CN103066326A - Electrolyte for chargeable magnesium battery - Google Patents
Electrolyte for chargeable magnesium battery Download PDFInfo
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- CN103066326A CN103066326A CN2013100273061A CN201310027306A CN103066326A CN 103066326 A CN103066326 A CN 103066326A CN 2013100273061 A CN2013100273061 A CN 2013100273061A CN 201310027306 A CN201310027306 A CN 201310027306A CN 103066326 A CN103066326 A CN 103066326A
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- thiophenol
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- magnesium
- rechargeable
- cell
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses electrolyte for a chargeable magnesium battery. Solutes of the electrolyte contain thiophenol-alkyl magnesium halide and aluminum trichloride, or thiophenol-dialkyl magnesium and aluminum trichloride, and a solvent of the electrolyte is ether. When the electrolyte is applied to the chargeable magnesium battery, the positive electrode oxidation decomposition electric potential of the electrolyte can be close to 3.0V vs. Mg above, and the efficiency during a stable circulation process can be kept at 90% above. The electrolyte of the chargeable magnesium battery has the advantages of simple preparation, cheap raw material, high magnesium deposition-dissolution current, and high positive electrode oxidation decomposition electric potential.
Description
Technical field
The present invention relates to a kind of electrolyte for rechargeable magnesium cell, relate in particular to a kind of application process of electrolyte in rechargeable magnesium cell that contains thiophenol; Belong to the rechargeable magnesium cell field.
Background technology
Magnesium is one of the abundantest light metal element of reserves on the earth, and it has good machinery, physics and chemistry performance in addition, is widely used in multiple fields in today that the problems such as energy shortage, environmental pollution seriously restrict contemporary mankind's social development.Magnesium is in cornerwise position with lithium in the periodic table of elements, ionic radius is close, and chemical property is similar; And cheap, easy processing processing, fail safe are higher, therefore become a kind of study hotspot of novel battery system as the rechargeable magnesium cell of negative pole with magnesium.
The feasibility of rechargeable magnesium cell proposes (Gregory T D by people such as Gregory first in nineteen ninety, Hoffman R J, Winterton, Development of an ambient secondary magnesium battery, J.Electrochem.Soc., 137 (1990) 775-780).2000, the people's such as Aurbach research realized important breakthrough (Aurbach D, the Lu Z in rechargeable magnesium cell field, Schechter A, et al.Prototype systems for rechargeable magnesium batteries.Nature, 2000,407:724-727).To the research of rechargeable magnesium cell, mainly concentrate on nonaqueous electrolytic solution and the reversible embedding Mg that takes off of energy that can realize the reversible deposition of magnesium
2+Positive electrode.The most ripe electrolyte of rechargeable magnesium cell is the 0.25molL that Israel scientist Aurbach proposes at present
-1Mg (AlCl
2EtBu
2)/Tetrahydrofuran System (wherein Et is ethyl, and Bu is butyl) is main, and its anodic oxidation decomposition electric potential is 2.5V vs.Mg(Aurbach D, Lu Z, Schechter A, Gofer Y, Gizbar H, Turgemann R, Cohen Y, Moshkovich M, Levi E, Nature, 407 (2000) 724-727).In order to promote the development of low cost and high-performance rechargeable magnesium cell, seek the main direction that the anodic oxidation decomposition electric potential is high, conductivity is high, the reversible deposition of magnesium-dissolution efficiency is high, cycle performance is excellent and electrolyte system remains present rechargeable magnesium cell development cheaply.
Summary of the invention
Because the defects of prior art, technical problem to be solved by this invention provides a kind of low cost and high performance electrolyte and the application in rechargeable magnesium cell thereof.
For achieving the above object, on the one hand, the invention provides a kind of low cost and high performance rechargeable magnesium cell electrolyte, the solute of this electrolyte contains thiophenol, alkyl magnesium halide and alchlor, or thiophenol, dialkyl magnesium and alchlor, and solvent is ethers;
Wherein, thiophenol is preferably by toluene-ω-thiol, the 2-thionaphthol, benzenethiol, to bromo thiophenol, the 4-chlorothio-phenol, between thiocresol, reptazin, to fluoro thiophenol, between fluoro thiophenol, adjacent fluoro thiophenol, the 3-chlorothio-phenol, the 2-chlorothio-phenol, o-toluene thiophenol, the phenyl-pentafluoride thiophenol, near amino thiophenols, 1,3-diphenyl disulfide phenol, thiohydroquinone, p-Nitrobenzenethiol, the 2-hydroxythiophenol, 2, the 4-thiophenol dichlorobenzene, the 3-methoxybenzenethiol, the p-isopropyl benzenethiol, 2, the 4-difluoro thiophenol, the 2-methoxybenzenethiol, between hydroxythiophenol, 3, the 5-thiophenol dichlorobenzene, the 3-aminothiophenol, the 3-ethoxylated thiophenol, 3, the 4-thiophenol dichlorobenzene, 2, the 5-thiophenol dichlorobenzene, 4-chloro-phenyl tetrafluoride thiophenol, 3-chloro-4-fluoro thiophenol, o-isopropyl phenyl thiophenol, 2, the 6-thiophenol dichlorobenzene, 3, the 4-difluoro thiophenol, 3,4-dimethoxy benzenethiol, at least a material in the group that 4-(trifluoromethyl) benzenethiol forms;
In electrolyte of the present invention, described alkyl is aryl or aliphatic group; Wherein, aliphatic group is that the number of carbon is C less than or equal to 15(
1-C
15) the straight or branched alkyl.
Solvent ether is preferably at least a material in the group that is comprised of oxolane, 2-methyltetrahydrofuran, DOX, diethyl ether, glycol dimethyl ether and tetraethyleneglycol dimethyl ether.
In the specific embodiment of the present invention, the alkyl magnesium halide is preferably alkyl magnesium bromide or alkyl magnesium chloride, for example phenyl-magnesium-bromide, phenyl-magnesium-chloride, methyl-magnesium-bromide, ethylmagnesium chloride, tert-butyl group chlorination magnesium, cyclopenta magnesium chloride, hexyl magnesium bromide, octyl group magnesium chloride, dodecyl chlorination magnesium, or pentadecyl bromination magnesium etc.
Dialkyl magnesium is preferably diphenyl magnesium, dimethyl magnesium, magnesium ethide, dibutylmagnesium or dihexyl magnesium etc.
In preferred embodiments of the present invention, the molar ratio of thiophenol and alkyl magnesium halide is 1:1 in the electrolyte, and the molar ratio of thiophenol and dialkyl magnesium is 1:1; The molar ratio of alchlor and thiophenol is 0:1～1:1;
In another preferred embodiments of the present invention, concentration of electrolyte is 0.2～2molL
-1
On the other hand, the present invention also provides the application of a kind of above-mentioned electrolyte in rechargeable magnesium cell.
When electrolyte of the present invention was applied in the rechargeable magnesium cell, the concrete operations of its method of testing were as follows:
In the triode, add 2～5mL electrolyte of the present invention, adopt metal to make the work electrode, magnesium metal is done electrode and reference electrode, is assembled into three-electrode system; Carry out cyclic voltammetry in the argon gas glove box, sweep speed is 1～300mVs
-1
It is anodal to adopt metal to do, and magnesium metal is made negative pole, and polyethylene film is barrier film, adds 0.1～0.5mL electrolyte, is assembled into button cell, carries out the test of magnesium deposition-dissolving out capability, and charging and discharging currents is 0.01～10mAcm
-2, discharging 5～120 minutes, charge cutoff voltage is 0.8V vs.Mg.
In a preferred embodiment of the present invention, the electrolyte that adds in the method for testing is 0.2～2molL
-1Electrolyte.
In an application of the invention, the metal of use is preferably platinum, copper, aluminium, nickel, silver, titanium or stainless steel.
In an application of the invention, when rechargeable magnesium cell adopts the electrolyte of thiophenol-alkyl magnesium halide/ethereal solution or thiophenol-dialkyl magnesium/ethereal solution, its anodic oxidation decomposition electric potential can reach more than the 2.3V vs.Mg, and the magnesium deposition-dissolution efficiency behind this stable system is higher than 90%.When rechargeable magnesium cell further adopts the electrolyte of thiophenol-alkyl magnesium halide and alchlor/ether or thiophenol-dialkyl magnesium and alchlor/ethereal solution, its anodic oxidation decomposition electric potential can be near 3.0V vs.Mg, and the magnesium deposition-dissolution efficiency behind this stable system is higher than 90%.Electrolyte of the present invention has the advantage that the preparation method is simple, raw material cheap, magnesium deposition-Stripping Currents is large, the anodic oxidation decomposition electric potential is high.
Be described further below with reference to the technique effect of accompanying drawing to design of the present invention, concrete structure and generation, to understand fully purpose of the present invention, feature and effect.
Description of drawings
Fig. 1 is the 0.66molL that embodiments of the invention 1 make
-1Toluene-ω-thiol-ethylmagnesium bromide/the cyclic voltammetry curve of oxolane electrolyte on the platinum work electrode;
Fig. 2 is the 0.4molL that embodiments of the invention 2 make
-1Alchlor+toluene-ω-thiol-ethylmagnesium bromide (the 0.5:1)/cyclic voltammetry curve of oxolane electrolyte on the platinum work electrode;
Fig. 3 is the 0.4molL that embodiments of the invention 2 make
-1Deposition-the stripping curve of alchlor+toluene-ω-thiol-ethylmagnesium bromide (0.5:1)/oxolane electrolyte magnesium on copper;
Fig. 4 is the 0.4molL that embodiments of the invention 2 make
-1The deposition of alchlor+toluene-ω-thiol-ethylmagnesium bromide (0.5:1)/oxolane electrolyte magnesium on copper-dissolution efficiency figure;
Fig. 5 is the 0.4molL that embodiments of the invention 3 make
-1Alchlor+isopropylbenzene thiophenol-ethylmagnesium bromide (the 0.5:1)/cyclic voltammetry curve of oxolane electrolyte on the platinum work electrode;
Fig. 6 is the 0.25molL that Comparative Examples 1 of the present invention makes
-1Mg (AlCl
2EtBu
2The cyclic voltammetry curve of)/oxolane electrolyte on the platinum work electrode.
Embodiment
Following examples are to further specify of the present invention, but the present invention not only is confined to following examples.
In the triode, adopt the platinum electrode of working, add the 0.66molL of 3mL
-1Toluene-ω-thiol-ethylmagnesium bromide/oxolane electrolyte, magnesium metal is done electrode and reference electrode, is assembled into three-electrode system, carries out cyclic voltammetry in the argon gas glove box, and sweep speed is 50mVs
-1The cyclic voltammetric result as shown in Figure 1, as shown in Figure 1, near the reduction-oxidation process that occurs-0.2V vs.Mg is corresponding to deposition and the stripping of magnesium, the anodic oxidation current potential can reach 1.6V vs.Mg.
It is anodal to adopt copper to do, and adds the 0.66molL of 0.3mL
-1Toluene-ω-thiol-ethylmagnesium bromide/oxolane electrolyte, magnesium metal is made negative pole, and polyethylene film is barrier film, is assembled into button cell, carries out the test of magnesium deposition-dissolving out capability, and charging and discharging currents is 0.088mAcm
-2, discharging 30 minutes, charge cutoff voltage is 0.8V vs.Mg.Deposition-the dissolution efficiency of magnesium is higher than 90% after the stable circulation.
In the triode, adopt the platinum electrode of working, add the 0.4molL of 3mL
-1Alchlor+toluene-ω-thiol-ethylmagnesium bromide (mol ratio is 0.5:1)/oxolane electrolyte, magnesium metal is done electrode and reference electrode, is assembled into three-electrode system, carries out cyclic voltammetry in the argon gas glove box, and sweep speed is 50mVs
-1The cyclic voltammetric result as shown in Figure 2, as shown in Figure 2, near the reduction-oxidation process that occurs-0.2V vs.Mg is corresponding to deposition and the stripping of magnesium, the anodic oxidation current potential can reach 2.3V vs.Mg.
It is anodal to adopt copper to do, and adds the 0.4molL of 0.3mL
-1Alchlor+toluene-ω-thiol-ethylmagnesium bromide (mol ratio is 0.5:1)/oxolane electrolyte, magnesium metal is made negative pole, and polyethylene film is barrier film, is assembled into button cell, carries out the test of magnesium deposition-dissolving out capability, and charging and discharging currents is 0.088mAcm
-2, discharging 30 minutes, charge cutoff voltage is 0.8V vs.Mg.Fig. 3 is magnesium deposition-stripping curve, and its sedimentation potential is-0.1V that the stripping current potential is 0.1V.Fig. 4 is deposition-dissolution efficiency figure, and the deposition-dissolution efficiency of magnesium is higher than 90% after the stable circulation as shown in Figure 4.
In the triode, adopt the platinum electrode of working, add the 0.4molL of 3mL
-1Alchlor+p-isopropyl benzenethiol-ethylmagnesium bromide (mol ratio is 0.5:1)/oxolane electrolyte, magnesium metal is done electrode and reference electrode, is assembled into three-electrode system, carries out cyclic voltammetry in the argon gas glove box, and sweep speed is 50mVs
-1The cyclic voltammetric result as shown in Figure 5, as shown in Figure 5, near the reduction-oxidation process that occurs-0.2V vs.Mg is corresponding to deposition and the stripping of magnesium, the anodic oxidation current potential can reach 2.5V vs.Mg.With 0.25molL in the Comparative Examples
-1Mg (AlCl
2EtBu
2The cyclic voltammetric result of)/oxolane electrolyte compares, and the deposition of magnesium-Stripping Currents value is larger.
Comparative Examples 1
In the triode, adopt the platinum electrode of working, add the 0.25molL of 3mL
-1Mg (AlCl
2EtBu
2)/oxolane electrolyte, magnesium metal is done electrode and reference electrode, is assembled into three-electrode system, carries out cyclic voltammetry in the argon gas glove box, and sweep speed is 50mVs
-1The cyclic voltammetric result as shown in Figure 6, as shown in Figure 6, near the reduction-oxidation process that occurs-0.2V vs.Mg is corresponding to deposition and the stripping of magnesium, the anodic oxidation current potential is 2.5V vs.Mg.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area need not creative work and just can design according to the present invention make many modifications and variations.Therefore, all in the art technical staff all should be in the determined protection range by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (6)
1. the electrolyte of a rechargeable magnesium cell is characterized in that, the solute of described electrolyte contains thiophenol, alkyl magnesium halide and alchlor, or thiophenol, dialkyl magnesium and alchlor, and solvent is ether;
Described thiophenol is for being selected from toluene-ω-thiol, the 2-thionaphthol, benzenethiol, to bromo thiophenol, the 4-chlorothio-phenol, between thiocresol, reptazin, to fluoro thiophenol, between fluoro thiophenol, adjacent fluoro thiophenol, the 3-chlorothio-phenol, the 2-chlorothio-phenol, o-toluene thiophenol, the phenyl-pentafluoride thiophenol, near amino thiophenols, 1,3-diphenyl disulfide phenol, thiohydroquinone, p-Nitrobenzenethiol, the 2-hydroxythiophenol, 2, the 4-thiophenol dichlorobenzene, the 3-methoxybenzenethiol, the p-isopropyl benzenethiol, 2, the 4-difluoro thiophenol, the 2-methoxybenzenethiol, between hydroxythiophenol, 3, the 5-thiophenol dichlorobenzene, the 3-aminothiophenol, the 3-ethoxylated thiophenol, 3, the 4-thiophenol dichlorobenzene, 2, the 5-thiophenol dichlorobenzene, 4-chloro-phenyl tetrafluoride thiophenol, 3-chloro-4-fluoro thiophenol, o-isopropyl phenyl thiophenol, 2, the 6-thiophenol dichlorobenzene, 3, the 4-difluoro thiophenol, 3,4-dimethoxy benzenethiol, at least a material in the group that 4-(trifluoromethyl) benzenethiol forms;
Described alkyl magnesium halide is selected from alkyl magnesium bromide or alkyl magnesium chloride;
Described alkyl is selected from aryl or C
1-C
15Aliphatic group.
2. the electrolyte of rechargeable magnesium cell as claimed in claim 1, wherein, described ether is at least a material that is selected from the group that oxolane, 2-methyltetrahydrofuran, DOX, diethyl ether, glycol dimethyl ether and tetraethyleneglycol dimethyl ether form.
3. the electrolyte of rechargeable magnesium cell as claimed in claim 1 or 2, wherein, the molar ratio of described thiophenol and alkyl magnesium halide is 1:1, the molar ratio of thiophenol and dialkyl magnesium is 1:1.
4. the electrolyte of rechargeable magnesium cell as claimed in claim 1 or 2, wherein, the molar ratio of described alchlor and thiophenol is 0:1～1:1.
5. the electrolyte of rechargeable magnesium cell as claimed in claim 1 or 2, wherein, described concentration of electrolyte is 0.2～2molL
-1
6. such as the application of the arbitrary described electrolyte of claim 1-5 in rechargeable magnesium cell.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106916173A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Monokaryon magnesium cation salt dissolving, its preparation method and application |
| WO2017113053A1 (en) * | 2015-12-28 | 2017-07-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Mononuclear magnesium cationized salt, preparation method and use thereof |
| CN109473714A (en) * | 2018-11-19 | 2019-03-15 | 哈尔滨工业大学 | A kind of preparation method and applications of magnesium sulphur battery electrolyte |
| CN109687027A (en) * | 2019-01-17 | 2019-04-26 | 上海交通大学 | A kind of rechargeable magnesium cell electrolyte and rechargeable magnesium cell |
| TWI674692B (en) * | 2014-11-28 | 2019-10-11 | 日商富士軟片和光純藥股份有限公司 | Magnesium-containing electrolyte solution |
| JP2020533378A (en) * | 2017-09-14 | 2020-11-19 | ダイソン・テクノロジー・リミテッド | Magnesium salt |
| WO2023145894A1 (en) * | 2022-01-31 | 2023-08-03 | パナソニックＩｐマネジメント株式会社 | Nonaqueous electrolyte for nonaqueous-electrolyte cell, and nonaqueous-electrolyte cell |
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| CN1365524A (en) * | 1999-07-29 | 2002-08-21 | 帕多瓦大学 | Magnesium-based (primary non-rechargeabel) and secondary (rechargeable) batteries |
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Non-Patent Citations (1)
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| WANG, FEI-FEI ET AL.: "A novel electrolyte system without a Grignard reagent for rechargeable magnesium batteries", 《CHEMICAL COMMUNICATIONS》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI674692B (en) * | 2014-11-28 | 2019-10-11 | 日商富士軟片和光純藥股份有限公司 | Magnesium-containing electrolyte solution |
| CN106916173A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院苏州纳米技术与纳米仿生研究所 | Monokaryon magnesium cation salt dissolving, its preparation method and application |
| WO2017113053A1 (en) * | 2015-12-28 | 2017-07-06 | 中国科学院苏州纳米技术与纳米仿生研究所 | Mononuclear magnesium cationized salt, preparation method and use thereof |
| CN106916173B (en) * | 2015-12-28 | 2019-03-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Monokaryon magnesium cation salt dissolving, preparation method and application |
| US10826125B2 (en) | 2015-12-28 | 2020-11-03 | Suzhou Institute Of Nano-Tech And Nano-Bionics (Sinano), Chinese Academy Of Sciences | Mono-nuclei cationized magnesium salt, preparation method and applications thereof |
| JP2020533378A (en) * | 2017-09-14 | 2020-11-19 | ダイソン・テクノロジー・リミテッド | Magnesium salt |
| JP7071493B2 (en) | 2017-09-14 | 2022-05-19 | ダイソン・テクノロジー・リミテッド | Magnesium salt |
| CN109473714A (en) * | 2018-11-19 | 2019-03-15 | 哈尔滨工业大学 | A kind of preparation method and applications of magnesium sulphur battery electrolyte |
| CN109473714B (en) * | 2018-11-19 | 2021-08-03 | 哈尔滨工业大学 | Preparation method and application of magnesium-sulfur battery electrolyte |
| CN109687027A (en) * | 2019-01-17 | 2019-04-26 | 上海交通大学 | A kind of rechargeable magnesium cell electrolyte and rechargeable magnesium cell |
| WO2023145894A1 (en) * | 2022-01-31 | 2023-08-03 | パナソニックＩｐマネジメント株式会社 | Nonaqueous electrolyte for nonaqueous-electrolyte cell, and nonaqueous-electrolyte cell |
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