CN105671598A - Method for directly preparing aluminum foil through low temperature electrolysis - Google Patents

Method for directly preparing aluminum foil through low temperature electrolysis Download PDF

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Publication number
CN105671598A
CN105671598A CN201610217913.8A CN201610217913A CN105671598A CN 105671598 A CN105671598 A CN 105671598A CN 201610217913 A CN201610217913 A CN 201610217913A CN 105671598 A CN105671598 A CN 105671598A
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deposition
ionic liquid
aluminum foil
aluminum
electrode
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涂贤能
张锁江
郎海燕
石朝辉
高洁
蔡迎军
张军玲
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Institute of Process Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/04—Wires; Strips; Foils
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/42—Electroplating: Baths therefor from solutions of light metals
    • C25D3/44—Aluminium

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

The invention discloses a method for directly preparing an aluminum foil through electrolysis at low temperature in an ionic liquid medium.Not only is the problem that a compact deposition layer is difficult to strip in the electrodeposition process of metallic aluminum in ionic liquid solved, but also a novel approach is provided for electrochemical preparation of the aluminum foil.The method is characterized in that a higher nucleation overpotential of metallic aluminum on a carbon cathode is utilized, a compact deposition layer is formed, and meanwhile the compatibility between the metallic aluminum and carbon material lattices is poor, so that the compact aluminum foil on the surface of the cathode is easy to strip.According to the method for directly preparing the aluminum foil through electrolysis, the low-temperature ionic liquid serves as the electrolyte, a carbon material with a smooth surface serves as the cathode, and by means of the characteristics that the ionic liquid is low in melting point and not prone to volatilization, the metallic aluminum foil is successfully prepared within the low-temperature range of 25 DEG C-100 DEG C.The method for directly preparing the aluminum foil through electrolysis has the advantages that the operation temperature is low, and the technological steps are simple and easy to operate; continuous production is easy to achieve, and the production energy consumption and cost of the aluminum and the aluminum foil can be significantly reduced.The method has a good application prospect in the aspect of preparation of the metallic aluminum and aluminum foil through low-temperature electrolysis.

Description

A kind of low-temperature electrolytic directly prepares the method for aluminium foil
Technical field
The invention belongs to electrolysis field, relate to a kind of Low-temperature electro-deposition and prepare the new method of aluminium foil.
Background technology
Aluminum i ndustry is one of electrochemical industry maximum in the world, and because it has the performance of a series of excellences such as density is little, plasticity is strong, the yield of primary aluminum and the recycling amount of aluminum are also in quick growth. By the end of the end of the year 2014, world's electrolytic aluminium annual production has reached 53,900,000 tons, and the yield of Chinese Aluminium accounts for the 45% of Gross World Product. Reduction potential relatively negative (deposition potential less than hydrogen) because of aluminum, it is impossible to electrolysis in aqueous as the non-ferrous metals such as Cu, Zn, Pb. In more than 100 year of past, the production of primary aluminum all adopts Hall Heroult process (Hall-H é roult), the method be at the temperature of about 950 DEG C by alumina dissolution in melted cryolite, and carry out electrolysis with unidirectional current. Electric tank cathode product is aluminum liquid, and anodic product is then CO2, the material such as CO and HF. Although Hall Heroult process also exists electrolysis temperature height, energy consumption is high, pollute the problems such as weight and product quality low (～99.5%), the method is still current industrial unique primary aluminum preparation method.
Scientists is exploring the alternative method that aluminum produces always untiringly, and these methods mainly include carbothermic method, low temperature molten salt electrolysis method and organic system electrolysis. Aluminum is difficult to be reduced, and the carbon thermal reduction of aluminum to carry out at about 2000 DEG C, and low-temperature molten salt method also to carry out electrolysis at 700 DEG C, and both has the problem that pyroprocess is common, as energy consumption is high, equipment corrosion is serious, pollutant discharge amount is big, production cost is high. Organic system electrolysis can overcome the problems referred to above to a certain extent, but organic system to have electrochemical window narrower, the shortcomings such as electrical conductivity is low, volatile, inflammable, limit the method commercial Application in prepared by metallic aluminium.
As far back as 1948, Hurley etc., when finding the electrolyte of electrolysis of aluminum oxide, obtained a kind of colourless liquid after N-ethylpyridinium chloride and AlCl3 being mixed, this liquid is chlorine aluminic acid type ionic liquid, is also referred to as first generation ionic liquid.Ionic liquid is a kind of desirably room temperature liquid electrolyte, it is non-volatile, nonflammable, generally there is good electric conductivity and wider electrochemical window, the reaction of the relatively active metal such as electrolytic aluminium, magnesium, titanium can be carried out under room temperature, both overcome aqueous solution electrolysis and cannot obtain a difficult problem for active metal, also overcome the high-temperature molten salt deep-etching to equipment, reduce the energy consumption of electrolytic process and the discharge of pollutant, it is expected to realize the green production of metallurgical process, makes traditional electrochemistry metallurgical technology generation revolutionary variation.
Different from conventional Hall method electrolytic aluminium, because of electrolytic aluminium reaction temperature relatively low (25 DEG C～100 DEG C) in ionic liquid, aluminum product exists in solid form. The aluminum product of solid-state usually exists with aluminium powder form, and aluminium powder is separated into, with electrolyte, the difficult problem that this Technology is amplified. Meanwhile, aluminum crystal growth in the deposition process of negative electrode easily produces dendrite, has had a strong impact on the stability of long-term electrolytic process.
ReddyR.G. wait research to find, the back side of electrode covered with nonconducting adhesive tape, thus electrode is modified, can pass through electrodeposition process in chlorine Ion-selective electrod at the bottom of at cuprio on produce the deposition layer of densification. Etc. ChangeJ.K. report at Mg alloy surface, the deposited aluminum layer of densification can also be obtained by ionic liquid low-temperature electro-deposition. ZhangS.J. research is waited to find to be added by suitable Organic substance, it is possible to be obtained the al deposition layer of bright in mirror surface on cathode or stainless steel cathode by ionic liquid low temperature deposition method. It should be noted that, the dense deposited layer that said method obtains is all in metal surface, owing to metallic cathode and al deposition layer Lattice Matching are better, deposition layer is difficult to strip off from substrate, therefore the method is only suitable for the modification of metal surface, is difficult to the electrolysis for the purpose of aluminum product or refining process.
The important innovations of the present invention is that smooth carbon cathode introduces the electrodeposition process of pure aluminum, first deposit different from the body on aluminum negative electrode, the research of the present invention finds the nucleation overpotential (accompanying drawing 1) that aluminum is higher on carbon cathode surface, can produce the deposition layer of densification on carbon electrode; Simultaneously as non-metal carbon is bigger with metallic aluminium lattice structure gap so that the surface combination power of the two is more weak, facilitates dense deposited layer and strips off from smooth carbon electrodes, makes product become easy with separating of electrode. The present invention is at 25～100 DEG C, and being successfully prepared diameter is 1cm, and thickness is at the bright aluminium foil of 10～100 μm.
Summary of the invention
The invention provides a kind of method that under low temperature, Direct Electrolysis prepares aluminium foil in ion liquid medium, its Core-technology is that the nucleation overpotential utilizing metallic aluminium higher on carbon cathode forms dense deposited layer, metallic aluminium is poor with material with carbon element lattice simultaneously, the fine and close aluminium foil making cathode surface is more weak with carbon electrode adhesive force, and aluminium foil is prone to and electrode separation. The method has that electrolysis temperature is low, processing step is simple to operation, be easily achieved continuous production, can significantly reduce aluminum and the advantage such as aluminium foil energy consumption and cost. Concrete technical scheme is as follows:
The method that Direct Electrolysis prepares aluminium foil at 25 DEG C～100 DEG C, first the aluminum source of chemical combination state is dissolved in ion liquid system, with ganoid material with carbon element for negative electrode, inert electrode or high pure metal aluminum are anode, carrying out constant voltage and Constant Electric Current deposition, electro-deposition product obtains aluminium foil after peeling off from electrode surface after Organic substance cleans and separates.
The present invention prepares the method for aluminium foil, and the described aluminium compound being dissolved in ionic liquid is anhydrous AlCl3With anhydrous AlBr3In one, its concentration in il electrolyte is 0.9M～2.7M.
The present invention prepares the method for aluminium foil, described ionic liquid cation be imidazole type, pyridine type, quaternary ammonium type, season type, Bi Kaxing, piperidines type, morpholine type and sulfonium salt type, the substituent group in its structure is alkyl, the one in alkoxyl, fluorine or hydrogen; Anion is F-、Cl-、Br-、I-、BF4 -、PF6 -[N (CF3SO2)2]-。
The present invention prepares the method for aluminium foil, and in described ionic liquid, in electro-deposition aluminium foil system, negative electrode is the material with carbon elements such as ganoid graphite, glass carbon, carbon fiber, and its surface roughness should be not more than 0.5 μm; In described anode, inert anode is the one in glass-carbon electrode and platinum electrode, and active anode is rafifinal.
The present invention prepares the method for aluminium foil, and in described deposition process, electric current density during galvanostatic deposition is 1.0～6.5A/dm2, during constant voltage deposition, voltage range is-1.5V～-3.2V.
The present invention prepares the method for aluminium foil, and first the aluminium foil that described electro-deposition obtains cleans, with DMF, the ionic liquid separating surface with after negative electrode mechanical separation, then dries up with cold nitrogen.
The present invention prepares the method for aluminium foil, its preferred condition be 50 DEG C containing 1.5MAlCl3Chlorination 1-butyl-3-Methylimidazole. [BmimCl] ionic liquid in, adopt the surface roughness glass carbon less than 0.5 μm as negative electrode, constant current density 4.0A/dm2Electrolysis 2h, product carries out repeatedly washing and obtains the aluminium foil of light, and its pattern and composition are shown in accompanying drawing 2 and accompanying drawing 3.
Accompanying drawing explanation
On Fig. 1 difference negative electrode deposition process time-measuring electric potential curve
The aluminium foil of deposition on Fig. 2 diameter 1cm glass carbon cathode
Deposition 1hSEM under 4A/dm2 figure at Figure 35 0 DEG C
Detailed description of the invention
Embodiment 1
By AlCl3Being dissolved in [BMIMCl] ionic liquid, active material concentration is 0.9M, and negative electrode is diameter is the glass carbon disk electrode of 3mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Constant voltage electro-deposition, running voltage is-1.5V, and temperature is 25 DEG C, it is electrodeposited in cathode surface through 3h and obtains fine and close aluminium foil, electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 2
By AlCl3It is dissolved in [PP14Cl] in ionic liquid, active material concentration is 1.3M, negative electrode is diameter is the glass carbon disk electrode of 3mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Constant voltage electro-deposition, running voltage is-1.8V, and temperature is 50 DEG C, it is electrodeposited in cathode surface through 3h and obtains fine and close aluminium foil, electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 3
By AlCl3It is dissolved in [N2222Cl] in ionic liquid, active material concentration is 1.5M, negative electrode is diameter is the glass carbon disk electrode of 3mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Constant voltage electro-deposition, running voltage is-2.3V, and temperature is 25 DEG C, it is electrodeposited in cathode surface through 2h and obtains fine and close aluminium foil, electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 4
By AlCl3It is dissolved in [S444Cl] in ionic liquid, active material concentration is 2.0M, negative electrode is diameter is the glass carbon disk electrode of 10mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Constant voltage electro-deposition, running voltage is-2.5V, and temperature is 40 DEG C, it is electrodeposited in cathode surface through 2h and obtains fine and close aluminium foil, electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 5
By AlCl3Being dissolved in [BMIMCl] ionic liquid, active material concentration is 2.3M, and negative electrode is diameter is the glass carbon disk electrode of 10mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Constant voltage electro-deposition, running voltage is-3.2V, and temperature is 50 DEG C, it is electrodeposited in cathode surface through 2h and obtains fine and close aluminium foil, electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 6
By AlCl3It is dissolved in [Py14Cl] in ionic liquid, active material concentration is 2.7M, negative electrode is diameter is the glass carbon disk electrode of 3mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Galvanostatic deposition, electric current density is 1.0A/dm2, temperature is 60 DEG C, is electrodeposited in cathode surface through 4h and obtains fine and close aluminium foil, and electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 7
By AlCl3It is dissolved in [N4441Cl] in ionic liquid, active material concentration is 2.7M, negative electrode is diameter is the glass carbon disk electrode of 10mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Galvanostatic deposition, electric current density is 3.0A/dm2, temperature is 80 DEG C, is electrodeposited in cathode surface through 4h and obtains fine and close aluminium foil, and electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.
Embodiment 8
By AlCl3It is dissolved in [PP13Cl] in ionic liquid, active material concentration is 2.7M, negative electrode is diameter is the glass carbon disk electrode of 10mm, and anode is inertia glass-carbon electrode, and reference electrode is aluminium wire. Galvanostatic deposition, electric current density is 6.5A/dm2, temperature is 100 DEG C, is electrodeposited in cathode surface through 2h and obtains fine and close aluminium foil, and electro-deposition aluminium foil first passes through dichloromethane and repeatedly washs to ensure that ionic liquid cleans up, then dried up by product with cold nitrogen after peeling off from cathode surface.

Claims (6)

1. the method that under a low temperature, Direct Electrolysis prepares aluminium foil, it is characterized in that: dissolved with in the ion liquid system of aluminium compound, with ganoid material with carbon element for negative electrode, inert electrode or high pure metal aluminum are anode, carrying out constant voltage and Constant Electric Current deposition at 25 DEG C～100 DEG C, electro-deposition product obtains aluminium foil after peeling off from electrode surface after Organic substance cleans and separates.
2. method according to claim 1, it is characterised in that: the aluminium compound being dissolved in ionic liquid is anhydrous AlCl3With anhydrous AlBr3In one.
3. method according to claim 1, it is characterised in that: ionic liquid cation be imidazole type, pyridine type, quaternary ammonium type, season type, Bi Kaxing, piperidines type, morpholine type and sulfonium salt type, its structure is as follows, R1、R2、R3、R4、R5、R6、R7Represent alkyl, alkoxyl, fluorine or hydrogen; Anion is F-、Cl-、Br-、I-、BF4 -、PF6 -[N (CF3SO2)2]-。
4. method according to claim 1, it is characterised in that: in described ionic liquid, in electro-deposition aluminium foil system, negative electrode is ganoid graphite, glass carbon, carbon fiber carbon material, and its surface roughness should be not more than 0.5 μm; In described anode, inert anode is the one in glass-carbon electrode and platinum electrode, and active anode is rafifinal.
5. method according to claim 1, it is characterised in that: described aluminum soluble salt concentration in il electrolyte is 0.9M～2.7M;In described deposition process, electric current density during galvanostatic deposition is 1.0～6.5A/dm2, during constant voltage deposition, voltage range is-1.5V～-3.2V.
6. method according to claim 1, it is characterised in that: first electro-deposition aluminium foil cleans, with dichloromethane, the ionic liquid separating surface after peeling off from cathode surface, then dries up with cold nitrogen.
CN201610217913.8A 2016-04-08 2016-04-08 Method for directly preparing aluminum foil through low temperature electrolysis Pending CN105671598A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108166021A (en) * 2017-12-27 2018-06-15 中国人民大学 A kind of method of the low-temperature electrolytic aluminium in depth congruent melting solvent
CN111118548A (en) * 2020-03-05 2020-05-08 吴君石 Method for preparing aluminum by low-temperature constant-current electrolysis of composite ionic liquid electrolyte system
CN117328111A (en) * 2023-12-01 2024-01-02 中铝材料应用研究院有限公司 Composite aluminum foil and preparation method thereof

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WO2015125899A1 (en) * 2014-02-20 2015-08-27 日立金属株式会社 Electrolytic aluminum foil, current collector for power storage device, electrode for power storage device, and power storage device
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108166021A (en) * 2017-12-27 2018-06-15 中国人民大学 A kind of method of the low-temperature electrolytic aluminium in depth congruent melting solvent
CN108166021B (en) * 2017-12-27 2019-10-11 中国人民大学 A method of the low-temperature electrolytic aluminium in depth congruent melting solvent
CN111118548A (en) * 2020-03-05 2020-05-08 吴君石 Method for preparing aluminum by low-temperature constant-current electrolysis of composite ionic liquid electrolyte system
CN117328111A (en) * 2023-12-01 2024-01-02 中铝材料应用研究院有限公司 Composite aluminum foil and preparation method thereof
CN117328111B (en) * 2023-12-01 2024-03-08 中铝材料应用研究院有限公司 Composite aluminum foil and preparation method thereof

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Application publication date: 20160615