CN102220502B - Method for preparing aluminum-scandium intermediate alloy by thermal reduction of aluminum-calcium alloy - Google Patents
Method for preparing aluminum-scandium intermediate alloy by thermal reduction of aluminum-calcium alloy Download PDFInfo
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- CN102220502B CN102220502B CN2011101387376A CN201110138737A CN102220502B CN 102220502 B CN102220502 B CN 102220502B CN 2011101387376 A CN2011101387376 A CN 2011101387376A CN 201110138737 A CN201110138737 A CN 201110138737A CN 102220502 B CN102220502 B CN 102220502B
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Abstract
The invention discloses a method for preparing an aluminum-scandium master alloy by thermal reduction of an aluminum-calcium alloy, which comprises the following steps: 1) calculating the weight of raw materials of aluminum-calcium alloy and scandium halide or molten salt thereof and alkali metal chloride required by smelting in each furnace according to the component content of the aluminum-scandium intermediate alloy; 2) uniformly mixing a scandium halide or a molten salt thereof with an alkali metal chloride, adding the mixture into a crucible, heating to 750-950 ℃ for melting, and obtaining a molten scandium-containing molten salt; 3) adding an aluminum-calcium alloy into the molten scandium-containing molten salt, and carrying out thermal reduction for 20-200 min after the aluminum-calcium alloy is molten; 4) and after the thermal reduction reaction is finished, adding excessive refining agent to remove calcium, when the content of calcium in the alloy is less than 50ppm, pouring and cooling the cast ingot, and leaching and removing slag to obtain the aluminum-scandium intermediate alloy. The process flow is simple and feasible, the metal yield is high, the method is simpler and more environment-friendly than the traditional method, green production can be realized, and the method has the advantages of simple operation, simple equipment, low production energy consumption, small environmental pollution, economy and stability.
Description
Technical field
The present invention relates to the scandium bearing master alloy preparing technical field, exactly relate to a kind of method that adopts hot reducing method to prepare scandium bearing master alloy.
Background technology
Scandium is widely used duraluminum, and duraluminum is played a part up to now the most effectively grain refining and suppresses recrystallize.The character of scandium is active, and scandium and aluminium fusing point difference are very big, therefore, in duraluminum, adds scandium and adds with the form of master alloy usually.Market is to the increase in demand of high-performance aluminum scandium alloy in recent years, and the preparation of scandium bearing master alloy also receives numerous metallargists' concern and research.
Aluminum current scandium alloy working method has the method for mixing, fused salt electrolysis process, thermit reduction etc., and complicated to mixing the method technological operation, the scandium scaling loss is serious, and metal recovery rate is not high, and the metal scandium preparation is comparatively complicated, and production cost is difficult for reducing.The fused salt electrolysis process equipment requirements is higher, and power consumption is bigger, is unfavorable for energy-saving and emission-reduction.Adopt among the hot reducing method preparation technology at present; Mainly contain scandium fluoride vacuum thermite process, Scium trioxide thermit reduction, Scium trioxide-sodium aluminum fluoride-sodium-chlor (potassium) fused salt; Scium trichloride-magnalium hot reducing method etc.; For example publication number is CN 101709394A, and the Chinese patent document that open day is on May 19th, 2010 discloses a kind of preparation method of scandium bearing master alloy, belongs to high-performance aluminium alloy raw material preparing technical field.It is characterized in that the raw material of said method is: Sc
2O
3, fine aluminium, molten salt system; Its preparation method is disposable with fine aluminium, Sc
2O
3Mix with molten salt system, add crucible, put into the resistance furnace heat fused, be warming up to 950 ℃ ± 20, be incubated 90-120 minute; Insulation finishes back casting sampling; Said molten salt system is NF
4HF
2, KCl, NaCl, NaF, nNaFAlF
3(sodium cryolite), nKFAlF
3(potassium cryolite), NF
4HF
2, NaF, KCl, NaCl, sodium cryolite and potassium cryolite blending ratio be that ratio is 10: 8: 5.4: 5.4: 3: 3; Said molten salt system and fine aluminium and Scium trioxide are 30 ± 1.5 by mass ratio: 100: 4 ± 0.1 adds crucible.Compared with prior art, the alloy grain degree of present method preparation is littler, Al
3Sc is evenly distributed, obviously reunion and size are not tiny.This master alloy is used in follow-up containing in the preparation of Sc alloy, has very excellent thinning effect.
But above-mentioned prior art all exists the recovery not high; Covering molten salt system, often to contain villiaumite such as sodium aluminum fluoride many, furnace wall and electrical equipment corrosion-resistant property are required height, and be unfavorable for environmental protection; Deficiencies such as equipment requirements complicacy.Equipment requirements was higher when sodium aluminum fluoride prepared in addition, and this has also restricted industrial large-scale application.
Summary of the invention
To the complicacy of processing unit and the deficiency of operating aspect in the above-mentioned aluminum scandium alloy production; The invention provides that a kind of simple to operate, equipment is simple, the recovery of metal scandium is high, production energy consumption is low, environmental pollution is little, the aluminum scandium alloy working method of economic stability.
The present invention realizes through adopting following technical proposals:
A kind of kalzium metal thermal reduction prepares the method for scandium bearing master alloy, it is characterized in that comprising:
1) component content by scandium bearing master alloy calculates required raw material kalzium metal, the halogenide of scandium or the weight of its fused salt and alkali metal chloride of every stove smelting, takes by weighing respectively;
2) halogenide of scandium or its fused salt and alkali metal chloride mixed to add in the crucible be warming up to 750 ℃ ~ 950 ℃ thawings, fusion contain the scandium fused salt;
3) kalzium metal is added said fusion and contain in the scandium fused salt, treat that kalzium metal melts back heat preservation hot reductase 12 0 ~ 200min;
4) treat that thermal reduction reaction is accomplished after, add excessive refining agent and carry out deliming, when treating that calcium contents is less than 50ppm in the alloy, cast ingot casting and cooling, the water logging slagging-off promptly obtains scandium bearing master alloy.
In the said kalzium metal, by weight, calcium contents is 3% ~ 20%, and surplus is aluminium and unavoidable impurities.
The halogenide of described scandium is that the anhydrous scandium halide that makes of chemical method or its contain the scandium fused salt, and said anhydrous scandium halide is anhydrous chlorides of rase scandium, anhydrous scandium fluoride, anhydrous scandium bromide or anhydrous scandium iodide, requires dehydration fully, and scandium halide content is 1% ~ 25% of fused salt amount.
Described alkali metal halide is one or both a mixture of sodium-chlor, Repone K, and the weight ratio of sodium-chlor and Repone K is in the mixture: 75-98:25-2, the consumption of alkali metal halide are 0.1 ~ 1.5 times of kalzium metal weight.
Described crucible is plumbago crucible, corundum crucible, iron crucible or tantalum crucible.
Described refining agent is the refining slag system that ALUMNIUM FLUORIDE, sodium aluminum fluoride are formed, and refining agent adopts a kind of of following two kinds of schemes, all by mass ratio:
1. 40%Na
3AlF
6The fused salt mixt of+40%NaCl+20%KCl;
2. 40%Na
3AlF
6The fused salt mixt of+60%NaCl.
The said type of cooling is to adopt 60 ~ 100 ℃ water cooling.
4) back slag recovering step in addition; Slag is adopted direct water logging, and immersion liquid is used as flux through the evaporative crystallization continued, soaks slag under 180 ~ 200 ℃; Adding the vitriol oil leaches; The tail gas that produces in the acidleach process adopts alkali lye to absorb, soak slag acidleach fully after, be recyclable scandium after dilution, extracting and separating, purification.
Compared with prior art, the technique effect that the present invention reached is following:
1, the present invention adopts 1), 2), 3), 4) and 5) technical scheme that forms; Its reaction principle for reaching technique effect is: covering under the molten salt system protection; With the scandium halide is raw material; With alkali-metal halogenide is flux, is reductive agent and collecting agent with the calloy, adopts calloy that the halogenide reduction of scandium is formed scandium bearing master alloy; Its processing condition are: the mixing halogen with the alkali metal chloride-scandium halide of 0.1 ~ 1.5 times of kalzium metal weight is the molten protection system, and wherein scandium halide accounts for fused salt mixt 1 ~ 25%; Reduction temperature: 750 ℃ ~ 950 ℃, reaction times 20 ~ 120min, react completely back refining deliming, founding promptly get scandium bearing master alloy.Alloy product contains scandium 2 ~ 10%, Sc+Al>99%, other impurity such as Ca, Na, F equal size are less than 50ppm, and the recovery of Sc is greater than 90%, and product meets the XB/T402-2008 standard.The present invention adopts the method for thermal reduction; This technical process simple possible; The recovery of metal scandium is high, than the more simple environmental protection of traditional method, can realize green production; Have that simple to operate, equipment is simple, the recovery of metal scandium is high, production energy consumption is low, environmental pollution is little, the advantage of economic stability.
2, in the kalzium metal that the present invention adopts, by weight, calcium contents is 3% ~ 20%; Scandium halide content is 1% ~ 25% of fused salt amount, and crucible is plumbago crucible, corundum crucible, iron crucible or tantalum crucible, and refining agent is the refining slag system that ALUMNIUM FLUORIDE, sodium aluminum fluoride are formed; The type of cooling is to adopt 60 ~ 100 ℃ water cooling; Such technical scheme finally makes the quality of the scandium bearing master alloy of preparation reach best, and the recovery of scandium reaches more than 92%; Other impurity Ca, Na, F equal size have concrete experiment all less than 50ppm referring to embodiment.
Description of drawings
To combine Figure of description and embodiment that the present invention is done further detailed description below, wherein: Fig. 1 is the process flow sheet of embodiment 2.
Embodiment
Embodiment 1
The invention discloses the method that a kind of kalzium metal thermal reduction prepares scandium bearing master alloy, comprising:
1) component content by scandium bearing master alloy calculates required raw material kalzium metal, the halogenide of scandium or the weight of its fused salt and alkali metal chloride of every stove smelting, takes by weighing respectively;
2) halogenide of scandium or its fused salt and alkali metal chloride mixed to add in the crucible be warming up to 750 ℃ ~ 950 ℃ thawings, fusion contain the scandium fused salt;
3) kalzium metal is added said fusion and contain in the scandium fused salt, treat that kalzium metal melts back heat preservation hot reductase 12 0 ~ 200min;
4) treat that thermal reduction reaction is accomplished after, add excessive refining agent and carry out deliming, when treating that calcium contents is less than 50ppm in the alloy, cast ingot casting and cooling, the water logging slagging-off promptly obtains scandium bearing master alloy.
Reaction principle is: covering under the molten salt system protection; With the scandium halide is raw material; With alkali-metal halogenide is flux, is reductive agent and collecting agent with the calloy, adopts calloy that the halogenide reduction of scandium is formed scandium bearing master alloy; Its processing condition are: the mixing halogen with the alkali metal chloride-scandium halide of 0.1 ~ 1.5 times of kalzium metal weight is the molten protection system, and wherein scandium halide accounts for fused salt mixt 1 ~ 25%; Reduction temperature: 750 ℃ ~ 950 ℃, reaction times 20 ~ 120min, react completely back refining deliming, founding promptly get scandium bearing master alloy.Alloy product contains scandium 2 ~ 10%, Sc+Al>99%, other impurity such as Ca, Na, F equal size are less than 50ppm, and the recovery of Sc is greater than 90%, and product meets the XB/T402-2008 standard.
Embodiment 2
On the basis of embodiment 1, preferred forms of the present invention is: in the kalzium metal, by weight, calcium contents is 3% ~ 20%, and surplus is aluminium and unavoidable impurities.The halogenide of scandium is that the anhydrous scandium halide that makes of chemical method or its contain the scandium fused salt, and said anhydrous scandium halide is anhydrous chlorides of rase scandium, anhydrous scandium fluoride, anhydrous scandium bromide or anhydrous scandium iodide, requires dehydration fully, and scandium halide content is 1% ~ 25% of fused salt amount.Alkali metal halide is one or both a mixture of sodium-chlor, Repone K, and the weight ratio of sodium-chlor and Repone K is in the mixture: 75-98:25-2, the consumption of alkali metal halide are 0.1 ~ 1.5 times of kalzium metal weight.Crucible is plumbago crucible, corundum crucible, iron crucible or tantalum crucible.Refining agent is the refining slag system that ALUMNIUM FLUORIDE, sodium aluminum fluoride are formed, and refining agent adopts a kind of of following two kinds of schemes, all by mass ratio: 1. 40%Na
3AlF
6The fused salt mixt of+40%NaCl+20%KCl; 2. 40%Na
3AlF
6The fused salt mixt of+60%NaCl.The type of cooling is to adopt 60 ~ 100 ℃ water cooling.4) back slag recovering step in addition; Slag is adopted direct water logging, and immersion liquid is used as flux through the evaporative crystallization continued, soaks slag under 180 ~ 200 ℃; Adding the vitriol oil leaches; The tail gas that produces in the acidleach process adopts alkali lye to absorb, soak slag acidleach fully after, be recyclable scandium after dilution, extracting and separating, purification.
Be concrete experiment embodiment of the present invention below:
Embodiment 3
Take by weighing sodium-chlor 42.6g, Repone K 42.6g, scandium fluoride 10.6g, mix the back and add in the plumbago crucible, be warming up to 800 ℃; Treat that fused salt melts the kalzium metal 213.0g that the back adds calcium contents 3.2%, treat that kalzium metal melts after, insulation retailoring 20min; Add kalzium metal weight 4% refining agent insulation deliming 30min; Take out crucible, the slagging-off founding demoulding is with 60 ~ 100 ℃ of water coolings.The weighing of removing slag obtains scandium bearing master alloy 212.3g, analyzes through ICP-AES, and containing the scandium amount is 2.06%, the recovery 93.2% of scandium.Other impurity Ca, Na, F equal size are all less than 50ppm.The slag recycling.
Embodiment 4
Take by weighing sodium-chlor 64.8g, Repone K 64.8g, scandium fluoride 24.5g mix the back and add in the corundum crucible; Be warming up to 950 ℃, treat that fused salt melts the kalzium metal 216.0g that the back adds calcium contents 9.4%, treat that kalzium metal melts after; Insulation retailoring 40min adds kalzium metal weight 4% refining agent insulation deliming 40min, takes out crucible; The slagging-off founding demoulding is with 60 ~ 100 ℃ of water coolings.The weighing of removing slag obtains scandium bearing master alloy 211.7g, analyzes through ICP-AES, and containing the scandium amount is 4.76%, the recovery 93.7% of scandium.Other impurity Ca, Na, F equal size are all less than 50ppm.The slag recycling.
Embodiment 5
Take by weighing sodium-chlor 62.4g, Repone K 62.4g, scandium fluoride 47.2g mix the back and add in the corundum crucible; Be warming up to 1000 ℃, treat that fused salt melts the kalzium metal 208.0g that the back adds calcium contents 15.3%, treat that kalzium metal melts after; Insulation retailoring 50min adds kalzium metal weight 5% refining agent insulation deliming 30min, takes out crucible; The slagging-off founding demoulding is with 60 ~ 100 ℃ of water coolings.The weighing of removing slag obtains scandium bearing master alloy 203.4g, analyzes through ICP-AES, and containing the scandium amount is 9.43%, the recovery 92.8% of scandium.Other impurity Ca, Na, F equal size are all less than 50ppm.The slag recycling.
Embodiment 6
Take by weighing sodium-chlor 1.67kg, Repone K 1.67kg, scandium fluoride 0.123kg mix the back and add in the corundum crucible; Be warming up to 800 ℃, treat that fused salt melts the kalzium metal 5.57kg that the back adds calcium contents 3.2%, treat that kalzium metal melts after; Insulation retailoring 40min adds kalzium metal weight 5% refining agent insulation deliming 30min, takes out crucible; The slagging-off founding demoulding is with 60 ~ 100 ℃ of water coolings.The weighing of removing slag obtains scandium bearing master alloy 5.54Kg, analyzes through ICP-AES, and containing the scandium amount is 2.12%, the recovery 94.2% of scandium.Other impurity Ca, Na, F equal size are all less than 50ppm.The slag recycling.
Claims (8)
1. a kalzium metal thermal reduction prepares the method for scandium bearing master alloy, it is characterized in that comprising:
1) component content by scandium bearing master alloy calculates required raw material kalzium metal, the halogenide of scandium or the weight of its fused salt and alkali metal chloride of every stove smelting, takes by weighing respectively;
2) halogenide of scandium or its fused salt and alkali metal chloride mixed to add in the crucible be warming up to 750 ℃ ~ 950 ℃ thawings, fusion contain the scandium fused salt;
3) kalzium metal is added said fusion and contain in the scandium fused salt, treat that kalzium metal melts back heat preservation hot reductase 12 0 ~ 200min;
4) treat that thermal reduction reaction is accomplished after, add excessive refining agent and carry out deliming, when treating that calcium contents is less than 50ppm in the alloy, cast ingot casting and cooling, the water logging slagging-off promptly obtains scandium bearing master alloy.
2. kalzium metal thermal reduction according to claim 1 prepares the method for scandium bearing master alloy, it is characterized in that: in the said kalzium metal, by weight, calcium contents is 3% ~ 20%, and surplus is aluminium and unavoidable impurities.
3. kalzium metal thermal reduction according to claim 2 prepares the method for scandium bearing master alloy; It is characterized in that: the halogenide of described scandium is that the anhydrous scandium halide that makes of chemical method or its contain the scandium fused salt; Said anhydrous scandium halide is anhydrous chlorides of rase scandium, anhydrous scandium fluoride, anhydrous scandium bromide or anhydrous scandium iodide; Require dehydration fully, scandium halide content is 1% ~ 25% of fused salt amount.
4. kalzium metal thermal reduction according to claim 3 prepares the method for scandium bearing master alloy; It is characterized in that: described alkali metal chloride is one or both a mixture of sodium-chlor, Repone K; The weight ratio of sodium-chlor and Repone K is in the mixture: 75-98:25-2, the consumption of alkali metal chloride are 0.1 ~ 1.5 times of kalzium metal weight.
5. kalzium metal thermal reduction according to claim 4 prepares the method for scandium bearing master alloy, it is characterized in that: described crucible is plumbago crucible, corundum crucible, iron crucible or tantalum crucible.
6. kalzium metal thermal reduction according to claim 5 prepares the method for scandium bearing master alloy, it is characterized in that: described refining agent is the refining slag system that ALUMNIUM FLUORIDE, sodium aluminum fluoride are formed, and refining agent adopts a kind of of following two kinds of schemes, all by mass ratio:
1. 40%Na
3AlF
6The fused salt mixt of+40%NaCl+20%KCl;
2. 40%Na
3AlF
6The fused salt mixt of+60%NaCl.
7. kalzium metal thermal reduction according to claim 6 prepares the method for scandium bearing master alloy, it is characterized in that: the said type of cooling is to adopt 60 ~ 100 ℃ water cooling.
8. kalzium metal thermal reduction according to claim 1 prepares the method for scandium bearing master alloy, it is characterized in that: 4) back slag recovering step in addition, adopt direct water logging with slag; Immersion liquid is used as flux through the evaporative crystallization continued; Soak slag under 180 ~ 200 ℃, add the vitriol oil and leach, the tail gas that produces in the acidleach process adopts alkali lye to absorb; After soaking slag acidleach fully, after dilution, extracting and separating, purification recyclable scandium.
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| WO2014138813A1 (en) * | 2013-03-15 | 2014-09-18 | Commonwealth Scientific And Industrial Research Organisation | Production of aluminium-scandium alloys |
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| CN108118202A (en) * | 2017-12-28 | 2018-06-05 | 包头稀土研究院 | The method that calciothermy prepares aluminium yttrium intermediate alloy |
| US11384412B2 (en) | 2018-01-16 | 2022-07-12 | Scandium International Mining Corporation | Direct scandium alloying |
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| CN114288837B (en) * | 2021-12-13 | 2022-09-16 | 中国科学院上海应用物理研究所 | Chemical decarburization device and chemical decarburization method for halide molten salt |
| CN115261620B (en) * | 2022-05-23 | 2024-04-26 | 中国恩菲工程技术有限公司 | Method for preparing metal scandium by metallothermic reduction and application of metal scandium |
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|---|---|---|---|---|
| WO2014138813A1 (en) * | 2013-03-15 | 2014-09-18 | Commonwealth Scientific And Industrial Research Organisation | Production of aluminium-scandium alloys |
| AU2013201572A1 (en) * | 2013-03-15 | 2014-10-02 | Commonwealth Scientific And Industrial Research Organisation | Production of Aluminium-Scandium Alloys |
| AU2013201572B2 (en) * | 2013-03-15 | 2014-12-11 | Commonwealth Scientific And Industrial Research Organisation | Production of Aluminium-Scandium Alloys |
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