CN102154661A - Method for preparing aluminum ingot by low-temperature electrolysis of metal monocrystal surface electrodes - Google Patents
Method for preparing aluminum ingot by low-temperature electrolysis of metal monocrystal surface electrodes Download PDFInfo
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Abstract
The invention relates to a method for preparing an aluminum ingot by low-temperature electrolysis of metal monocrystal surface electrodes, which belongs to the field of electrochemistry, metal smelting and the like. The method is characterized by comprising the following steps of: consuming electrolyte, and generating chlorine on an anode to obtain the aluminum ingot on a cathode if the anode is an inert electrode; or sacrificing the anode to obtain the aluminum ingot on the cathode if the anode is a thick aluminum electrode, wherein the used cathode is a monocrystal surface electrode, and used electrolyte solution is AlCl3 type ionic liquid or low-temperature inorganic molten salt.
Description
Technical field
The present invention relates to and a kind ofly prepare the method for aluminium ingot, belong to the Metal smelting field by metal single crystal face electrode low-temperature electrolytic.
Background technology
Aluminium is little because of its density, and electrical and thermal conductivity performance is good, and ductility is good, and the physicochemical property that erosion resistance etc. are good make it be widely used in aspects such as machinofacture, Transport Machinery, power machine, aircraft industry, material of construction, wrapping material, finishing material.
The method of industrial production aluminium mainly is the Hall-Heroult method now, i.e. sodium aluminum fluoride-alumina eltrolysis method.This method keeps the thermal equilibrium of electrolyzer in order to keep the high temperature of reaction, needs a large amount of heat of additive decrementation.Electrolytic aluminum be exactly by consume one times of theoretical electric energy with on keep high groove temperature, cause its capacity usage ratio less than 50%.Therefore realize that low-temperature electrolytic aluminium is to solve one of in-problem important measures of modern aluminum industry.The realization of low-temperature electrolytic aluminium not only helps energy-saving and emission-reduction, and can promote the application of novel material and the exploitation of novel process.Cold condition can be selected novel inert anode material down, consumes carbon anode material minimizing emission of carbon-dioxide thereby break away from, for the exploitation of electrolytic aluminum friendly process is laid a good foundation.
Our country is being in world's antecedent aspect the research of low-temperature electrolytic aluminium, center of gravity mainly is the improvement in conventional high-temperature melting salt system, but temperature is still above 900 ℃.The low-temperature molten salt system more and more is subjected to people's attention, and wherein topmost is exactly inorganic fused salt and organic molten salt.The common system of inorganic fused salt has NaCl-AlCl
3And NaCl-KCl-AlCl
3Deng, organic molten salt is also referred to as ionic liquid at room temperature, generally is made up of metal halide and organic salt.
And abroad just begin low-temperature electrolytic aluminium is studied the fifties from eighties of last century, accumulated rich experience.Mainly contain two big primary structures, melting salt system and organic solvent system.The melting salt system mainly comprises inorganic fused salt and ionic liquid at room temperature.Wherein the inorganic fused salt temperature is generally more than 100 ℃, and the room temperature melting salt new medium that chlorine aluminic acid ionic liquid is a fluid-like state wide ranges, specific conductivity height, electrochemical window is wide, vapour pressure is extremely low has broad prospects in electrolytic aluminum research and application facet.
Chinese patent CN1664170A discloses the method for a kind of producing aluminium under low-temperature and aluminium alloy, is exactly with AlCl
3The type ionic liquid is as low-temperature electrolyte.But they are to be that the raw material chlorination obtains Aluminum chloride anhydrous and further handles and obtain AlCl with aluminum oxide or the mineral that contain aluminosilicate
3The type ionic liquid.Chinese patent CN101265588A also discloses the method that a kind of low-temperature electrolytic generates aluminium, and they adopt bisulfate ion (HSO
4 -) type anion ion liquid dissolved oxygen aluminium, as low-temperature electrolytes, be the direct dc electrolysis of raw material with the aluminum oxide.Li Qingfeng etc. are at low temperature NaCl-AlCl
3Obtain dendroid or how empty shape aluminium lamination in the system.Wang Jihui etc. are at low temperature NaCl-KCl-AlCl
3Obtain needle-like coating in the system.But they have just obtained thin al deposition layer or dendritic aluminium dendrite on electrode.
Summary of the invention
Purpose of the present invention is at the high energy consumption in present industrial electrolysis and the refined aluminum process, and is expensive, and problems such as high environmental pollution provide a kind of and prepare the aluminium ingot method by metal single crystal face electrode low-temperature electrolytic.The low-temperature electrolytic aluminium of bibliographical information, otherwise heavy layer is thin, or grow dendrite; We have adopted the single facet electrode, make the al deposition bed thickness that electrolysis obtains and do not have dendrite to generate.It is low that the present invention has an electrolysis temperature, and advantage such as pollution-free has favorable industrial application prospect.
Of the present inventionly a kind ofly prepare the method for aluminium ingot, with AlCl by metal single crystal face electrode low-temperature electrolytic
3Type ionic liquid or inorganic fused salt are negative electrode as electrolytic solution with metal single crystal face electrode.
Of the present inventionly a kind ofly prepare the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, its feature mainly contain following some:
1) water-content is less than 5ppm, and oxygen level is less than under the 5ppm condition, AlCl
3The type ionic liquid is as electrolytic solution, and noble electrode is as anode, and deposition of aluminum obtains aluminium ingot on metal single crystal face negative electrode;
2) water-content is less than 5ppm, and oxygen level is less than under the 5ppm condition, AlCl
3The type ionic liquid is as electrolytic solution, and the crude aluminum electrode is as anode, and deposition of aluminum obtains aluminium ingot on metal single crystal face negative electrode;
3) in atmosphere of inert gases, the low temperature inorganic fused salt is as electrolytic solution, and the crude aluminum electrode is as anode, and deposition of aluminum obtains aluminium ingot on metal single crystal face negative electrode;
4) in atmosphere of inert gases, the low temperature inorganic fused salt is as electrolytic solution, and noble electrode is as anode, and deposition of aluminum obtains aluminium ingot on metal single crystal face negative electrode.
Above-mentioned a kind ofly prepare in the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, electrolytic solution is AlCl
3The type ionic liquid.AlCl
3The type ionic liquid mainly comprises following several: [Bmim] Cl-AlCl
3(1-butyl-3-Methylimidazole chloro-aluminate), [Emim] Cl-AlCl
3(1-ethyl-3-Methylimidazole chloro-aluminate), [Bdmim] Cl-AlCl
3(1-butyl-2,3-methylimidazole chloro-aluminate), TMBAC-AlCl
3(benzyltrimethylammon.um chloro-aluminate), TEBAC-AlCl
3(benzyltrimethylammon.um chloro-aluminate), BPC-AlCl
3(butylpyridinium chloroaluminate), [Py (1,4)] Tf
2N-AlCl
3(1, the two fluoroform sulfimide chloro-aluminates of 4-pyridine), [Emim] Tf
2N-AlCl
3(the two fluoroform sulfimide chloro-aluminates of 1-ethyl-3-Methylimidazole), [Bmim] Br-AlCl
3(bromination 1-butyl-3-Methylimidazole chloro-aluminate), [Bmim] BF
4-AlCl
3(1-butyl-3-Methylimidazole Tetrafluoroboric acid chloro-aluminate).The AlCl that is prepared
3Anhydrous AlCl in the type ionic liquid
3Shared molar ratio is 1: 1～3: 1.
Above-mentionedly a kind ofly prepare in the method for aluminium ingot AlCl by metal single crystal face electrode low-temperature electrolytic
3The type preparation method of ionic liquid is: with ionic liquid ([Bmim] Cl, [Emim] Cl etc.) thorough drying in vacuum drying oven, put in the vacuum glove box then.With anhydrous AlCl
3According to mol ratio is 1: 1.5 mixed, continues to stir, up to the solution transparent and homogeneous.Contain reasons such as moisture owing to local temperature is too high in the building-up process and generate a little foreign pigment, need the preelectrolysis purifying.Preelectrolysis just is to use two high-purity aluminium flakes of handling well as anode and cathode, adds 1.0V direct current electrolysis 24 hours, and electrolysis temperature maintains about 60 ℃.Purifying is successfully by the cyclic voltammetry test for electrolytic solution, and adopting the platinum filament of two 6mm*6mm is working electrode and counter electrode, and high-purity aluminium wire is done reference electrode, does not have other assorted peak except the redox peak of aluminium.
Above-mentioned a kind ofly prepare in the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, negative electrode is a metal single crystal face electrode.Its characteristics are that metal single crystal face negative electrode comprises Al (100), Al (111), Al crystal faces such as (110); Au (100), Au crystal faces such as (111); Pt (100), Pt (110), Pt crystal faces such as (111); Cu (100), Cu (110), Cu crystal faces such as (111); Ni (100), Ni (110), Ni crystal faces such as (111); W (100), W crystal faces such as (110); Comprise metal single crystal face electrodes such as Mg, Ti in addition.
Above-mentioned a kind ofly prepare in the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, inert anode comprises Graphite Electrodes, metal composite electrode, hanging mercury electrode, inert metal electrode (Au, Pt etc.) etc.
Above-mentioned a kind ofly prepare in the method for aluminium ingot, with AlCl by metal single crystal face electrode low-temperature electrolytic
3The type ionic liquid is during as electrolytic solution, AlCl
3Anhydrous AlCl in the type ionic liquid
3Shared molar ratio is 1: 1～3: 1, preferred 1.2: 1～2.0: 1; Temperature of reaction can be carried out in 20～110 ℃ of scopes, preferred 25～80 ℃; Current density is 0.5～50mA/cm
2, preferred 1～20mA/cm
2Electrolysis time is 0.2～24h, preferred 2～12h; Stirring velocity is 10～2000r/min, preferred 40～1000r/min, and cathode efficiency is more than 95%.Reaction can be carried out in vacuum glove box or other can be realized the electrolyzer of anhydrous and oxygen-free.
Above-mentioned a kind ofly prepare in the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, low temperature inorganic fused salt system mainly is NaCl-AlCl
3And NaCl-KCl-AlCl
3Deng.
Above-mentioned a kind ofly prepare in the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic is at binary system NaCl-AlCl
3Middle AlCl
3Massfraction is 40%～80%, at ternary system NaCl-KCl-AlCl
3Middle AlCl
3Massfraction is 40%～90%.
Above-mentioned a kind ofly prepare in the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, during as electrolytic solution, temperature of reaction can be carried out in 90～300 ℃ of scopes, preferred 100～250 ℃ with the low temperature inorganic fused salt; Current density is 0.015～40mA/cm
2, preferred 0.15～30mA/cm
2Electrolysis time is 0.1～12h, preferred 1～6h; Cathode efficiency is more than 80%.
Proposed by the invention a kind ofly prepare the method for aluminium ingot, have following advantage by metal single crystal face electrode low-temperature electrolytic:
1) realized that electrolysis generates aluminium ingot under the cold condition, and ionic liquid can reuse environmentally safe etc.
2) overcome other electrode surface settled layers and approached, formed the shortcoming of dendrite easily.
Embodiment:
Embodiment 1
At [Bmim] Cl-AlCl
3In the electrolytic solution, dc electrolysis is an anode with the crude aluminum electrode, and Al (110) electrode is a negative electrode, and filamentary silver is a reference electrode, and electrolysis temperature maintains about 60 ℃, pole span 1cm, and current density is 1mA/cm
2, electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains fine and close thicker al deposition layer.
Embodiment 2
At [Emim] Cl-AlCl
3In the electrolytic solution, dc electrolysis is an anode with the crude aluminum electrode, and Al (110) electrode is a negative electrode, and filamentary silver is a reference electrode, and electrolysis temperature maintains about 60 ℃, pole span 1cm, and current density is 1mA/cm
2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains fine and close thicker al deposition layer.
Embodiment 3
At [Py (1,4)] Tf
2N-AlCl
3In the electrolytic solution, dc electrolysis is an anode with the crude aluminum electrode, and Al (110) electrode is a negative electrode, and filamentary silver is a reference electrode, and electrolysis temperature maintains about 60 ℃, pole span 1cm, and current density is 1mA/cm
2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains fine and close thicker al deposition layer.
Embodiment 4
At [Bmim] Cl-AlCl
3In the electrolytic solution, dc electrolysis is an anode with graphite, and Al (110) electrode is a negative electrode, and filamentary silver is a reference electrode, and electrolysis temperature maintains about 60 ℃, pole span 1cm, and current density is 1mA/cm
2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains fine and close thicker al deposition layer.
Embodiment 5
At [Emim] Cl-AlCl
3In the electrolytic solution, dc electrolysis is an anode with graphite, and Al (110) electrode is a negative electrode, and filamentary silver is a reference electrode, and electrolysis temperature maintains about 60 ℃, pole span 1cm, and current density is 1mA/cm
2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains fine and close thicker al deposition layer.
Embodiment 6
At [Py (1,4)] Tf
2N-AlCl
3In the electrolytic solution, dc electrolysis is an anode with graphite, and Al (110) electrode is a negative electrode, and filamentary silver is a reference electrode, and electrolysis temperature maintains about 60 ℃, pole span 1cm, and current density is 1mA/cm
2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains fine and close thicker al deposition layer.
Be noted that at last, more than given embodiment only be used for illustrating technical scheme of the present invention but not concrete restriction, technical solution of the present invention is made amendment or be equal to replacement with reference to embodiments of the invention, and do not depart from the scope of the present invention, it all should be encompassed in the claim scope of the present invention.
Claims (8)
1. one kind prepares the method for aluminium ingot by metal single crystal face electrode low-temperature electrolytic, it is characterized by
1) water-content is less than 5ppm, and oxygen level is less than under the 5ppm condition, AlCl
3The type ionic liquid is as electrolytic solution, and noble electrode obtains aluminium ingot as anode on metal single crystal face negative electrode;
Or 2) water-content is less than 5ppm, and oxygen level is less than under the 5ppm condition, AlCl
3The type ionic liquid is as electrolytic solution, and the crude aluminum electrode obtains aluminium ingot as anode on metal single crystal face negative electrode;
Or 3) in atmosphere of inert gases, the low temperature inorganic fused salt is as electrolytic solution, and the crude aluminum electrode obtains aluminium ingot as anode on metal single crystal face negative electrode
Or 4) in atmosphere of inert gases, the low temperature inorganic fused salt is as electrolytic solution, and noble electrode obtains aluminium ingot as anode on metal single crystal face negative electrode.
2. method according to claim 1, metal single crystal face negative electrode comprises Al (100), Al (111), Al (110), Au (100), Au (111), Pt (100), Pt (110), Pt (111), Cu (100), Cu (110), Cu (111), Ni (100), Ni (110), Ni (111), W (100), W (110) and Mg, metal single crystal face electrodes such as Ti.
3. method according to claim 1, AlCl
3The type ionic liquid mainly comprises following several:
[Bmim] Cl-AlCl
3(1-butyl-3-Methylimidazole chloro-aluminate), [Emim] Cl-AlCl
3(1-ethyl-3-Methylimidazole chloro-aluminate), [Bdmim] Cl-AlCl
3(1-butyl-2,3-methylimidazole chloro-aluminate), TMBAC-AlCl
3(benzyltrimethylammon.um chloro-aluminate), TEBAC-AlCl
3(benzyltrimethylammon.um chloro-aluminate), BPC-AlCl
3(butylpyridinium chloroaluminate), [Py (1,4)] Tf
2N-AlCl
3(1, the two fluoroform sulfimide chloro-aluminates of 4-pyridine), [Emim] Tf
2N-AlCl
3(the two fluoroform sulfimide chloro-aluminates of 1-ethyl-3-Methylimidazole), [Bmim] Br-AlCl
3(bromination 1-butyl-3-Methylimidazole chloro-aluminate), [Bmim] BF
4-AlCl
3(1-butyl-3-Methylimidazole Tetrafluoroboric acid chloro-aluminate).
4. according to claim 1 or the described method of claim 3, AlCl
3Anhydrous AlCl in the type ionic liquid
3Shared molar ratio is 1.0～3.0.
5. according in the claim 1 1), or 2) described method, it is characterized in that adopting the mode of dc electrolysis, AlCl
3Anhydrous AlCl in the type ionic liquid
3Shared molar ratio is 1: 1～3: 1; Temperature of reaction is carried out in 20～110 ℃ of scopes; Current density is 0.5～50mA/cm
2Electrolysis time is 0.2～24h; Stirring velocity is 10～2000r/min; Cathode efficiency is more than 95%.
6. method according to claim 1, the low temperature inorganic fused salt is NaCl-AlCl
3Or NaCl-KCl-AlCl
3System is at binary system NaCl-AlCl
3Middle AlCl
3Massfraction is 40%～80%, at ternary system NaCl-KCl-AlCl
3Middle AlCl
3Massfraction is 40%～90%.
7. according in the claim 1 3) or 4) described method, it is characterized in that the mode of the dc electrolysis that adopts, temperature of reaction is carried out in 90～300 ℃ of scopes; Current density is 0.015～40mA/cm
2Electrolysis time is 0.1～12h; Cathode efficiency is more than 80%.
8. method according to claim 1, inert anode comprises Graphite Electrodes, metal composite electrode, hanging mercury electrode, inert metal electrode etc.
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Cited By (7)
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| CN103556197A (en) * | 2013-10-31 | 2014-02-05 | 陕西师范大学 | Method for preparing monoatomic-layer-thick metal film on flexible curled conducting substrate |
| CN108456897A (en) * | 2017-02-17 | 2018-08-28 | 中国科学院过程工程研究所 | For the silicon source of electrolytic preparation aluminium-containing alloy, preparation method and the method for preparing aluminium-containing alloy using it |
| CN108493502A (en) * | 2018-04-13 | 2018-09-04 | 深圳市得朗高科技有限公司 | A kind of double charcoals and the double poles MXene ion heavy-duty batteries |
| CN108796601A (en) * | 2017-05-02 | 2018-11-13 | 上海奇谋能源技术开发有限公司 | A method of producing single-crystal metal |
| CN108796615A (en) * | 2017-05-02 | 2018-11-13 | 上海奇谋能源技术开发有限公司 | A method of improving metal purity |
| CN110863217A (en) * | 2019-12-09 | 2020-03-06 | 安阳工学院 | Novel ionic liquid electrolyte and method for low-temperature electrolytic refining of raw aluminum by using same |
| CN111074300A (en) * | 2020-03-05 | 2020-04-28 | 吴君石 | Method for preparing aluminum by low-temperature constant-current multistage electrolysis of ionic liquid electrolyte system |
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| CN103556197B (en) * | 2013-10-31 | 2016-04-06 | 陕西师范大学 | The method of monoatomic layer thicknesses of metal film prepared by flexible curling conductive substrates |
| CN108456897A (en) * | 2017-02-17 | 2018-08-28 | 中国科学院过程工程研究所 | For the silicon source of electrolytic preparation aluminium-containing alloy, preparation method and the method for preparing aluminium-containing alloy using it |
| CN108796601A (en) * | 2017-05-02 | 2018-11-13 | 上海奇谋能源技术开发有限公司 | A method of producing single-crystal metal |
| CN108796615A (en) * | 2017-05-02 | 2018-11-13 | 上海奇谋能源技术开发有限公司 | A method of improving metal purity |
| CN108493502A (en) * | 2018-04-13 | 2018-09-04 | 深圳市得朗高科技有限公司 | A kind of double charcoals and the double poles MXene ion heavy-duty batteries |
| CN110863217A (en) * | 2019-12-09 | 2020-03-06 | 安阳工学院 | Novel ionic liquid electrolyte and method for low-temperature electrolytic refining of raw aluminum by using same |
| CN111074300A (en) * | 2020-03-05 | 2020-04-28 | 吴君石 | Method for preparing aluminum by low-temperature constant-current multistage electrolysis of ionic liquid electrolyte system |
| CN111074300B (en) * | 2020-03-05 | 2021-09-24 | 广州市香港科大霍英东研究院 | Method for preparing aluminum by low-temperature constant-current multistage electrolysis of ionic liquid electrolyte system |
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Application publication date: 20110817 |