CN101702447A - Nonaqueous electrolytic solution for high-voltage lithium ion batteries and preparation method and application thereof - Google Patents
Nonaqueous electrolytic solution for high-voltage lithium ion batteries and preparation method and application thereof Download PDFInfo
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a nonaqueous electrolytic solution for high-voltage lithium ion batteries and a preparation method and application thereof. In the invention, the preparation method comprises the following steps: mixing cyclic carbonate and chain carbonate according to the mass ratio of 1:(1.5-3), and purifying the mixture to obtain a nonaqueous solvent; then, dissolving lithium salts into the nonaqueous solvent to obtain a common electrolytic solution, wherein the concentration of the lithium salts is 0.8-1.5mol/L; and adding additives into the common electrolytic solution to obtain the nonaqueous electrolytic solution for high-voltage lithium ion batteries, wherein the using quality of the additives is 0.01-5% of the quality of the common electrolytic solution. The voltage of the high-voltage lithium ion batteries prepared from the nonaqueous electrolytic solution for high-voltage lithium ion batteries can reach 4.9V, and the cycle performance of the prepared high-voltage lithium ion batteries is improved. The preparation method of the invention is simple, and the prepared nonaqueous electrolytic solution for high-voltage lithium ion batteries has low cost and better application prospect.
Description
Technical field
The present invention relates to a kind of electrolyte of lithium ion battery, particularly a kind of nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries and preparation method thereof and application.
Background technology
Lithium ion battery becomes the research focus of present new energy field with advantages such as its operating voltage height, energy density are big and have extended cycle life.The operating voltage of existing lithium ion battery is 3.7V, and the charging cut-ff voltage is 4.2V, can not satisfy the requirement of 3G epoch to lithium ion battery.Therefore, the energy density of raising lithium ion battery seems more urgent.
The operating voltage that improves lithium ion battery is considered to improve the most effective a kind of method of its energy density.In theory, can be from improving the operating voltage that positive and negative pole material and electrolyte improve lithium ion battery.For this reason, the researcher has carried out a large amount of research, has developed diversified positive and negative pole material: be used for anodal material and comprise transition metal stratiform oxide, spinel oxide, olivine-type salt and transient metal sulfide or the like; Be used for negative material and comprise lamellar graphite, lithium titanate and silica-based and kamash alloy or the like.These positive and negative pole materials can satisfy the high-tension requirement of lithium ion battery 4.9V, but do not have the electrolyte of coupling, and the electrolyte of prior art can decompose more than 4.5V in a large number.
Because the instability of electrolyte under high potential causes oxidation Decomposition, make that the inflatable under high voltage condition of battery is serious, cycle performance is poor.No matter electrolyte system in constantly development and renewal, is that electrolyte lithium salt, novel organic solvent or the research of electrolysis additive are underway always also.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome existing lithium-ion electrolyte and causes oxidation Decomposition owing to instability under high potential, make the inflatable under high voltage condition of battery serious, the deficiency and the shortcoming of cycle performance difference, a kind of nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries is provided.
Another object of the present invention is to provide the described preparation method who is used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
A further object of the present invention is to provide the described application that is used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
Purpose of the present invention is achieved through the following technical solutions: a kind of nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries comprises following composition: cyclic carbonate, linear carbonate, lithium salts and additive; Wherein, cyclic carbonate and linear carbonate are pressed mass ratio 1: mix (1.5～3), the concentration of lithium salts in the mixed liquor that cyclic carbonate and linear carbonate form is 0.8～1.5mol/L, and the service quality of additive is equivalent to 0.01～5% of solution quality that above-mentioned cyclic carbonate, linear carbonate and lithium salts form;
Described additive is 2,3-dihydrofuran or 1,4-dioxy cyclic ethylene ether;
Described cyclic carbonate is preferably at least a in ethylene carbonate (EC), propene carbonate (PC) or the gamma-butyrolacton (GBL);
The form of described chain carbonic ether is liquid;
Described linear carbonate is preferably at least a in dimethyl carbonate, diethyl carbonate, Methylethyl carbonic ester, methyl-propyl carbonic ester or the ethyl propyl carbonic ester;
The concentration of described lithium salts is 0.8～1.2mol/L more preferably;
Described lithium salts is preferably LiPF
6, LiBF
4, LiClO
4, LiAsF
6, LiCF
3SO
3, LiN (CF
3SO
2)
2, LiBOB, LiDFOB, LiPF
4C
2O
4Or LiN (C
2F
5SO
2)
2In at least a;
The described preparation method who is used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries may further comprise the steps:
(1) cyclic carbonate and linear carbonate are pressed mass ratio 1: mix (1.5～3), and purifying obtains nonaqueous solvents;
(2) lithium salts is dissolved in the nonaqueous solvents that step (1) obtains, concentration is 0.8～1.5mol/L, obtains common electrolyte;
(3) add additive in the common electrolyte that step (2) obtains, the service quality of additive is 0.01～5% of a common electrolyte quality, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries;
The described purifying of step (1) is removal of impurities and dewaters;
Described removal of impurities preferably realizes by molecular sieve;
Described molecular sieve is preferably diameter
Molecular sieve;
Described dewatering preferably undertaken by at least a material in active carbon, calcium hydride, sodium hydride, anhydrous calcium oxide or the phosphorus pentoxide;
The mode that described lithium salts in the step (2) adds described nonaqueous solvents adds for dividing 2 times at least, and the temperature of the described common electrolyte of generation will be controlled at below 40 ℃;
The described nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries is applied to prepare high-voltage lithium;
Described high voltage refers to the voltage of 4.9V.
Inventive principle of the present invention: 2,3-dihydrofuran, 1,4-dioxy cyclic ethylene ether has high reaction activity and high, can show the generation oxidative decomposition at positive pole prior to electrolyte solvent, forms anodal interfacial film.Anodal interfacial film can suppress the bad interaction between intercalation materials of li ions and electrolyte solution, has suppressed the oxidation Decomposition of electrolyte under the high voltage condition, thereby improves the performance of high-voltage lithium ion batteries.
The present invention has following advantage and effect with respect to prior art:
(1) use the voltage of the high-voltage lithium that the nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries of the present invention prepares to reach 4.9V, and the cycle performance of the high-voltage lithium ion batteries that makes increase.
(2) preparation method of the present invention is simple, and cost is low, has application promise in clinical practice.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) are mixed, mass ratio is EC: DMC: DEC=1: 1: 1, and adopt
Molecular sieve, calcium hydride and sodium hydride removal of impurities and dewater, decompress filter in being full of the glove box of high-purity argon gas obtains nonaqueous solvents then;
(2) with LiPF
6Gradation adds in the nonaqueous solvents, and adition process is controlled temperature below 40 ℃, LiPF
6Concentration be 1mol/L, and stir, obtain common electrolyte;
(3) in common electrolyte, add 2,5-dihydrofuran, consumption are common electrolyte quality 0.5%, obtain being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the nonaqueous electrolytic solution 30 μ l that obtain being used for high-voltage lithium ion batteries.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial capacity is 1.76mAh, circulates that the discharge capacity of battery is 1.34mAh after 50 times, and capability retention is 76.1%, has illustrated that lithium ion battery cycle life under high voltage of the nonaqueous electrolytic solution preparation of present embodiment preparation is improved.
Embodiment 2
Use the common electrolyte of embodiment 1 preparation, add 1,4-dioxy cyclic ethylene ether, consumption is common electrolyte quality 0.2%, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the nonaqueous electrolytic solution 30 μ L that are used for high-voltage lithium ion batteries.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial capacity is 1.44mAh, circulates that the discharge capacity of battery is 1.11mAh after 50 times, and capability retention is 77.1%, has illustrated that lithium ion battery cycle life under high voltage of the nonaqueous electrolytic solution preparation of present embodiment preparation is improved.
Embodiment 3
(1) ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) are mixed, mass ratio is EC: DMC: DEC=1: 0.5: 1, and adopt
Molecular sieve, calcium hydride and sodium hydride removal of impurities and dewater, decompress filter in being full of the glove box of high-purity argon gas obtains nonaqueous solvents then;
(2) with LiPF
6Gradation adds in the nonaqueous solvents, and adition process is controlled temperature below 40 ℃, LiPF
6Concentration be 1.5mol/L, and stir, obtain common electrolyte;
(3) in common electrolyte, add 2,5-dihydrofuran, consumption are common electrolyte quality 0.01%, obtain being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the nonaqueous electrolytic solution 30 μ l that obtain being used for high-voltage lithium ion batteries.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial capacity is 1.74mAh, circulates that the discharge capacity of battery is 1.32mAh after 50 times, and capability retention is 75.9%, has illustrated that lithium ion battery cycle life under high voltage of the nonaqueous electrolytic solution preparation of present embodiment preparation is improved.
Embodiment 4
Use the common electrolyte of embodiment 3 preparations, add 1,4-dioxy cyclic ethylene ether, consumption is common electrolyte quality 0.01%, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the nonaqueous electrolytic solution 30 μ L that are used for high-voltage lithium ion batteries.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial capacity is 1.41mAh, circulates that the discharge capacity of battery is 1.08mAh after 50 times, and capability retention is 76.6%, has illustrated that lithium ion battery cycle life under high voltage of the nonaqueous electrolytic solution preparation of present embodiment preparation is improved.
Embodiment 5
(1) ethylene carbonate (EC), dimethyl carbonate (DMC) and diethyl carbonate (DEC) are mixed, mass ratio is EC: DMC: DEC=1: 2: 1, and adopt
Molecular sieve, calcium hydride and sodium hydride removal of impurities and dewater, decompress filter in being full of the glove box of high-purity argon gas obtains nonaqueous solvents then;
(2) with LiPF
6Gradation adds in the nonaqueous solvents, and adition process is controlled temperature below 40 ℃, LiPF
6Concentration be 0.8mol/L, and stir, obtain common electrolyte;
(3) in common electrolyte, add 2,5-dihydrofuran, consumption are common electrolyte quality 5%, obtain being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the nonaqueous electrolytic solution 30 μ l that obtain being used for high-voltage lithium ion batteries.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial capacity is 1.78mAh, circulates that the discharge capacity of battery is 1.36mAh after 50 times, and capability retention is 76.4%, has illustrated that lithium ion battery cycle life under high voltage of the nonaqueous electrolytic solution preparation of present embodiment preparation is improved.
Embodiment 6
Use the common electrolyte of embodiment 5 preparations, add 1,4-dioxy cyclic ethylene ether, consumption is common electrolyte quality 5%, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the nonaqueous electrolytic solution 30 μ l that are used for high-voltage lithium ion batteries.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial capacity is 1.51mAh, circulates that the discharge capacity of battery is 1.2mAh after 50 times, and capability retention is 79.5%, has illustrated that lithium ion battery cycle life under high voltage of the nonaqueous electrolytic solution preparation of present embodiment preparation is improved.
The comparative example
With Li
1.17Mn
0.58Ni
0.25O
2Be positive electrode; Negative pole is that carbonaceous mesophase spherules (MCMB) is formed button cell, adds the common electrolyte 30 μ l of embodiment 1 preparation.Under 25 ℃ of constant temperature of room temperature, to discharging and recharging between 4.9V battery is activated at 2.0V with 1/20C, 1/10C and 1/5C respectively, circulation subsequently all 1/5C discharge and recharge.The battery initial discharge capacity is 1.66mAh, circulates that the discharge capacity of battery is 1.07mAh after 50 times, and capability retention is 64.4%, as seen do not contain 2,5-dihydrofuran or 1, the button cell cycle performance of the common electrolyte preparation of 4-dioxy cyclic ethylene ether is relatively poor, and capacity attenuation is fast.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries is characterized in that: comprise following composition: cyclic carbonate, linear carbonate, lithium salts and additive; Wherein, cyclic carbonate and linear carbonate are pressed mass ratio 1: mix (1.5～3), the concentration of lithium salts in the mixed liquor that cyclic carbonate and linear carbonate form is 0.8～1.5mol/L, and the service quality of additive is equivalent to 0.01～5% of solution quality that above-mentioned cyclic carbonate, linear carbonate and lithium salts form; Described additive is 2,3-dihydrofuran or 1,4-dioxy cyclic ethylene ether.
2. the nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries according to claim 1 is characterized in that: described cyclic carbonate is at least a in ethylene carbonate, propene carbonate or the gamma-butyrolacton.
3. the nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries according to claim 1 is characterized in that: described linear carbonate is at least a in dimethyl carbonate, diethyl carbonate, Methylethyl carbonic ester, methyl-propyl carbonic ester or the ethyl propyl carbonic ester.
4. the nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries according to claim 1 is characterized in that: the concentration of described lithium salts is 0.8～1.2mol/L.
5. the nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries according to claim 1 is characterized in that: described lithium salts is LiPF
6, LiBF
4, LiClO
4, LiAsF
6, LiCF
3SO
3, LiN (CF
3SO
2)
2, LiBOB, LiDFOB, LiPF
4C
2O
4Or LiN (C
2F
5SO
2)
2In at least a.
6. each described preparation method who is used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries of claim 1～5 is characterized in that: may further comprise the steps:
(1) cyclic carbonate and linear carbonate are pressed mass ratio 1: mix (1.5～3), and purifying obtains nonaqueous solvents;
(2) lithium salts is dissolved in the nonaqueous solvents that step (1) obtains, concentration is 0.8～1.5mol/L, obtains common electrolyte;
(3) add additive in the common electrolyte that step (2) obtains, the service quality of additive is 0.01～5% of a common electrolyte quality, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
7. preparation method according to claim 6 is characterized in that: the described purifying of step (1) is removal of impurities and dewaters.
8. preparation method according to claim 6 is characterized in that: the mode that the described lithium salts in the step (2) adds described nonaqueous solvents adds for dividing 2 times at least, and the temperature of the described common electrolyte of generation is controlled at below 40 ℃.
9. each described application that is used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries of claim 1～5, it is characterized in that: the described nonaqueous electrolytic solution that is used for high-voltage lithium ion batteries is applied to prepare high-voltage lithium.
10. application according to claim 9 is characterized in that: described high voltage refers to 4.9V voltage.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102024989A (en) * | 2010-11-26 | 2011-04-20 | 南开大学 | Preparation method of high-voltage lithium-ion battery |
| CN102751533A (en) * | 2012-06-14 | 2012-10-24 | 合肥国轩高科动力能源有限公司 | Functional additive for high-voltage working electrolyte of lithium ion battery and preparation method of electrolyte |
| CN103401021A (en) * | 2013-08-23 | 2013-11-20 | 轻工业化学电源研究所 | Non-aqueous electrolyte and lithium titanate battery |
| CN103515651A (en) * | 2013-10-29 | 2014-01-15 | 华南师范大学 | High voltage carbonic ester base electrolyte of lithium ion battery as well as preparation method and application thereof |
| CN103545552A (en) * | 2013-10-14 | 2014-01-29 | 合肥国轩高科动力能源股份公司 | Electrolyte suitable for high-voltage lithium ion battery |
| CN103891036A (en) * | 2011-10-17 | 2014-06-25 | 宇部兴产株式会社 | Non-aqueous electrolyte solution and electricity-storage device using same |
| CN103928707A (en) * | 2014-05-07 | 2014-07-16 | 华南师范大学 | High voltage lithium ion battery functional electrolyte and preparation method and application |
| CN104157903A (en) * | 2014-08-22 | 2014-11-19 | 华南师范大学 | High-voltage lithium ion battery carbonate-based electrolyte solution and preparation method and application thereof |
| CN104733781A (en) * | 2015-03-27 | 2015-06-24 | 山东海容电源材料有限公司 | 4.4V high-voltage lithium cobalt oxide lithium battery electrolyte solution |
| CN105826606A (en) * | 2016-05-16 | 2016-08-03 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery containing same |
| CN107808981A (en) * | 2016-09-09 | 2018-03-16 | 中国科学院宁波材料技术与工程研究所 | Electrolyte and lithium ion battery |
| CN113871712A (en) * | 2021-09-24 | 2021-12-31 | 远景动力技术(江苏)有限公司 | Lithium ion battery electrolyte, preparation method thereof and lithium ion battery |
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2009
- 2009-11-03 CN CN200910193637A patent/CN101702447A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102024989A (en) * | 2010-11-26 | 2011-04-20 | 南开大学 | Preparation method of high-voltage lithium-ion battery |
| CN103891036A (en) * | 2011-10-17 | 2014-06-25 | 宇部兴产株式会社 | Non-aqueous electrolyte solution and electricity-storage device using same |
| CN103891036B (en) * | 2011-10-17 | 2016-01-06 | 宇部兴产株式会社 | Nonaqueous electrolytic solution and employ the electric energy storage device of this nonaqueous electrolytic solution |
| CN102751533A (en) * | 2012-06-14 | 2012-10-24 | 合肥国轩高科动力能源有限公司 | Functional additive for high-voltage working electrolyte of lithium ion battery and preparation method of electrolyte |
| CN103401021A (en) * | 2013-08-23 | 2013-11-20 | 轻工业化学电源研究所 | Non-aqueous electrolyte and lithium titanate battery |
| CN103401021B (en) * | 2013-08-23 | 2016-02-03 | 轻工业化学电源研究所 | A kind of nonaqueous electrolytic solution and lithium titanate battery |
| CN103545552A (en) * | 2013-10-14 | 2014-01-29 | 合肥国轩高科动力能源股份公司 | Electrolyte suitable for high-voltage lithium ion battery |
| CN103545552B (en) * | 2013-10-14 | 2016-03-09 | 合肥国轩高科动力能源有限公司 | Electrolyte suitable for high-voltage lithium ion battery |
| CN103515651B (en) * | 2013-10-29 | 2016-08-17 | 华南师范大学 | A kind of lithium ion battery high-voltage carbonate group electrolyte and preparation method and application |
| CN103515651A (en) * | 2013-10-29 | 2014-01-15 | 华南师范大学 | High voltage carbonic ester base electrolyte of lithium ion battery as well as preparation method and application thereof |
| CN103928707A (en) * | 2014-05-07 | 2014-07-16 | 华南师范大学 | High voltage lithium ion battery functional electrolyte and preparation method and application |
| CN104157903A (en) * | 2014-08-22 | 2014-11-19 | 华南师范大学 | High-voltage lithium ion battery carbonate-based electrolyte solution and preparation method and application thereof |
| CN104733781A (en) * | 2015-03-27 | 2015-06-24 | 山东海容电源材料有限公司 | 4.4V high-voltage lithium cobalt oxide lithium battery electrolyte solution |
| CN105826606A (en) * | 2016-05-16 | 2016-08-03 | 宁德时代新能源科技股份有限公司 | Electrolyte and lithium ion battery containing same |
| CN107808981A (en) * | 2016-09-09 | 2018-03-16 | 中国科学院宁波材料技术与工程研究所 | Electrolyte and lithium ion battery |
| CN113871712A (en) * | 2021-09-24 | 2021-12-31 | 远景动力技术(江苏)有限公司 | Lithium ion battery electrolyte, preparation method thereof and lithium ion battery |
| CN113871712B (en) * | 2021-09-24 | 2024-01-26 | 远景动力技术(江苏)有限公司 | Lithium ion battery electrolyte, preparation method thereof and lithium ion battery |
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