CN103160853A - Method for electrolyzing aluminum by using amino-functionalized ionic liquid electrolyte - Google Patents

Method for electrolyzing aluminum by using amino-functionalized ionic liquid electrolyte Download PDF

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CN103160853A
CN103160853A CN2011104106124A CN201110410612A CN103160853A CN 103160853 A CN103160853 A CN 103160853A CN 2011104106124 A CN2011104106124 A CN 2011104106124A CN 201110410612 A CN201110410612 A CN 201110410612A CN 103160853 A CN103160853 A CN 103160853A
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aniline
ionic liquid
amine
aluminium
electrolysis
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张建敏
张锁江
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Institute of Process Engineering of CAS
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Institute of Process Engineering of CAS
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention relates to a method for preparing aluminum through low-temperature electrolysis by using an ionic liquid as an electrolyte. The ionic liquid is composed of an amino compound and anhydrous aluminum chloride. The ratio of amino group in the amino compound to the anhydrous aluminum chloride can be regulated under a condition that a product is in a liquid state during electrolysis. Therefore, aluminum large-scale electrochemical preparation under room temperature can be realized.

Description

A kind of method with amino functional il electrolyte electrolytic aluminum
Technical field
The present invention relates to a kind of amino functional ionic liquid as the method for used for electrolyte in electrolytic aluminum, belong to the Metal smelting field.
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 the aspects such as machinofacture, Transport Machinery, power machine, aircraft industry, material of construction, wrapping material, finishing material.
The method of industrial production aluminium is mainly Hall-H é roult method, i.e. sodium aluminum fluoride-alumina eltrolysis method now.This method need to be kept suitable electrolyzer temperature by the theoretical electric energy that consumes more than a times in order to keep the 900-1000 celsius temperature of reaction, causes 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 is conducive to energy-saving and emission-reduction, and can promote the application of novel material and the exploitation of novel process.Can select novel inert anode material under cold condition, consume thereby break away from the discharging that carbon anode material reduces carbonic acid gas, this makes the low-temperature molten salt system more and more receive people's concern, and wherein topmost is exactly inorganic molten salt and organic melting salt.The common system of inorganic molten salt has NaCl-AlCl 3And NaCl-KCl-AlCl 3Deng, organic melting salt generally is comprised of metal halide and organic salt also referred to as ionic liquid at room temperature.The room temperature melting salt new medium that wherein chlorine aluminic acid ionic liquid is a fluid-like state wide ranges, specific conductivity is high, electrochemical window is wide, vapour pressure is extremely low has broad prospects in electrolytic aluminum research and application facet.
Chinese patent CN1664170A discloses a kind of method of producing aluminium under low-temperature and aluminium alloy, is exactly with AlCl 3The type ionic liquid is as low-temperature electrolyte.But they obtain Aluminum chloride anhydrous further to process and obtain AlCl take aluminum oxide or the mineral that contain aluminosilicate as the raw material chlorination 3The type ionic liquid.Chinese patent CN101265588A also discloses a kind of method that low-temperature electrolytic generates aluminium, and they adopt bisulfate ion (HSO 4 -) type anion ion liquid dissolved oxygen aluminium, as low-temperature electrolytes, take aluminum oxide as the raw material Direct Electrolysis.Li Qingfeng etc. are at low temperature NaCl-AlCl 3Obtain dendroid or how empty shape aluminium lamination in system.Wang Jihui etc. are at low temperature NaCl-KCl-AlCl 3In obtain needle-like coating.But they have just obtained thinner al deposition layer or dendritic aluminium dendrite on electrode.
This laboratory replaces the application of cryolite fused salt in the electrolytic aluminum system to carry out desk study (Zhang Suojiang, Xu Hui, Zhang Jianmin, Zheng Yong, Liu's love, a relative, Lv Xingmei to ionic liquid as ionogen early stage.The method of the micro-nano aluminium powder of a kind of ionic liquid electrolytic preparation.Application number 201110092066.4; Zhang Suojiang, Xu Hui, Zhang Jianmin, Zheng Yong, Zhang Li, business's jade-like stone, Wang Zanxia, Lv Xingmei, Zhang Xiangping.A kind of method for preparing aluminium ingot by low-temperature electrolysis of metal monocrystal surface electrodes.Application number: 201110069197.0; Zhang Suojiang, Zheng Yong, Lv Xingmei, left brave, Cai Yingjun, Zhang Xiangping, Zhang Jianmin. a kind of ionic liquid low-temperature electrolytic aluminium method application number take glass carbon as inert anode: 201110038552.8), find to adopt electrolyzing aluminum from ionic liquid electrolysis temperature can be down to below 150 degrees centigrade.Compare with traditional sodium aluminum fluoride technique, this has reduced electrolysis temperature undoubtedly, has greatly reduced energy consumption.But glyoxaline ion liquid commonly used is owing to containing unsaturated link(age) at present; thereby may react with the chlorine that produces in the process of electrolysis and cause the ionic liquid structural damage; the preparation cost of this kind ionic liquid is higher simultaneously, is unfavorable for the large-scale production of ionic liquid low-temperature electrolytic aluminium.
Summary of the invention
The invention provides a kind of method of aluminium for preparing as the electrolytic solution low-temperature electrolytic with the amino functional ionic liquid, directly adopt aminocompound and aluminum chloride to form ionic liquid, stable chemical nature, cheap, have good prospects for commercial application.
Amino functional ionic liquid of the present invention is used for the method for room temperature electrolytic aluminum, and the ionic liquid that forms take aminocompound and Aluminum chloride anhydrous prepares 100 degrees centigrade of extensive electrochemistry that can realize aluminium as electrolytic solution.Amino in aminocompound and the ratio of Aluminum chloride anhydrous can present liquid the adjusting in the situation that keep product under the electrolysis state.For example urea (urea) can and Aluminum chloride anhydrous regulate between the mol ratio of 1: 1 and 1: 2.Aminocompound comprises: the structures such as imines that urea (urea), guanidine derivatives (as tetramethyl guanidine), acid amides (as ethanamide), aliphatic amide (propylamine, butylamine, amylamine, hexylamine, heptyl amice, octylame etc.), aromatic amine (as aniline, pentanoic, triphenylamine, perchloro-aniline etc.), imidazoles, piperidines, pyridine, pyrimidine, hydrazine and above-mentioned substance form.
This electrolytic process can produce chlorine, can adopt ionic membrane with isolation aluminium product and chlorine, or take away chlorine in the mode that rare gas element carries.Amino functional ionic liquid proposed by the invention is used for the method for low-temperature electrolytic aluminium, has advantages of following:
1) realized that under cold condition, electrolysis generates aluminium, ionic liquid can reuse, environmentally safe etc.
2) make the cost of ionic liquid be able to decrease, as the ionic liquid of urea (urea) with the Aluminum chloride anhydrous configuration, its cost makes the technique of ionic liquid low-temperature electrolytic aluminium possess great advantage at cost lower than 6000 yuan/tons.
Embodiment:
Embodiment 1
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 2
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 1.5) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 3
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 2) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 4
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adopts anion-selective membrane as barrier film, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 5
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 1.5) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adopts anion-selective membrane as barrier film, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 6
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 2) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adopts anion-selective membrane as barrier film, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 7
At CH 3CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 8
At C 6H 5NH 2-AlCl 3In (two kinds of material mol ratios are 1: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 9
At CH 3CH 2CH 2CH 2NH 2-AlCl 3In (two kinds of material mol ratios are 1: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 10
At NH 2CH 2CH 2CH 2CH 2NH 2-AlCl 3In (two kinds of material mol ratios are 1: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adopts anion-selective membrane as barrier film, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 11
At NH 2CH 2CH 2CH 2CH 2NH 2-AlCl 3In (two kinds of material mol ratios are 1: 1.5) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adopts anion-selective membrane as barrier film, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 12
At NH 2CH 2CH 2CH 2CH 2NH 2-AlCl 3In (two kinds of material mol ratios are 1: 2) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adopts anion-selective membrane as barrier film, electrolysis temperature maintains 80 ℃ of left and right, pole span 1cm, current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains loose bright aluminium powder.
Embodiment 13
At imidazoles-AlCl 3In (two kinds of material mol ratios are 0.5: 1) electrolytic solution, the direct current constant-current electrolysis, take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, and logical argon gas carries chlorine, and electrolysis temperature maintains 120 ℃ of left and right, pole span 1cm, current density is 180mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 90%, and negative electrode obtains loose bright aluminium powder.
Embodiment 14
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 1.5) electrolytic solution, the direct current constant-current electrolysis is take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adds brightener such as toluene etc., and logical argon gas carries chlorine, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, and current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains bright fine and close aluminium.
Embodiment 15
At NH 2CONH 2-AlCl 3In (two kinds of material mol ratios are 1: 2) electrolytic solution, the direct current constant-current electrolysis is take Graphite Electrodes as anode, the aluminium flake electrode is negative electrode, adds brightener such as toluene etc., and logical argon gas carries chlorine, electrolysis temperature maintains 100 ℃ of left and right, pole span 1cm, and current density is 200mA/cm 2Electrolysis time is 12h, and cathode efficiency is more than 95%, and negative electrode obtains bright fine and close aluminium.
Be noted that at last, above given embodiment only is used for illustrating technical scheme of the present invention but not concrete restriction, technical solution of the present invention is modified 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 claim scope of the present invention.

Claims (9)

1. one kind is carried out with the amino functional ionic liquid method that low-temperature electrolytic prepares aluminium, it is characterized in that, the ionic liquid that forms take aminocompound and Aluminum chloride anhydrous is realized the extensive electrochemistry preparation of aluminium as electrolytic solution at normal temperature.
2. method according to claim 1, described aminocompound comprise the structures such as molecule with amino group, ion, polymer.
3. method according to claim 2 comprises with the molecule of amino group: the structures such as imines that urea, guanidine derivatives, acid amides, aliphatic amide, alicyclic ring amine, aromatic amine, imidazoles, piperidines, pyridine, pyrimidine, hydrazine and above-mentioned substance form.
4. method according to claim 2 comprises with the ion of amino group: the structures such as alkyl imidazolium cation, ammonium cationoid, phosphine cationoid, miazines positively charged ion, pyridines positively charged ion, piperidines positively charged ion, amino acids negatively charged ion.
5. method according to claim 3, guanidine derivatives is tetramethyl guanidine, described acid amides is methane amide, ethanamide, propionic acid amide, butyramide, valeramide, hexanamide, heptamide, decoylamide, isobutyramide, acrylamide, polyacrylamide, hexanolactam, dimethyl formamide, N,N-DIMETHYLACETAMIDE, described aliphatic amide are propylamine, butylamine, amylamine, hexylamine, heptyl amice, octylame, decyl amine, amino dodecane, cetylamine, stearylamine, Diisopropylamine, dipropyl amine, cyclopropylamine, the 2-allylamine, diisobutylamine, isobutylamine, hexanediamine, 1,2-dimethyl propylamine, sec-butylamine, TERTIARY BUTYL AMINE, Putriscine, 1，10-diaminodecane, 1,5-dimethylhexylamine, described aliphatic cyclic amine comprises diethylenetriamine, vulkacit H, hexamethylene imine, the cyclic ethylene imines, triethylenediamine, piperazine, hexahydroaniline etc., described aromatic amine are aniline, pentanoic, triphenylamine, O-Phenylene Diamine, mphenylenediamine, Ursol D, o-toluidine, m-toluidine, to monomethylaniline, 23 dimethyl aniline, 2,4-xylidine, 2,5-xylidine, 2,6-xylidine, 3,4-xylidine, 3,5-xylidine, 2，4，6-trimethyl aniline, o ethyl aniline, the N-butylaniline, 2,6-Diethyl Aniline, formanilide, to butylaniline, monoacetylaniline, the 3-anisidine, Ortho-Chloro aniline, m-chloro aniline, p-Chlorobenzoic acid amide, O-ethoxyl amine, m-oxethyl aniline, p-ethoxyaniline, methylphenylamine, 2,3-dichlorphenamide bulk powder, 2,4 dichloro aniline, 2,6-DCA, 3,4-DCA, 3,5-dichlorphenamide bulk powder, 2,5-dichlorphenamide bulk powder, N-ethylaniline, o-bromoaniline, m-bromoaniline, para-bromoaniline, 245 trichloroaniline, 2,4,6-trichloroaniline, 2,4-dibromo aniline, 2,5-dibromo aniline, 2,6-dibromo aniline, m-bromoaniline, adjacent fluoroaniline, m-fluoroaniline, para-fluoroaniline, 2,4 difluorobenzene amine, 3,4-difluoroaniline, 2,3,4-trifluoromethyl aniline, o-Nitraniline, m-nitraniline, p-Nitroaniline, 2,4-dinitraniline, 3-chloro-4-fluoroaniline, Red G Salt or perchloro-, perfluor aniline etc.
6. method according to claim 2 comprises with the polymer of amino group: the structures such as polymine, PPI, polyaniline.
7. method according to claim 1, the amino in described aminocompound and the ratio of Aluminum chloride anhydrous can present liquid the adjusting in the situation that keep product under the electrolysis state.
8. method according to claim 1, this electrolytic process can produce chlorine, has adopted ionic membrane with isolation aluminium product and chlorine, or has taken away chlorine in the mode that vacuum or rare gas element carry.
9. method according to claim 1, the ionic liquid that aminocompound and Aluminum chloride anhydrous form can comprise one or more aminocompounds.
CN2011104106124A 2011-12-12 2011-12-12 Method for electrolyzing aluminum by using amino-functionalized ionic liquid electrolyte Pending CN103160853A (en)

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Cited By (4)

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CN106906494A (en) * 2017-04-06 2017-06-30 安阳工学院 A kind of new type low temperature fused electrolyte and the method using its preparation nano aluminum
CN107417588A (en) * 2017-06-16 2017-12-01 安阳工学院 A kind of novel ion liquid and the method using its electrolytic preparation nano aluminum
CN110683977A (en) * 2019-09-10 2020-01-14 山东大学 Aluminum ion battery electrolyte, preparation method and application
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

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CN102888630A (en) * 2011-07-20 2013-01-23 中国科学院过程工程研究所 Method for preparing nanometer aluminum or nanometer aluminum coating in low-temperature electro-deposition form by using ion liquid/additive system

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CN1687085A (en) * 2005-05-30 2005-10-26 中国科学院过程工程研究所 Ion liquid in phosphine group amino acid
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Publication number Priority date Publication date Assignee Title
CN106906494A (en) * 2017-04-06 2017-06-30 安阳工学院 A kind of new type low temperature fused electrolyte and the method using its preparation nano aluminum
CN107417588A (en) * 2017-06-16 2017-12-01 安阳工学院 A kind of novel ion liquid and the method using its electrolytic preparation nano aluminum
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CN110683977A (en) * 2019-09-10 2020-01-14 山东大学 Aluminum ion battery electrolyte, preparation method and application
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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

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Application publication date: 20130619