CN103849897A - Method of preparing metal aluminum - Google Patents
Method of preparing metal aluminum Download PDFInfo
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- CN103849897A CN103849897A CN201410072391.8A CN201410072391A CN103849897A CN 103849897 A CN103849897 A CN 103849897A CN 201410072391 A CN201410072391 A CN 201410072391A CN 103849897 A CN103849897 A CN 103849897A
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- aluminum oxide
- metallic aluminium
- fluoride
- ionogen
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Abstract
The invention discloses a method of preparing metal aluminum. The method comprises the following steps: preparing aluminum oxide by utilizing an acid process; and carrying out electrolytic treatment onto the aluminum oxide to obtain the metal aluminum. According to the method of preparing the metal aluminum in the embodiment of the invention, the aluminum oxide is prepared by adopting acid-process leaching treatment, and then, metal aluminum prepared by carrying out electrolytic treatment onto the aluminum oxide has higher purity and satisfies national standards; and moreover, industrial production needs can be satisfied.
Description
Technical field
The invention belongs to field of metallurgy, particularly, the present invention relates to a kind of method of preparing metallic aluminium.
Background technology
Aluminum oxide is the main raw material of Aluminium Electrolysis.Aluminum oxide physicals comprises: true specific gravity, capacity, granularity, specific surface area, angle of repose and coefficient of wear.The physicals of aluminum oxide, for ensureing that electrolytic process normally carries out, the technico-economical comparison and the environment protection relation that improve electrolytic process are very large.Therefore except chemical composition, the physicals of aluminum oxide has also been proposed to following requirement: (1) solubleness in ionogen is large, and dissolution rate is fast; (2) good fluidity, is convenient to pneumatic conveying and from feed bin to electrolyzer self-feeding; (3) Dust Capacity is little, carry and dust collector when reinforced few, there is good surfactivity, can effectively adsorb HF gas; (4) good heat insulating can form good crust on ionogen, to shield electrolyte melt, reduces thermosteresis; (5) can cover closely on anode carbon block, prevent that anode carbon block is oxidized in air, reduce anode consumption.
At present domestic aluminum oxide is to refine from bauxite on substantially, prepares aluminum oxide at the industrial alkaline process that only has being applied, and therefore acid system is prepared aluminum oxide and need further research.
Summary of the invention
The present invention is intended at least solve one of technical problem existing in prior art.For this reason, one object of the present invention is to propose a kind of method of preparing metallic aluminium, and the purity of metallic aluminium prepared by the method is high, meets national standard.
In one aspect of the invention, the present invention proposes a kind of method of preparing metallic aluminium, the method comprises:
Utilize acid system to prepare aluminum oxide; And
Described aluminum oxide is carried out to electrolysis treatment, to obtain described metallic aluminium.
According to the method for preparing metallic aluminium of the embodiment of the present invention, prepare aluminum oxide by adopting acid system to leach and processing, then aluminum oxide is carried out to metallic aluminium prepared by electrolysis treatment and there is higher purity, meet national standard, and can meet the demand of suitability for industrialized production.
In addition, the method for preparing metal according to the present invention also can have following additional technical feature:
In some embodiments of the invention, describedly utilize acid system to prepare aluminum oxide to comprise the following steps: to utilize ammonium fluoride solution to carry out immersion treatment to aluminous fly-ash, to obtain soak solution; In described soak solution, add sulphuric acid soln and leach processing, to obtain alum liquor; Described alum liquor and sulfate of ammoniac solution are carried out to combination treatment, to obtain ten sulfate dihydrate aluminium ammonium crystal; And described ten sulfate dihydrate aluminium ammonium crystal are carried out to calcination processing, to obtain described aluminum oxide.Thus, can significantly improve the productive rate of aluminum oxide.
In some embodiments of the invention, the purity of described aluminum oxide is 99.4 % by weight.Thus, can significantly improve the purity of metallic aluminium.
In some embodiments of the invention, the ionogen of described electrolysis treatment is taking sodium aluminum fluoride as solvent, and adds additive to prepare in described solvent.Thus, can further improve the purity of metallic aluminium.
In some embodiments of the invention, described additive is at least one being selected from magnesium fluoride and Calcium Fluoride (Fluorspan).Thus, can further improve the purity of metallic aluminium.
In some embodiments of the invention, based on the described ionogen of every 100 grams, described aluminum oxide add-on is that 1.5～3 grams, magnesium fluoride are that 3～5 grams, Calcium Fluoride (Fluorspan) are 4～5 grams.Thus, can further improve the purity of metallic aluminium.
In some embodiments of the invention, in described ionogen, contain: the fluorine element of 35～38wt%; The sodium element of 15～17wt%; The magnesium elements of 0.2～0.3wt%; The aluminium element of 31～35wt%; And the calcium constituent of 1.5～3.5wt%.Thus, can further improve the purity of metallic aluminium.
In some embodiments of the invention, in described ionogen, the mol ratio of Sodium Fluoride and aluminum fluoride is 2.3～2.7.Thus, can further improve the purity of metallic aluminium.
In some embodiments of the invention, described electrolysis treatment is to be 938-945 degree Celsius in temperature, and voltage is to carry out under the condition of 3.90～4.15 volts.Thus, can further improve the purity of metallic aluminium.
In some embodiments of the invention, in described electrolysis treatment process, anode electrode and cathode electrode are carbon material.Thus, can further improve the purity of metallic aluminium.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Brief description of the drawings
Above-mentioned and/or additional aspect of the present invention and advantage accompanying drawing below combination is understood becoming the description of embodiment obviously and easily, wherein:
Fig. 1 is the method flow schematic diagram of preparing according to an embodiment of the invention metallic aluminium;
Fig. 2 is the method flow schematic diagram of preparing metallic aluminium of another embodiment according to the present invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Be exemplary below by the embodiment being described with reference to the drawings, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention, it will be appreciated that, term " first ", " second " be only for describing object, and can not be interpreted as instruction or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more these features can be expressed or impliedly be comprised to the feature that is limited with " first ", " second ".In description of the invention, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
In prior art, aluminum oxide is to refine from bauxite on substantially, and the production method of aluminum oxide has acid system, alkaline process, soda acid associating preheating method.But, the aluminum oxide that adopts acid system to prepare makes it be subject to serious restriction in electrolytic industry field owing to containing compared with the high impurity such as Si, Fe, therefore make it in existing electrolyzer and existing electrolysis system, can meet electrolysis requirement, produce the aluminium ingot that meets national standard, always in the research and development stage.The present inventor, by large quantity research, is intended to probe into can adopt acid oxidation aluminium to carry out electrolysis treatment and preparing metallic aluminium.
For this reason, in one aspect of the invention, the present invention proposes a kind of method of preparing metallic aluminium.Below with reference to Fig. 1-2, the method for preparing metallic aluminium of the present invention is described in detail.According to embodiments of the invention, the method comprises:
S100: acid system is prepared aluminum oxide
According to embodiments of the invention, adopt acid system to prepare aluminum oxide.The process of acid system being prepared to aluminum oxide below with reference to Fig. 2 is described in detail.According to embodiments of the invention, acid system is prepared alumina process and is comprised the following steps:
S110: immersion treatment
According to embodiments of the invention, utilize ammonium fluoride solution to carry out immersion treatment to aluminous fly-ash, thereby can obtain soak solution.According to embodiments of the invention, in aluminous fly-ash, contain the oxide compounds such as aluminum oxide, silicon-dioxide, ferric oxide and titanium dioxide.In this step, concrete, the aluminum oxide great majority in aluminous fly-ash present vitreous state, aluminum oxide is wherein nonactive body, therefore use ammonium fluoride solution as solubility promoter, aluminum oxide can be discharged from vitreum, thereby can significantly improve the productive rate of aluminum oxide in subsequent reactions.
S120: leach and process
According to embodiments of the invention, in gained soak solution, add sulphuric acid soln and leach processing, thereby can obtain alum liquor.In this step, react as 3H
2sO
4+ 6NH
4f+SiO
2→ H
2siF
6+ 3 (NH
4)
2sO
4+ 2H
2o, 3H
2sO
4+ Al
2o
3→ Al
2(SO
4)
3+ 3H
2o.
S130: combination treatment
According to embodiments of the invention, gained alum liquor and sulfate of ammoniac solution are carried out to combination treatment, thereby can obtain ten sulfate dihydrate ammonium aluminium crystal.
S140: calcination processing
According to embodiments of the invention, ten sulfate dihydrate aluminium ammonium crystal are carried out to calcination processing, thereby can obtain aluminum oxide.According to embodiments of the invention, the purity of gained aluminum oxide can be 99.40 % by weight, the sodium oxide of the silicon-dioxide that wherein, contains 0.010～0.020 % by weight in gained aluminum oxide, the ferric oxide of 0.035～0.045 % by weight, 0.40～0.45 % by weight, the titanium dioxide of 0.0005～0.0010 % by weight, the Vanadium Pentoxide in FLAKES of 0.002～0.003 % by weight and the Vanadium Pentoxide in FLAKES of 0.0590～0.0595 % by weight.
S200: electrolysis treatment
According to embodiments of the invention, above gained aluminum oxide is carried out to electrolysis treatment, thereby can obtain metallic aluminium.According to embodiments of the invention, the ionogen using in electrolysis treatment process is also not particularly limited, according to a particular embodiment of the invention, the ionogen that electrolysis treatment process is used can be taking sodium aluminum fluoride as solvent, and adds additive to prepare in solvent.According to embodiments of the invention, use the particular type of additive and be not particularly limited, according to a particular embodiment of the invention, additive can be for being selected from least one in magnesium fluoride and Calcium Fluoride (Fluorspan).According to embodiments of the invention, based on the ionogen of every 100 grams, aluminum oxide add-on can be that 1.5～3 grams, magnesium fluoride can be that 3～5 grams, Calcium Fluoride (Fluorspan) can be 4～5 grams.According to embodiments of the invention, in ionogen, can contain: the calcium constituent of the magnesium elements of the fluorine element of 35～38wt%, the sodium element of 15～17wt%, 0.2～0.3wt%, the aluminium element of 31～35wt%, 1.5～3.5wt% and content is not all higher than element silicon, potassium element, nickel element and the phosphoric of 0.1wt%.
According to a particular embodiment of the invention, being also not particularly limited containing the composition of lithium aluminum fluoride in above-mentioned additive, what for example preferably adopt can comprise containing in lithium aluminum fluoride: 60～62% fluorion, 31～33% aluminum ion, 1～2% lithium ion.What have thus said components can provide for ionogen the lithium ion of q.s containing lithium aluminum fluoride salt, to reduce electrolytical resistivity, thereby reduces pole span.
According to embodiments of the invention, the content of Sodium Fluoride and aluminum fluoride being not particularly limited in ionogen, according to a particular embodiment of the invention, in ionogen, the mol ratio of Sodium Fluoride and aluminum fluoride can be 2.3～2.7.Contriver finds, in ionogen, the mol ratio of Sodium Fluoride and aluminum fluoride is less than at 3 o'clock, it is acid that ionogen is, the mol ratio of Sodium Fluoride and aluminum fluoride is greater than at 3 o'clock, ionogen is alkalescence, and the mol ratio of Sodium Fluoride and aluminum fluoride is conducive to reduce electrolysis temperature when lower, reduce secondary reaction, improve current efficiency, but mol ratio is too low, cause alumina dissolution degree to reduce, in groove, easily produce a large amount of precipitations, and mol ratio is when too high, electrolysis temperature is higher, current efficiency reduces, therefore selecting the mol ratio of Sodium Fluoride and aluminum fluoride in ionogen is between 2.3～2.7 scopes, both to have improved current efficiency, can improve again alumina dissolution degree.
According to embodiments of the invention, the electrode that electrolysis treatment process is used is also not particularly limited, and according to a particular embodiment of the invention, the anode electrode that electrolysis treatment process is used and cathode electrode can be carbon material.Particularly, in electrolysis treatment process, the reaction that anode electrode occurs is: C+2O
2-(coordination ion) – 4e=CO
2↑, and cathode electrode does not participate in reaction, only plays conduction, the reaction that wherein negative electrode occurs is: Al
3+(coordination ion)+3e=Al.
According to embodiments of the invention, the condition of electrolysis treatment is also not particularly limited, and according to a particular embodiment of the invention, electrolysis treatment can be 938～945 degrees Celsius in temperature, and voltage is to carry out under the condition of 3.90～4.15 volts.Contriver's discovery, the electrolysis treatment of carrying out under this condition can obtain the metallic aluminium of higher degree.
Prepare the method for metallic aluminium according to the embodiment of the present invention, show good solubility, diffustivity and electroconductibility by adopting acid system leaching to process the aluminum oxide preparing, thereby can adapt to existing electrolyte system completely, and adopt this aluminum oxide to carry out metallic aluminium prepared by electrolysis treatment and there is higher purity, therefore can meet the demand of industrial sector.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiment are only descriptive, and do not limit the present invention in any way.
Embodiment
1, the preparation of acid oxidation aluminium
First to aluminium sesquioxide mass content, the aluminous fly-ash more than 30% carries out iron removal by magnetic separation, adds wherein a small amount of ammonium fluoride solution after deironing, and aluminous fly-ash is carried out to immersion treatment, obtains soak solution; To add concentration in soak solution be 40% sulphuric acid soln and fully mix, and under the pressure of 0.9MPa and 160 degrees Celsius, carry out agitation leach and process 1.5～2 hours, obtain alum liquor, Al is with Al
2(SO
4)
3form from flyash, leach; Alum liquor and sulfate of ammoniac solution are carried out to combination treatment, obtain ten sulfate dihydrate aluminium ammonium crystal (NH
4al(SO
4)
212H
2o); Finally ten sulfate dihydrate aluminium ammonium crystal are calcined and obtained acid oxidation aluminium under 960 degrees Celsius.Wherein, acid consumption is that aluminum oxide per ton consumes 40～70 kilograms, sulfuric acid.
2, the preparation work before test
1) adopt electrolyzer to carry out the test of acid oxidation aluminium uniform blanking, understand its mobility in existing cylinder feeder and the weight in average value of homogeneity and each discharge quantity.Day-to-day test 20 times, average, continuously tested (is put the material in alumina reservoir on electrolytic bath totally for 3 days as far as possible, cut off electrolyzer aluminum oxide feeder system, do not affect the aluminum oxide feed that other produce groove, electrolytic bath material loading case lid is dismantled, by manually adding acid oxidation aluminium, after having tested, put clean hopper clout);
2) test and electrolyzer was carried out taking inventory at product aluminium in first 6 days, and anode change is adjusted to mornig shift and change, and measure aluminium level under anode, stove side, finds out burner hearth situation;
3) test measurement collection shell temperature first 1 week every day (just temperature of fenestella temperature, bottom temperature, side), averages so that reference relatively in process of the test;
4) in test the last week, control processing parameter well, guarantee that groove condition operational excellence (requires: aluminium level >=25cm; More than electrolyte level >=16cm; 938～945 DEG C of groove temperature; In ionogen between the mol ratio 2.3～2.7 of Sodium Fluoride and aluminum fluoride);
5) reinforced previous class stops feed, treats to remove hopper top cover before hopper material is finished, and removes feeder system, empties hopper.
3, acid oxidation al dissolution test
1) before reinforced, the shell temperature of measurement electrolyzer, electrolysis temperature, bath voltage, two levels, molecular ratio, alumina concentration, pole span, furnace bottom pressure drop, aluminium liquid Chemical Composition etc.;
2) reinforced test: acid oxidation aluminium is added to electrolyzer (mulch is also used acid oxidation aluminium instead when the change poles) with the feed rate of every 30 minutes 30kg, continue one week, observe and record " acid oxidation aluminium " and dissolve and spread condition in ionogen, fluoride salt addition is by condition of production control;
3) test after feeding intake
First week, the variation of getting alumina concentration in two ionogen samples and aluminium liquid sample analysis ionogen every day between aluminium flowing-out mouth and rear large B4 and B5, observed simultaneously and records anode electrolytic cell effect situation and bearth precipitation situation, and other conventionally tests remain unchanged;
Second week, between aluminium flowing-out mouth and rear large B4 and B5, get two ionogen samples and aluminium liquid sample every day and analyze alumina concentration, the variation of Chemical Composition and the variation of aluminium liquid Chemical Composition in ionogen, observe simultaneously and record anode electrolytic cell effect situation, two horizontal changing conditions and bearth precipitation situation, other conventionally tests remain unchanged.
4, production test
1) feed way
Acid oxidation aluminium is joined in the alumina reservoir on the electrolytic bath having emptied and (on acid oxidation aluminium, before groove, need to measure bulk density), open the control of computer alumina blanking, start production test;
2) determining of test technology technical parameter
Adjust NB interval according to the physical properties of acid oxidation aluminium (bulk density) and acid oxidation aluminium uniform blanking test-results, maintain bath voltage, electrolysis temperature and the aluminium level of diffustivity test, and according to test in place situation, above-mentioned parameter is adjusted, carry out to maintain the stable of test;
3) test of the each production and technical indication of duration of test
In process of the test, need test and record following parameters every day: bath voltage, molecular ratio, electrolyte level, aluminium level, electrolysis temperature, shell temperature, anode effect coefficient, alumina concentration, aluminium liquid Chemical Composition; Weekly composition of electrolyte is analyzed and record; At the beginning of duration of test every month, adopt to add the mode that copper takes inventory the inherent aluminium amount of producing of electrolyzer is accurately taken inventory, to calculate the of that month current efficiency of test.
4) certain hour is carried out in test, and tissue carries out performance appraisal, for incomplete place, formulates corresponding measure, Continual Improvement.
5, test-results
1) acid oxidation aluminium " three property "
Mobility: good at electrolytic bath feed box and barrel internal mobility, blanking is unobstructed, not putty;
Diffustivity: in the ionogen of chemical examination difference position, alumina content is basic identical, shows that its diffustivity is good;
Solvability: bearth precipitation is few, groove is pressed without abnormal, shows that this alumina dissolution is good.
2) material balance
Computer statistics discharge quantity, addition material amount and the theoretical alumina amount three quantity correspondence that consumes of the aluminium that produces, show in electrolytic tank electrolysis process, to there is good material balance.
3) thermal equilibrium
Thermal equilibrium is mainly reacted from electrolysis temperature, bath voltage and shell temperature.Relatively balance of groove temperature on the whole, generally at 940～950 DEG C, in the short period of time, fluctuation not quite, illustrates that thermal equilibrium is in a more stable state; And from the temperature of pot shell, shell temperature within the scope of 310～350 DEG C, belongs to safety value substantially, and numerical fluctuations is less, therefore duration of test electrolyzer is safer; Meanwhile, duration of test stove side keeps 10cm left and right always, the 9cm left and right of stretching one's legs; Above data show that in acid oxidation electrolysis of aluminum process of the test, thermal balance state is better.
4) metallic aluminium purity test
The purity that records gained metallic aluminium is more than 99.7%, to meet national standard.
Conclusion: acid oxidation aluminium can adapt to existing electrolyte system completely, shows good solubility, diffustivity and electroconductibility; Duration of test electrolytic bath current efficiency 90.3%, average voltage 4.1V, and every the ton aluminum direct current consumes is 13530kWh; Through test, acid oxidation aluminium can be produced standard compliant aluminium ingot in existing electrolyzer and existing electrolyte system, can meet the requirement of industrialization, can carry out Industry Promotion.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " illustrative examples ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, the schematic statement of above-mentioned term is not necessarily referred to identical embodiment or example.And specific features, structure, material or the feature of description can be with suitable mode combination in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: in the situation that not departing from principle of the present invention and aim, can carry out multiple variation, amendment, replacement and modification to these embodiment, scope of the present invention is limited by claim and equivalent thereof.
Claims (10)
1. a method of preparing metallic aluminium, is characterized in that, comprising:
Utilize acid system to prepare aluminum oxide; And
Described aluminum oxide is carried out in ionogen to electrolytic reaction, to obtain described metallic aluminium.
2. the method for preparing metallic aluminium according to claim 1, is characterized in that, describedly utilizes acid system to prepare aluminum oxide to comprise the following steps:
Utilize ammonium fluoride solution to carry out immersion treatment to aluminous fly-ash, to obtain soak solution;
In described soak solution, add sulphuric acid soln and leach processing, to obtain alum liquor;
Described alum liquor and sulfate of ammoniac solution are carried out to combination treatment, to obtain ten sulfate dihydrate aluminium ammonium crystal; And
Described ten sulfate dihydrate aluminium ammonium crystal are carried out to calcination processing, to obtain described aluminum oxide.
3. the method for preparing metallic aluminium according to claim 1, is characterized in that, the purity of described aluminum oxide is 99.40 % by weight.
4. the method for preparing metallic aluminium according to claim 1, is characterized in that, described ionogen is taking sodium aluminum fluoride as solvent, and adds additive to prepare in described solvent,
Wherein, described additive is at least one being selected from magnesium fluoride and Calcium Fluoride (Fluorspan).
5. the method for preparing metallic aluminium according to claim 4, is characterized in that, based on the described ionogen of every 100 grams, the content of described sodium aluminum fluoride is 90～93 grams, and the content of described magnesium fluoride is that 3～5 grams, the content of described Calcium Fluoride (Fluorspan) are 4～5 grams.
6. the method for preparing metallic aluminium according to claim 1, is characterized in that, described electrolytic reaction is to add the described aluminum oxide of 1.5～3 grams to carry out in based on every 100 grams of ionogen.
7. the method for preparing metallic aluminium according to claim 4, is characterized in that, in described ionogen, contains:
The fluorine element of 35～38wt%;
The sodium element of 15～17wt%;
The magnesium elements of 0.2～0.3wt%;
The aluminium element of 31～35wt%; And
The calcium constituent of 1.5～3.5wt%.
8. the method for preparing metallic aluminium according to claim 4, is characterized in that, in described ionogen, the mol ratio of Sodium Fluoride and aluminum fluoride is 2.3～2.7.
9. the method for preparing metallic aluminium according to claim 1, is characterized in that, described electrolytic reaction is to be 938～945 degrees Celsius in temperature, and voltage is to carry out under the condition of 3.90～4.15 volts.
10. the method for preparing metallic aluminium according to claim 1, is characterized in that, anode electrode and cathode electrode that described electrolytic reaction adopts are carbon material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107201534A (en) * | 2017-05-27 | 2017-09-26 | 重庆旗能电铝有限公司 | One kind goes out aluminium task computation method |
| CN110093631A (en) * | 2019-05-31 | 2019-08-06 | 中国神华能源股份有限公司 | Highly dissoluble acid oxidation aluminium electrolyte system used for aluminium electrolysis and its application |
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| CN102398913A (en) * | 2010-09-14 | 2012-04-04 | 贵阳铝镁设计研究院有限公司 | Process for extracting metallurgical grade alumina through treatment of high alumina fly ash by using sulfuric acid method |
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| CN101284668A (en) * | 2007-04-12 | 2008-10-15 | 清华大学 | Process for abstracting earth silicon, oxide of alumina and gallium oxide from high-alumina flying ash |
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| CN110093631A (en) * | 2019-05-31 | 2019-08-06 | 中国神华能源股份有限公司 | Highly dissoluble acid oxidation aluminium electrolyte system used for aluminium electrolysis and its application |
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| CN103849897B (en) | 2016-06-01 |
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