000 remelting refined aluminium ingot 5.5N standard.
Claims (6)
1. a separating and purifying method for rafifinal, is characterized in that comprising following steps:
1), by industrial aluminum raw material, surface is cleared up and is dried;
2) step 1) gained raw material is put into smelting furnace, heating is incubated after fusing completely;
3) to step 2) add refining agent master alloy in gained fused solution, start to stir, after stirring reaction, leave standstill insulation, the aluminium liquid of bottom 1-10% is discharged;
4) step 3) residual Al liquid is proceeded to segregation stove, after 558-665 DEG C of insulation, cooling and compacting crystal, simultaneously brilliant by the stripping of intermittent type ultrasonic wave, during to aluminium liquid residue 15-35%, stop, and upper strata residual Al liquid is poured out;
5) be cooled to normal temperature, take out aluminium ingot, the head of crystallization ingot and afterbody are removed respectively to the 3-15% of crystallization ingot weight, obtain rafifinal product.
2. method according to claim 1, is characterized in that, described industrial aluminum material purity is more than or equal to 99.7%.
3. method according to claim 1, is characterized in that, gained rafifinal product purity is 99.99-99.9999%.
4. method according to claim 1, is characterized in that step 2) described in be heated to be and be heated to 680-750 DEG C.
5. method according to claim 1, is characterized in that step 2) described soaking time is 0.5-2 hour, and the stirring reaction time is 0.5-2 hour described in step 3), and soaking time is 0.5-2 hour described in step 4).
6. the segregation stove for the separating and purifying method of aluminium described in claim 1-5 any one, it is characterized in that, comprise interval type ultrasonic wave and shell brilliant device (3), compaction apparatus (4), annular gas cooling duct (5), heating unit (6), plumbago crucible (2) and Stainless Steel Crucible (7), and plumbago crucible is placed in Stainless Steel Crucible, heating unit from top to bottom interval is fixedly installed in Stainless Steel Crucible and furnace shell takes between interlayer; Annular gas cooling duct directly contacts with Stainless Steel Crucible, and is placed in its outside; The brilliant device of the ultrasonic stripping of intermittent type and annular gas cooling duct horizontal positioned, and directly contact, ultrasonic source is placed in outside furnace shell.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779604A (en) * | 2017-11-28 | 2018-03-09 | 河钢股份有限公司承德分公司 | A kind of method for handling aluminium vanadium folder Fe alloy slag |
| CN109609778A (en) * | 2019-02-19 | 2019-04-12 | 东北大学 | A method of primary aluminum, which is carried out, using metal extraction removes gallium |
| CN111378850A (en) * | 2020-05-08 | 2020-07-07 | 河南中孚实业股份有限公司 | Method for purifying high-purity aluminum by segregation |
| CN111926197A (en) * | 2020-09-01 | 2020-11-13 | 南通泰德电子材料科技有限公司 | Purification method of ultra-high purity aluminum |
| CN115404356A (en) * | 2022-09-22 | 2022-11-29 | 同创普润(上海)机电高科技有限公司 | Method for reducing content of infusible matter in high-purity aluminum melt |
| CN115418496A (en) * | 2022-09-20 | 2022-12-02 | 广元华博精铝科技有限公司 | Process method and production device for segregation purification of high-purity aluminum |
| CN115572840A (en) * | 2022-09-29 | 2023-01-06 | 吉利百矿集团有限公司 | Method for purifying electrolytic aluminum liquid by segregation method |
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| CN101748291A (en) * | 2010-01-28 | 2010-06-23 | 上海交通大学 | High-purity aluminum purification device based on segregation method |
| CN101775504A (en) * | 2010-03-10 | 2010-07-14 | 抚顺东工冶金材料技术有限公司 | Method for preparing clean fine-grained aluminium alloy wire rod |
| CN102251135A (en) * | 2011-08-05 | 2011-11-23 | 中信戴卡轮毂制造股份有限公司 | Improved aluminum liquid refining process |
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Patent Citations (3)
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| CN101748291A (en) * | 2010-01-28 | 2010-06-23 | 上海交通大学 | High-purity aluminum purification device based on segregation method |
| CN101775504A (en) * | 2010-03-10 | 2010-07-14 | 抚顺东工冶金材料技术有限公司 | Method for preparing clean fine-grained aluminium alloy wire rod |
| CN102251135A (en) * | 2011-08-05 | 2011-11-23 | 中信戴卡轮毂制造股份有限公司 | Improved aluminum liquid refining process |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107779604A (en) * | 2017-11-28 | 2018-03-09 | 河钢股份有限公司承德分公司 | A kind of method for handling aluminium vanadium folder Fe alloy slag |
| CN109609778A (en) * | 2019-02-19 | 2019-04-12 | 东北大学 | A method of primary aluminum, which is carried out, using metal extraction removes gallium |
| CN111378850A (en) * | 2020-05-08 | 2020-07-07 | 河南中孚实业股份有限公司 | Method for purifying high-purity aluminum by segregation |
| CN111926197A (en) * | 2020-09-01 | 2020-11-13 | 南通泰德电子材料科技有限公司 | Purification method of ultra-high purity aluminum |
| CN115418496A (en) * | 2022-09-20 | 2022-12-02 | 广元华博精铝科技有限公司 | Process method and production device for segregation purification of high-purity aluminum |
| CN115404356A (en) * | 2022-09-22 | 2022-11-29 | 同创普润(上海)机电高科技有限公司 | Method for reducing content of infusible matter in high-purity aluminum melt |
| CN115404356B (en) * | 2022-09-22 | 2024-03-22 | 同创普润(上海)机电高科技有限公司 | Method for reducing content of unmelted matters in high-purity aluminum melt |
| CN115572840A (en) * | 2022-09-29 | 2023-01-06 | 吉利百矿集团有限公司 | Method for purifying electrolytic aluminum liquid by segregation method |
| CN115572840B (en) * | 2022-09-29 | 2024-01-16 | 吉利百矿集团有限公司 | Method for purifying electrolytic aluminum liquid by segregation method |
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Address after: No. 368 East Sunshine Science Park 523871 Guangdong city of Dongguan province Changan Zhen Sha Zhen'an Road Applicant after: DONGGUAN DONGYANG GUANGKE R & D CO., LTD. Address before: No. 368 East Sunshine Science Park 523871 Guangdong city of Dongguan province Changan Zhen Sha Zhen'an Road Applicant before: Dongyang, Dongguan City Chang'an light Aluminum research and development company limited |
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Application publication date: 20140702 |