CN102634817A - Ionic liquid low-temperature aluminum electrolysis method with glassy carbon as inert anode - Google Patents
Ionic liquid low-temperature aluminum electrolysis method with glassy carbon as inert anode Download PDFInfo
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Abstract
The invention relates to an ionic liquid low-temperature aluminum electrolysis method with glassy carbon as an inert anode. In the method, glassy carbon is used as a new inert anode, a conventional material such as graphite is used as a cathode, and an ionic liquid-AlCl3 system is electrolyzed at 25-200 DEG C to obtain solid-state aluminum. The method has the advantages of improving current efficiency of ionic liquid low-temperature aluminum electrolysis and the quality of the aluminum products significantly, reducing reaction energy consumption effectively, and realizing cyclic utilization of ionic liquid and anode fully. The method overcomes the shortcoming that the traditional anode materials are poor in stability and low in reaction efficiency, and is beneficial for the industrialized promotion of ionic liquid low-temperature aluminum electrolysis technology, therefore, the method has the important research and application value.
Description
Technical field
The invention belongs to the Metal smelting field, being specifically related to a kind of is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon.
Background technology
As a kind of common metallic substance; Aluminium is being played the part of more and more important effect in promoting world economy and social development; This not only depends on aluminium element at the extensive distribution of occurring in nature and high content, also because metallic aluminium has physicochemical property such as good electrical conductivity, ductility, thermal conductivity and erosion resistance.
At present, aluminium industry is one of maximum in the world electrochemical industry.In metal, the YO of aluminium is only second to steel, is higher than other common non-ferrous metal.Generally adopt Hall-Heroult process (Hall-H é roult) to carry out the suitability for industrialized production of aluminium now both at home and abroad.This method be under the temperature about 950 ℃ with alumina dissolution in the fused sodium aluminum fluoride, and carry out electrolysis with direct current.After the electrolysis, the product of electric tank cathode is an aluminium liquid, and anodic product then is CO
2, material such as CO and HF.Can obtain commercial aluminium product behind the extraction of aluminium liquid process vacuum, the purifying.Through 100 years of development, Hall-Heroult process has developed comparatively ripely, has advantages such as reduced investment, technical equipment is simple, the construction period is short, and temperature is high, the high (13～15kWhKg of energy consumption but also exist simultaneously
-1), pollute heavy and quality product low (＜99.5%) waits deficiency.Therefore, in the today of advocating scientific development and energy-saving and emission-reduction, press for the electrolytic aluminum industry is carried out technical renovation, reduces production energy consumption and reduced the discharging of pollutent.
Can the key that address the above problem be realize the electrolysis of aluminum under the lesser temps that therefore ionic liquid arises.Ionic liquid is a kind of watery fusion salt, generally is made up of organic cation and inorganic/organic anion, because this particular structural, ionic liquid has lower fusing point, usually near in addition be lower than room temperature.Therefore very in addition, ionic liquid also has higher specific conductivity, the electrochemical window and the extremely low advantages such as vp of stability, broad preferably, is suitable as the ionogen of low-temperature electrolytic aluminium.As far back as 1948, Hurley etc. were when seeking the electrolyte of electrolysis of aluminum oxide, with N-ethylpyridine muriate and AlCl
3Obtained a kind of colourless liquid after the mixing, this liquid is chlorine aluminic acid type ionic liquid, also is called as first-generation ionic liquid.Up to 1992, reported first such as Carling at dialkylimidazolium villaumite-AlCl
3The method of electrolytic aluminum in the ion liquid system.After this, the electrolysis of aluminum in the ionic liquid is launched extensive studies both at home and abroad, obtained interim progress.Wherein the most representative system mainly contains [Emim] Cl (1-ethyl-3-Methylimidazole villaumite)-AlCl
3, [Bmim] Cl (1-butyl-3-Methylimidazole villaumite)-AlCl
3[TMPA] Cl (trimethylammonium puratized agricultural spray villaumite)-AlCl
3Deng.These systems all can be implemented in the electrolytic aluminum process under the low temperature (25～150 ℃), and wherein negative electrode, anode are separated out solid aluminum and chlorine respectively.The bath voltage of this method is generally 2～6V, and energy consumption is merely 6～9kWhKg
-1, the aluminium product purity can reach 99%, and this has not only significantly reduced the energy consumption of reaction of electrolytic aluminum, when obtaining the high-quality Al product, can also obtain the chlorine of high added value, has reduced CO simultaneously
2The isothermal chamber gas purging.We can say that ionic liquid low-temperature electrolytic aluminum technology is expected to replace traditional Hall-Heroult process, become the leading working method of following aluminum electrolysis industry.
Though ionic liquid has huge advantage and potentiality on low-temperature electrolytic aluminium; But also come with some shortcomings; Wherein the most outstanding is not find the inert anode material that is applicable to ion liquid system as yet, has usually caused anode electrolysis efficient situation of decomposing with ion liquid section on the low side.Even the widely used chlorine inert anode of analysing in traditional electrolytic industry also can't be competent at like graphite and ruthenium titanium anode.For example, at 100 ℃ and 3mA/cm
2Current density under, obvious corrosion has just taken place in work after less than 2h in ruthenium titanium anode, ruthenium oxide coatings is destroyed; And traditional graphite anode is swollen in that identical condition is next gradually, comes off even ruptures, be difficult to keep the electrolytic aluminum reaction and carry out smoothly for a long time, and anodic current efficiency less than 20%, side reaction is serious.So the development of new inert anode material is to solve this skilled industry key in application.
In view of above present Research, it is inert anode material that the present invention adopts glass carbon (glass carbon element) first, uses it for ionic liquid low-temperature electrolytic reactive aluminum.Experimental result shows; Glass carbon has very high stability; After through electrolytic aluminum reaction in 1000 hours, glass carbon still keeps good physics and chemical property, and anode efficiency has obtained significant raising; The side reaction of electrolysis simultaneously obviously reduces, and glass carbon and ionic liquid can be realized recycling after treatment.So glass carbon has not only overcome all deficiencies of conventional anode material as a kind of novel inert anode material, and help the industrialization promotion of ionic liquid low-temperature electrolytic aluminum technology, therefore have important research and using value.
Summary of the invention
The invention provides a kind of is the ionic liquid low-temperature electrolytic aluminium novel method of inert anode with glass carbon.The characteristics of present method are to be novel inert anode with glass carbon, and comparatively stable conventional materials such as graphite, aluminium, copper and iron are negative electrode, ionic liquid+AlCl
3System is an ionogen, can realize the electrolytic aluminum reaction at low temperatures smoothly.Not only can significantly improve the current efficiency of ionic liquid low-temperature electrolytic aluminium and the quality of aluminium product through present method, can also effectively lower energy consumption of reaction, fully realize the recycle of ionic liquid and glass carbon anode.
In the present invention, glass carbon is meant through the special glassy armorphous carbon of being processed into, also often is called vitreous carbon or glass carbon element.Its main character is following: 1) apparent density is about 1.51g/cm
32) resistivity is about 42 μ Ω m; 3) anti-ly tear intensity open greater than 100MPa; 4) SH is about 120; 5) thermal conductivity is about 5.8W/mK.Related ionic liquid can be divided into imidazole type, pyridine type, quaternary ammonium type 、 quaternary phosphine type, pyrroles's type, piperidines type, morpholine type and sulfonium salt type from cationic structural, and valence state is+and 1, shown in the following structural formula of its structure, R
1, R
2, R
3, R
4, R
5, R
6, R
7The expression alkyl, alkoxyl group, fluorine or hydrogen; Negatively charged ion is F
-, Cl
-, Br
-, I
-, SCN
-, CN
-, [N (CF
3SO
2)
2]
-[N (CN)
2]
-Deng can with AlCl
3Form the anionic ion of solvay-type.
Imidazole type positively charged ion pyridine type cationic quaternary ammonium type Yang ion quaternary phosphine type positively charged ion
Pyrroles's type positively charged ion piperidines type positively charged ion morpholine type positively charged ion sulfonium salt type positively charged ion
Electrolyzer used in the present invention is made up of anolyte compartment and cathode compartment, separates through G1 type glass sand plate between two electrode vessels, isolates anode chlorine of separating out and the purpose that improves current efficiency to reach.Ionic liquid low-temperature electrolytic reactive aluminum can be accomplished by constant voltage or two kinds of electrolysis modes of continuous current, and temperature of reaction is 25～200 ℃, and bath voltage is 2～6V, and vacuum tightness is about-0.1MPa AlCl in the groove
3Concentration in ionic liquid is generally greater than 1mol/L.Under above-mentioned system and experiment condition, anode, cathode efficiency can reach respectively more than 90% and 98%, and the solid aluminum that obtains, the purity of chlorine can reach respectively more than 99.5% and 98%.
In the present invention, the current efficiency of anode, negative electrode is got with the ratio of theoretical yield by the actual output of chlorine, aluminium respectively, and its value equates with separately actual recovery.The actual output of aluminium is obtained by difference assay; When calculating the actual output of chlorine, at first pass through NaOH-Na
2S
2O
3Mixing solutions absorbs the chlorine of separating out and also all is converted into Cl
-, utilize chromatography of ions to obtain Cl then
-Content and the final conversion output that obtains chlorine.The electric weight that the theoretical yield of chlorine, aluminium then passes through according to Faraday's law and electrode calculates.
Embodiment
The present invention explains through following examples, but the present invention also not only is confined to following examples, and the implementing method of said aim was all in technical scope of the present invention before and after all met.
Embodiment 1
With [Bmim] Cl-2AlCl
3(1-butyl-3-Methylimidazole chloro-aluminate) is ionogen, and glass carbon, copper sheet be respectively as anode and negative electrode, at 50 ℃, and the voltage of 3～5V, 10mA/cm
2The vacuum of current density and-0.1MPa under electrolysis 2h, through assay determination, the current efficiency of anode and negative electrode can reach 93.3% and 99.2% respectively, the purity of aluminium and chlorine is respectively 99.8% and 99.0%.
Embodiment 2
With [Bdmim] Cl-2AlCl
3(1-butyl-2,3-methylimidazole chloro-aluminate) is ionogen, and glass carbon, graphite is respectively as anode and negative electrode, at 100 ℃, and the voltage of 2～4V, 20mA/cm
2The vacuum of current density and-0.1MPa under electrolysis 2h, through assay determination, the current efficiency of anode and negative electrode can reach 92.1% and 98.7% respectively, the purity of aluminium and chlorine is respectively 99.6% and 98.4%.
Embodiment 3
With [H1mim] Cl-2AlCl
3(1-hydrogen-3-Methylimidazole chloro-aluminate) is ionogen, and glass carbon, aluminium flake be respectively as anode and negative electrode, at 60 ℃, and the voltage of 3～5V, 15mA/cm
2The vacuum of current density and-0.1MPa under electrolysis 2h, through assay determination, the current efficiency of anode and negative electrode can reach 92.5% and 98.6% respectively, the purity of aluminium and chlorine is respectively 99.7% and 98.5%.
Embodiment 4
With [TMPA] Cl-2AlCl
3(trimethylammonium puratized agricultural spray chloro-aluminate) is ionogen, and glass carbon, graphite is respectively as anode and negative electrode, at 120 ℃, and the voltage of 2～4V, 30mA/cm
2The vacuum of current density and-0.1MPa under electrolysis 2h, through assay determination, the current efficiency of anode and negative electrode can reach 91.4% and 98.3% respectively, the purity of aluminium and chlorine is respectively 99.6% and 98.3%.
Embodiment 5
With [TBP] Cl-2AlCl
3(4-butyl-phosphonium chloro-aluminate) is ionogen, and glass carbon, graphite is respectively as anode and negative electrode, at 150 ℃, and the voltage of 2～4V, 70mA/cm
2The vacuum of current density and-0.1MPa under electrolysis 2h, through assay determination, the current efficiency of anode and negative electrode can reach 90.9% and 98.1% respectively, the purity of aluminium and chlorine is respectively 99.6% and 98.2%.
Embodiment 6
With [EPy] Cl-2AlCl
3(N-ethylpyridine chloro-aluminate) is ionogen; Glass carbon, copper sheet are respectively as anode and negative electrode; At 80 ℃, electrolysis 2h under the vacuum of the voltage of 4V and-0.1MPa is through assay determination; The current efficiency of anode and negative electrode can reach 92.2% and 98.9% respectively, and the purity of aluminium and chlorine is respectively 99.7% and 98.6%.
Embodiment 7
With [Et
3NH] Cl-2AlCl
3(triethyl ammonium chloro-aluminate) is ionogen; Glass carbon, aluminium flake are respectively as anode and negative electrode; At 60 ℃, electrolysis 2h under the vacuum of the voltage of 3V and-0.1MPa is through assay determination; The current efficiency of anode and negative electrode can reach 91.5% and 98.7% respectively, and the purity of aluminium and chlorine is respectively 99.8% and 98.5%.
Claims (6)
1. one kind is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon, it is characterized in that with glass carbon be novel inert anode, ionic liquid+AlCl
3Be ionogen, can obtain solid aluminum and chlorine at negative electrode, anode through low-temperature electrolytic, electrode current efficient is significantly improved simultaneously, and the glass carbon anode still keeps good physicochemical property in work after thousands of hours.
2. according to claim 1 is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon; Said glass carbon; Also often being called vitreous carbon or glass carbon element, is that its main character is following: 1) apparent density is about 1.51g/cm through the special glassy armorphous carbon of being processed into
32) resistivity is about 42 μ Ω m; 3) anti-ly tear intensity open greater than 100MPa; 4) SH is about 120; 5) thermal conductivity is about 5.8W/mK.
3. according to claim 1 is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon, and described negative electrode is a cathode material common in the electrolytic industry, for example comparatively stable conventional materials such as graphite, aluminium, copper and iron.
4. according to claim 1 is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon; Said ionic liquid positively charged ion is imidazole type, pyridine type, quaternary ammonium type 、 quaternary phosphine type, pyrroles's type, piperidines type, morpholine type and sulfonium salt type; Valence state is+and 1, its structure is shown in the following figure, R
1, R
2, R
3, R
4, R
5, R
6, R
7The expression alkyl, alkoxyl group, fluorine or hydrogen; Negatively charged ion is F
-, Cl
-, Br
-, I
-, SCN
-, CN
-, [N (CF
3SO
2)
2]
-[N (CN)
2]
-Deng can with AlCl
3Form the anionic ion of solvay-type.
Imidazole type positively charged ion pyridine type cationic quaternary ammonium type Yang ion quaternary phosphine type positively charged ion
Pyrroles's type positively charged ion piperidines type positively charged ion morpholine type positively charged ion sulfonium salt type positively charged ion
5. according to claim 1 is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon; Wherein electrolysis can be accomplished by constant voltage or two kinds of electrolysis modes of continuous current; Temperature of reaction is 25～200 ℃, and bath voltage is 2～6V, and electrode current density is 1～100mA/cm
2, vacuum tightness is about-0.1MPa AlCl in the groove
3Concentration in ionic liquid is generally greater than 1mol/L.
6. according to claim 1 is the ionic liquid low-temperature electrolytic aluminium method of inert anode with glass carbon; Anode in this method, cathode efficiency can reach respectively more than 90% and 98%, and the solid aluminum that obtains, the purity of chlorine can reach respectively more than 99.5% and 98%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104141150A (en) * | 2014-07-25 | 2014-11-12 | 东北大学 | Method for making aluminum through low temperature electrolysis with ionic liquid and aluminum chloride as electrolytes |
| CN105063660A (en) * | 2015-08-03 | 2015-11-18 | 中南大学 | Method for directly preparing nanometer silicon powder in electrolytic refining process |
| CN105671598A (en) * | 2016-04-08 | 2016-06-15 | 中国科学院过程工程研究所 | Method for directly preparing aluminum foil through low temperature electrolysis |
| 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 |
| CN110129823A (en) * | 2019-04-19 | 2019-08-16 | 安阳工学院 | A kind of novel ion liquid complex media and the preparation method and application thereof and application method |
| 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 |
| CN111041193A (en) * | 2020-03-05 | 2020-04-21 | 吴君石 | Method for preparing aluminum from fly ash by using ionic liquid |
| CN111321427A (en) * | 2020-03-05 | 2020-06-23 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
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Cited By (10)
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| CN104141150A (en) * | 2014-07-25 | 2014-11-12 | 东北大学 | Method for making aluminum through low temperature electrolysis with ionic liquid and aluminum chloride as electrolytes |
| CN105063660A (en) * | 2015-08-03 | 2015-11-18 | 中南大学 | Method for directly preparing nanometer silicon powder in electrolytic refining process |
| CN105671598A (en) * | 2016-04-08 | 2016-06-15 | 中国科学院过程工程研究所 | Method for directly preparing aluminum foil through low temperature electrolysis |
| 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 |
| CN107417588B (en) * | 2017-06-16 | 2019-05-10 | 安阳工学院 | A kind of novel ion liquid and the method using its electrolytic preparation nano aluminum |
| CN110129823A (en) * | 2019-04-19 | 2019-08-16 | 安阳工学院 | A kind of novel ion liquid complex media and the preparation method and application thereof and application method |
| 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 |
| CN111041193A (en) * | 2020-03-05 | 2020-04-21 | 吴君石 | Method for preparing aluminum from fly ash by using ionic liquid |
| CN111321427A (en) * | 2020-03-05 | 2020-06-23 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
| CN111321427B (en) * | 2020-03-05 | 2021-05-28 | 惠州大亚湾艾利荣化工科技有限公司 | Method for low-temperature and low-pressure electrolysis of aluminum by using ionic liquid electrolyte |
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Application publication date: 20120815 |