CN102751533A - Functional additive used for high-voltage work electrolyte of lithium ion battery, and electrolyte preparation method - Google Patents
Functional additive used for high-voltage work electrolyte of lithium ion battery, and electrolyte preparation method Download PDFInfo
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- CN102751533A CN102751533A CN2012101971282A CN201210197128A CN102751533A CN 102751533 A CN102751533 A CN 102751533A CN 2012101971282 A CN2012101971282 A CN 2012101971282A CN 201210197128 A CN201210197128 A CN 201210197128A CN 102751533 A CN102751533 A CN 102751533A
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Abstract
The invention provides a functional additive used for a high-voltage work electrolyte of a lithium ion battery, and an electrolyte preparation method. A common carbonate is adopted as a solvent served as an organic solvent component of the electrolyte, a lithium salt LiPF6 is dissolved in a non-aqueous solvent to make the concentration of the lithium salt be 1.0-1.2mol/l to obtain a common high-voltage electrolyte, the necessary functional additive having a mass being 1.0-3.5% of the mass of the electrolyte composed of the carbonate solvent and the lithium salt is added to the common high-voltage electrolyte, and the high-voltage cycle performance of the lithium ion battery can be effectively improved and the oxidation resistance of the routine carbonate electrolyte is improved to 5.0V through using the additive. The additive has the advantages of low cost, obvious effects, and good application prospect.
Description
Technical field:
The present invention relates to a kind of lithium ion battery high-pressure work electrolysis liquid, particularly can be used in the functional additive and the preparation method of electrolyte of lithium ion battery high-pressure work electrolysis liquid.
Background technology:
These two problems of the environmental pollution that energy crisis and fuel oil vehicle emissions toxic gas cause come into one's own just day by day, and are being one of basic ways that addresses this problem at flourish electric motor car just.What electric motor car needed is high-power battery.Though lithium ion battery has many good performances, the power of lithium ion battery is still very low at present.The power of lithium ion battery is relevant with operating voltage, so lithium ion battery will be used in the electric automobile field on a large scale, must further improve their operating voltage, and operating voltage is mainly by the performance decision of cell positive material.The positive electrode that research and development have a high working voltage is the lithium ion battery inexorable trend that lithium ion battery develops when being applied to pure electric automobile (EV), hybrid-electric car (HEV) field of etc.ing as the high power electrical source of power.
Exploitation high potential positive electrode just needs can be at the electrolyte of steady operation under the high voltage.Since historical reasons, present widely used LiPF
6The main application fields of electrolyte is to be positive pole with cobalt acid lithium; With graphite is the lithium ion battery of negative pole; The operating voltage of this type battery is the highest also can only to reach 4.2V; So the design of electrolyte system also generally can only guarantee in the scope below 4.5V stable the use, and high potential positive electrode-nickel LiMn2O4, its high charge cut-ff voltage can reach 5.2V; Therefore conventional electrolysis liquid oxidation Decomposition problem with this understanding becomes obviously, so it is most important to develop suitable high-voltage lithium ion batteries Working electrolyte.
At present, the exploitation of high voltage electrolyte mainly is to realize through in common high-pressure electrolysis liquid, adding necessary function property additive.Document Electrochemistry Communications (2007; 9:801 – 806) and show all among patent CN 101702447 A that the adding of functional additive is improved the barotolerance of electrolyte, the cycle performance of the high-voltage lithium ion batteries of preparation is significantly improved.
Summary of the invention:
Primary and foremost purpose of the present invention is to be provided for lithium ion battery high-pressure work electrolysis liquid functional additive and preparation method of electrolyte; To satisfy the demand of high-voltage lithium ion batteries to high voltage electrolyte; Use this additive that electrolyte stability is improved; Can oxidation Decomposition about 5V, can effectively improve the cycle life of lithium ion battery.This electrolyte adopts the carbonates organic solvent system of purifying; And cooperation succinic anhydride (SA) and 2; (2,5DF) anodal film for additive has stopped the contact-making surface of electrolyte and positive electrode active materials to the 5-dihydrofuran; Slowed down this oxidation Decomposition of electrolyte effectively, thereby prepared high pressure resistant Working electrolyte in surface of active material.
The object of the invention is realized through following technical scheme: adopting common carbonates is that solvent serves as electrolyte organic solvent part, then with lithium salts LiPF
6Be dissolved in the nonaqueous solvents; Lithium salt is 1.0～1.2mol/l; Can obtain common high-pressure type electrolyte, in common high-pressure type electrolyte, add the necessary function additive again, its consumption is equivalent to carbonate solvent and lithium salts is formed 1.0～3.5% of electrolyte quality; Last evenly mixing can obtain lithium ion battery high pressure worker additive.
The functional additive that is used for lithium ion battery high-pressure work electrolysis liquid; It is characterized in that: its consumption is equivalent to carbonate solvent and lithium salts is formed 1.0～3.5% of electrolyte quality; Described functional additive is a succinic anhydride (SA) or/and 2, and the 5-dihydrofuran (2,5DF).
Said functional additive consumption is 1.0～2.5% of a described electrolyte quality.
Described lithium salts is LiPF
6, LiBF
4, LiClO
4, at least a among the LiBOB.
Contain the preparation method of the lithium ion battery high-pressure work electrolysis liquid of described functional additive, it is characterized in that, comprise following processing step:
⑴. with cyclic carbonate and linear carbonate elder generation purifying, then according to volume ratio 1: (2～3) mixing obtains the organic mixed solvent of non-water;
⑵. lithium salts is dissolved in the organic mixed solvent of the non-water of step ⑴, and concentration is 1.0～1.2mol/l, obtains common high-pressure type electrolyte;
⑶. in the common high-pressure type electrolyte that step ⑵ obtains, add functional additive succinic anhydride (SA) and 2, (2,5DF), the consumption of additive is 1.0～3.5% of a common high-pressure electrolysis liquid quality to the 5-dihydrofuran, obtains lithium ion battery high-pressure work electrolysis liquid.
The described cyclic carbonate of step ⑴ is at least a in ethylene carbonate, the propene carbonate; Linear carbonate is one or both in methyl ethyl carbonate, dimethyl carbonate and the diethyl carbonate.
The described carbonate solvent purifying of step ⑴ is meant removal of impurities and dewaters.
The described lithium salts of step ⑵ must constantly slowly add under the stirring condition, and ambient temperature is controlled at below 35 ℃.
Dewater and preferentially adopt at least a processing the in calcium hydride, sodium hydride, the magnesium sulfate, it is 4 molecular sieves that diameter is selected in removal of impurities for use.
The principle of the invention: on the carbonic ester mixed solvent system basis of existing tolerance 4.2～4.5V voltage, add blended anode film for additive succinic anhydride (SA) and 2,5-dihydrofuran (2; 5DF); These two kinds of additive reaction activity are higher, in battery first charge-discharge process, can form anodal SEI film preferentially in surface of positive electrode active material generation oxidation Decomposition; Thereby suppress the reaction of positive electrode active materials and electrolyte; Improved the useful life of electrolyte, therefore, the overall performance of high-voltage lithium ion batteries has obtained bigger lifting.
The present invention has the following advantages and effect with respect to present prior art:
(1) utilization high-pressure work electrolysis liquid functional additive of the present invention can make the decomposition electric potential of conventional electrolysis liquid bring up to 5.0V, satisfies the demand of high-voltage anode material to high voltage electrolyte, and the cycle performance of lithium ion battery is highly improved;
(2) two kinds of additive costs of the present invention are lower, and anodal film-formation result is good, has a extensive future.
Description of drawings:
Fig. 1 doesLithium ion battery high-pressure work electrolysis liquid preparing process flow process.
Embodiment:
Below in conjunction with embodiment the present invention is done further detailed description, but execution mode of the present invention is not limited thereto.
Embodiment 1
At first, ethylene carbonate (EC), methyl ethyl carbonate (EMC), dimethyl carbonate (DMC) being dewatered with calcium hydride earlier, dewater with 4 molecular sieve removal of impurities, is that EC/EMC/DEC (1:1:1vol) makes nonaqueous solvents according to volume ratio then; Secondly, under 35 ℃ of following conditions with lithium salts LiPF
6Slowly be dissolved in the nonaqueous solvents, compound concentration is the common high-pressure electrolysis liquid of 1mol/l, and the process for preparation of whole electrolyte must be accomplished in being full of the glove box of high-purity argon gas.。
With LiNi
0.5Mn
1.5O
4Be positive electrode, the lithium sheet is that negative material, nickel foam are negative current collector, adds the common high-pressure electrolysis liquid 30 μ l that prepare; Under 25 ℃ of room temperature conditions with 0.5C to battery charging and discharging; The battery initial capacity is 50mAh, and after 100 circulations, the battery capacity conservation rate is 38.7%; The battery cycle life reduction under high pressure of plain edition high-pressure electrolysis liquid preparation has been used in this explanation, and capacity attenuation is very fast.
Embodiment 2
The common high-pressure electrolysis liquid of the 1mol/l that employing embodiment 1 prepares adds additive succinic anhydride (SA) then in the common high-pressure electrolysis liquid of preparation, consumption is 2% of a common high-pressure electrolysis liquid quality, obtains being used for the high-pressure work electrolysis liquid of lithium ion battery.
With LiNi
0.5Mn
1.5O
4Be positive electrode; The lithium sheet is that negative material, nickel foam are that negative current collector is formed button cell, adds the high-pressure work electrolysis liquid 30 μ l that prepare, under 25 ℃ of room temperature conditions with 0.5C to battery charging and discharging; The battery initial capacity is 50mAh; After 100 circulations, the battery capacity conservation rate is 77.3%, this explanation used preparation the preparation of high-pressure electrolysis liquid battery under high pressure cycle life be greatly improved.
Embodiment 3
Utilize the common high-pressure electrolysis liquid of embodiment 1 preparation, add additive 2, (2,5DF), consumption is 3% of a common high-pressure electrolysis liquid quality to the 5-dihydrofuran, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With LiNi
0.5Mn
1.5O
4Be positive electrode; The lithium sheet is that negative material, nickel foam are negative current collector, adds the high-pressure work electrolysis liquid 30 μ l prepare, under 25 ℃ of room temperature conditions with 0.5C to battery charging and discharging; The battery initial capacity is 50mAh; After 100 circulations, the battery capacity conservation rate is 76%, this explanation used preparation the preparation of high-pressure electrolysis liquid battery under high pressure cycle life be greatly improved.
Embodiment 4
Utilize the electrolyte of embodiment 1 preparation, add additive succinic anhydride (SA), 2, (2,5DF), consumption is respectively 2% and 3% of common high-pressure electrolysis liquid quality to the 5-dihydrofuran, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With LiNi
0.5Mn
1.5O
4Be positive electrode; The lithium sheet is that negative material, nickel foam are negative current collector, adds the high-pressure work electrolysis liquid 30 μ l prepare, under 25 ℃ of room temperature conditions with 0.5C to battery charging and discharging; The battery initial capacity is 50mAh; After 100 circulations, the battery capacity conservation rate is 81.5%, and the battery that the high-pressure electrolysis liquid that this explanation has used additive package to prepare prepares under high pressure cycle life has obtained significant raising.
Embodiment 5
At first, ethylene carbonate (EC), methyl ethyl carbonate (EMC), dimethyl carbonate (DMC) being dewatered with calcium hydride earlier, dewater with 4 molecular sieve removal of impurities, is that EC/EMC/DEC (1:1:2vol) makes nonaqueous solvents according to volume ratio then; Secondly, under 35 ℃ of following conditions with lithium salts LiPF
6Slowly be dissolved in the nonaqueous solvents, compound concentration is the common high-pressure electrolysis liquid of 1.2mol/l; At last, in the common high-pressure electrolysis liquid of preparation, add additive succinic anhydride (SA), consumption is 2% of a common electrolyte quality; 2, (2,5DF), consumption is respectively 3% of common high-pressure electrolysis liquid quality to the 5-dihydrofuran, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With LiNi
0.5Mn
1.5O
4Be positive electrode; The lithium sheet is that negative material, nickel foam are negative current collector, adds the high-pressure work electrolysis liquid 30 μ l prepare, under 25 ℃ of room temperature conditions with 0.5C to battery charging and discharging; The battery initial capacity is 50mAh; After 100 circulations, the battery capacity conservation rate is 80.1%, and the battery that the high-pressure electrolysis liquid that this explanation has used additive package to prepare prepares under high pressure cycle life has obtained higher lifting.
Embodiment 6
At first, ethylene carbonate (EC), methyl ethyl carbonate (EMC), dimethyl carbonate (DMC) being dewatered with calcium hydride earlier, dewater with 4 molecular sieve removal of impurities, is that EC/EMC/DEC (1:2:1vol) makes nonaqueous solvents according to volume ratio then; Secondly, under 35 ℃ of following conditions with lithium salts LiPF
6Slowly be dissolved in the nonaqueous solvents, compound concentration is the common high-pressure electrolysis liquid of 1.2mol/l; At last, in the common high-pressure electrolysis liquid of preparation, add additive succinic anhydride (SA), consumption is 2% of a common high-pressure electrolysis liquid quality; 2, (2,5DF), consumption is respectively 3% of common high-pressure electrolysis liquid quality to the 5-dihydrofuran, obtains being used for the nonaqueous electrolytic solution of high-voltage lithium ion batteries.
With LiNi
0.5Mn
1.5O
4Be positive electrode; The lithium sheet is that negative material, nickel foam are negative current collector, adds the high-pressure work electrolysis liquid 30 μ l prepare, under 25 ℃ of room temperature conditions with 0.5C to battery charging and discharging; The battery initial capacity is 50mAh; After 100 circulations, the battery capacity conservation rate is 80.3%, and the battery that the high-pressure electrolysis liquid that this explanation has used additive package to prepare prepares under high pressure cycle life has obtained significant raising.
Claims (8)
1. the functional additive that is used for lithium ion battery high-pressure work electrolysis liquid; It is characterized in that: its consumption is equivalent to carbonate solvent and lithium salts is formed 1.0～3.5% of electrolyte quality; Described functional additive is a succinic anhydride (SA) or/and 2, and the 5-dihydrofuran (2,5DF).
2. the functional additive that is used for lithium ion battery high-pressure work electrolysis liquid according to claim 1 is characterized in that: said functional additive consumption is 1.0～2.5% of a described electrolyte quality.
3. the functional additive that is used for lithium ion battery high-pressure work electrolysis liquid according to claim 1 is characterized in that: described lithium salts is LiPF
6, LiBF
4, LiClO
4, at least a among the LiBOB.
4. contain the preparation method of the lithium ion battery high-pressure work electrolysis liquid of the described functional additive of claim 1, it is characterized in that, comprise following processing step:
⑴. with cyclic carbonate and linear carbonate elder generation purifying, then according to volume ratio 1: (2～3) mixing obtains the organic mixed solvent of non-water;
⑵. lithium salts is dissolved in the organic mixed solvent of the non-water of step ⑴, and concentration is 1.0～1.2mol/l, obtains common high-pressure type electrolyte;
⑶. in the common high-pressure type electrolyte that step ⑵ obtains, add functional additive succinic anhydride (SA) and 2, (2,5DF), the consumption of additive is 1.0～3.5% of a common high-pressure electrolysis liquid quality to the 5-dihydrofuran, obtains lithium ion battery high-pressure work electrolysis liquid.
5. the preparation method of lithium ion battery high-pressure work electrolysis liquid according to claim 4 is characterized in that: the described cyclic carbonate of step ⑴ is at least a in ethylene carbonate, the propene carbonate; Linear carbonate is one or both in methyl ethyl carbonate, dimethyl carbonate and the diethyl carbonate.
6. the preparation method of lithium ion battery high-pressure work electrolysis liquid according to claim 4 is characterized in that: the described carbonate solvent purifying of step ⑴ is meant removal of impurities and dewaters.
7. the preparation method of lithium ion battery high-pressure work electrolysis liquid according to claim 4 is characterized in that: the described lithium salts of step ⑵ must constantly slowly add under the stirring condition, and ambient temperature is controlled at below 35 ℃.
8. the preparation method of lithium ion battery high-pressure work electrolysis liquid according to claim 6 is characterized in that: preferential at least a processing the in calcium hydride, sodium hydride, the magnesium sulfate of adopting that dewater, it is 4 molecular sieves that diameter is selected in removal of impurities for use.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107369849A (en) * | 2017-08-04 | 2017-11-21 | 广州天赐高新材料股份有限公司 | A kind of lithium secondary cell electrolyte and lithium secondary battery |
| US10074874B2 (en) | 2012-06-01 | 2018-09-11 | Solvay Sa | Additives to improve electrolyte performance in lithium ion batteries |
| US10686220B2 (en) | 2013-04-04 | 2020-06-16 | Solvay Sa | Nonaqueous electrolyte compositions |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101702447A (en) * | 2009-11-03 | 2010-05-05 | 华南师范大学 | Nonaqueous electrolytic solution for high-voltage lithium ion batteries and preparation method and application thereof |
| CN101841065A (en) * | 2010-05-21 | 2010-09-22 | 东莞新能源科技有限公司 | Lithium-ion secondary battery and electrolyte thereof |
-
2012
- 2012-06-14 CN CN2012101971282A patent/CN102751533A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101702447A (en) * | 2009-11-03 | 2010-05-05 | 华南师范大学 | Nonaqueous electrolytic solution for high-voltage lithium ion batteries and preparation method and application thereof |
| CN101841065A (en) * | 2010-05-21 | 2010-09-22 | 东莞新能源科技有限公司 | Lithium-ion secondary battery and electrolyte thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10074874B2 (en) | 2012-06-01 | 2018-09-11 | Solvay Sa | Additives to improve electrolyte performance in lithium ion batteries |
| US10686220B2 (en) | 2013-04-04 | 2020-06-16 | Solvay Sa | Nonaqueous electrolyte compositions |
| US10916805B2 (en) | 2013-04-04 | 2021-02-09 | Solvay Sa | Nonaqueous electrolyte compositions |
| CN107369849A (en) * | 2017-08-04 | 2017-11-21 | 广州天赐高新材料股份有限公司 | A kind of lithium secondary cell electrolyte and lithium secondary battery |
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Application publication date: 20121024 |