CN103050706A - Maleimide additive for lithium battery and corresponding lithium battery anode formula - Google Patents
Maleimide additive for lithium battery and corresponding lithium battery anode formula Download PDFInfo
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Abstract
The invention discloses a maleimide additive for a lithium battery and a corresponding lithium battery anode formula. The additive is bismaleimide modified by cyanamide and melamine. For the battery prepared by the additive, a needling test proves that the stability of an obtained battery anode active material is increased, and the cycle life of the battery is prolonged. With the adoption of the additive, a protective film is formed on the surface of the anode active material, the anode active material can be prevented from being cracked during internal short circuit, and the battery is safer; in addition, as the good safe protective film is formed on the surface of the anode active material, the service life of the lithium battery is prolonged.
Description
Technical field
The present invention relates to the battery material field, be specifically related to a kind of lithium battery modified maleimide additive and corresponding lithium battery anode prescription.
Background technology
Lithium rechargeable battery is the concept that is proposed by Armand the eighties in 20th century, and the positive and negative pole material that he proposes battery adopts the lithium ion material that can store and exchange, and utilizes when discharging and recharging, and energy exchange is carried out in moving around of ion.
Produced by LiCoO by Japanese Sony Corporation in 1991
2For positive electrode, carbon black are the commercial Li-ion battery of negative material, since then, lithium ion battery has substituted rapidly NI-G, Ni-MH battery in various fields.Lithium ion battery is having very wide application prospect aspect electric motor car and the accumulate.Therefore, have solid polymer lithium ion battery ultra-thin, ultralight, high-energy-density and in succession be developed and move towards market.
But present lithium ion battery and not exclusively satisfy existing the use, there is poor heat stability in positive electrode especially of the prior art owing to reasons such as its atomic structures, causes under normal temperature or the high temperature cycle performance poor, and battery life is low, the problems such as fail safe deficiency.
Summary of the invention
For addressing the above problem, the present invention adopts cyanamide and cyanurotriamide modified maleimide, additive as lithium battery anode slurry, can get minus plate through conventional technology batch mixing coating film forming, then be made into battery, charging gets final product safely, the lithium ion battery of cycle life excellence under normal temperature and the high temperature after the encapsulation.
A kind of lithium battery refers to the modified maleimide modified by cyanamide and melamine with the maleimide additive.Described maleimide additive can be applicable to the anode formula composition material of lithium ion battery or lithium macromolecule battery.
The described lithium battery anode prescription that contains the modified maleimide additive contains the material of following percentage by weight:
(ⅰ) 0.1 ~ 5% by cyanamide and cyanurotriamide modified bismaleimides or/and single maleimide reaction products therefrom;
(ⅱ) 0.1 ~ 15% Kynoar, acrylic resin and butadiene-styrene rubber;
(ⅲ) positive active material;
(ⅳ) 0.1 ~ 5% conductive additive: such as KS6 or CGCF or SP or VGCF.
Further, positive active material is in the described anode formula material: LiCoO
2Or LiMnO
2Or LiFePO
4Or LNCM or NCA, or its mixture.
Further, bismaleimide structure is in the described anode formula material:
Wherein, m, n, o are 1,2,3,4,5
Or
Wherein, R can be a kind of in the following group :-(CH
2)
2-,-(CH
2)
6-,-(CH
2)
8-,-(CH
2)
12-,
,
,
,
,
,
Further, single maleimide can be a kind of in the following material in the described anode formula material:
(1). phenyl maleimide
(2). N-(to methylbenzene) maleimide
(3). N-(o-methyl-benzene) maleimide
(4). N-(methylbenzene) maleimide
(5). the N-CYCLOHEXANE maleimide
(6). maleimide
(7). dimaleoyl imino phenol
(8). the dimaleoyl imino benzocyclobutene
(9). phosphorous maleimide
(10). the phosphate-containing maleimide
(11). the silicone-containing maleimide
(12). N-(4-THP trtrahydropyranyl-hydroxyphenyl) maleimide
(13). 2,6-benzhydryl-maleimide.
Further, melamine or derivatives thereof in the described anode formula material, its structure can be:
Wherein, H can be by R
1, R
2, R
3, R
4, R
5, R
6Replace.Wherein, R
1, R
2, R
3, R
4, R
5, R
6Can be linearity or branched alkyl.
Further, cyanamide is in the described anode formula material:
Wherein, R
1, R
2Be H or linearity or branched alkyl.
Further, can add reaction initiator in the described anode formula material.
Further, the reaction initiator in the described anode formula material is peroxide or azodiisobutyronitrile.
Further, in the described anode formula material, (ⅳ) middle conductive additive can carry out surface treatment.
Further, in the described anode formula material, (ⅳ) surface treatment of middle conductive additive can be used following coupling agent:
(1) with the oxosilane coupling agent of vinyl-functional;
(2) unsaturated linear chain hydrocarbon carboxylic acids, its structural formula is:
CH
3(CH
2)
nCH=CH (CH
2)
nCOOH; N is 1 ~ 14 integer.
Further, the unsaturated linear chain hydrocarbon carboxylic acids of the coupling agent of described anode formula material is oleic acid.
Further, the mol ratio of bismaleimides or single maleimide and melamine or derivatives thereof is 25:1 ~ 1:1 in the described anode formula material.
Further, in the described anode formula material, (ⅰ) described in the mol ratio of melamine or derivatives thereof and amino nitrile be 1.0:1.0 ~ 1.0:0.1.
Good effect of the present invention is:
(1) the present invention adopts the bismaleimides of cyanamide and the modification of trimerization of nitriles ammonia to synthesize the lithium ion battery of special molecular structure or the additive of lithium macromolecule battery anode sizing agent, its battery that is prepared into is passed through lancing test, increase the stability of positive electrode active materials, and promoted the cycle life of battery;
(2) because additive contains the bismaleimides of cyanamide and the modification of trimerization of nitriles ammonia, so that it can cover surface of positive electrode active material, thereby avoid and suppressed electrolyte directly and the caused positive electrode active materials structural instability of positive electrode active materials generation surface action, so just promoted the cycle life of battery;
(3) additive therefor of the present invention has formed diaphragm at surface of positive electrode active material; can when internal short-circuit, stop the positive electrode active materials cracking; so that battery is safer, the safety protective film because forming at surface of positive electrode active material has simultaneously promoted useful life of lithium battery.
Embodiment
Describe technical scheme of the present invention in detail below in conjunction with embodiment, but protection range is not so limited.
The preparation of the Maleimide additive of embodiment 1 cyanamide modification
With 0.1mol melamine and 0.02mol cyanamide as initator, 340 mL NMP are solvent, to 0.2mol N, N '-4,4 '-diphenyl methane-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LiCoO
2, the KS6 of 120 g, the PVDF of 60 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 11.4g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
The preparation of the Maleimide additive of embodiment 2 cyanamide modifications
With 0.1mol melamine and 0.02mol cyanamide as initator, 340mL NMP is solvent, to 0.2mol reactant N, N '-4,4 '-diphenyl ether-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LiCoO
2, the KS6 of 120 g, the PVDF of 60 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 11.4g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
The preparation of the Maleimide additive of embodiment 3 cyanamide modifications
With 0.1mol melamine and 0.02mol cyanamide as initator, 270mLNMP is solvent, to 0.2mol reactant N, N '-4,4 '-phenyl-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LiMnO
2, the CGCF of 120 g, the PVDF of 60 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 11.0g and mix, then add to mix and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
The preparation of the Maleimide additive of embodiment 4 cyanamide modifications
With 0.1mol melamine and 0.02mol cyanamide as initator, 282mLNMP is solvent, to 0.2mol reactant N, N '-4,4 '-dimethyl-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LNCM, the SP of 120 g, the PVDF of 60 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 2.9 g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
The preparation of the Maleimide additive of embodiment 5 cyanamide modifications
With 0.1mol melamine and 0.02mol cyanamide as initator, 340 mL NMP are solvent, to 0.2mol N, N '-4,4 '-diphenyl methane-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LiCoO
2, the KS6 of 120 g, the PVDF of 364 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 120g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
The preparation of the Maleimide additive of embodiment 6 cyanamide modifications
With 0.1mol melamine and 0.02mol cyanamide as initator, 340mL NMP is solvent, to 0.2mol reactant N, N '-4,4 '-diphenyl ether-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g NCA, the VGCF of 2.5 g, the PVDF of 2.5g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 10g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
Wherein, the preparation process of standard positive electrode plate is described in the embodiment 1 ~ 6:
(1) utilize coating machine with the coating speed of 1 meter/min the gained anode sizing agent, it is 180 microns slurry wet film at the copper foil surface coating thickness of 15 micron thickness, the slurry wet film respectively through the oven drying 30min of 100 ℃ and 130 ℃, is obtained thickness and is 120 microns dry film;
(2) on another surface of above-mentioned dry film, adopt the dry film of 120 microns of same step coating same thickness;
(3) utilize roller to roll to be coated with the aluminium foil of slurry, the rate of rolling is 0.7, obtains negative anode plate.
The preparation process of described standard negative pole plate is:
(1) with MCMB, the 10gVGCF of 930g, 60gPVDF, 750gNMP mixes, and then adds to pour out mixture after the zirconium pearl mixes 2.5h, filters the zirconium pearl, gets cathode size;
(2) utilize coating machine with the coating speed of 1 meter/min the gained cathode size, it is 180 microns slurry wet film at the copper foil surface coating thickness of 10 micron thickness, the slurry wet film respectively through the oven drying 30min of 100 ℃ and 130 ℃, is obtained thickness and is 120 microns dry film;
(3) on another surface of above-mentioned dry film, adopt the dry film of 120 microns of same step coating same thickness;
(4) utilize roller to roll to be coated with the aluminium foil of slurry, the rate of rolling is 0.7, obtains negative plates.
In order to confirm technique effect of the present invention, the properties of the lithium ion battery described in the present invention is measured, the result is as follows:
Embodiment battery end properties and related data
。
(wherein, remaining 1 is under the normal temperature, the discharge residual volume of 500 circulations of 1C/1C, and remaining 2 is under 55 ℃, the discharge residual volume of 500 circulations of 1C/1C.Condition of Acupuncture: 2.5mm O.D; Speed 1mm/s).
Simultaneously, the present invention is directed to embodiment 1 and embodiment 2 does and has carried out the contrast experiment:
Comparative Examples 1:
Only with the 0.1mol melamine as initator, 340 mL NMP are solvent, to 0.2mol N, N '-4,4 '-diphenyl methane-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LiCoO
2, the KS6 of 120 g, the PVDF of 60 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 11.4g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
Comparative Examples 2:
With the 0.1mol melamine as initator, 340mL NMP is solvent, to 0.2mol reactant N, N '-4,4 '-diphenyl ether-bismaleimides is carried out modification, above-mentioned substance obtains the modified maleimide that contains cyanamide take NMP as solvent at 130 ℃ of lower reaction 3h, is used as the additive of electrode material of lithium battery constituent prescription.
With 1820g LiCoO
2, the KS6 of 120 g, the PVDF of 60 g and 850gNMP mix to get anode sizing agent.Then add the above-mentioned additive of 11.4g and mix, then add and pour out mixture after the zirconium pearl mixes 2.5h, filter the zirconium pearl, obtain anode sizing agent.
The preparation method prepares positive plate by the standard lithium ion battery positive plate, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
Comparative Examples 3:
The preparation method prepares positive plate by the standard lithium ion anode, collocation standard negative pole plate, load onto the standard cell core that is of a size of 5mm (height) * 59mm (length) * 37mm (wide), pour into above-mentioned liquid standard electrolytic liquid 4.2g, get lithium ion battery after the encapsulation.
In the Comparative Examples, battery end properties related data is:
Claims (15)
1. lithium battery maleimide additive is characterized in that: described additive refers to contain the modified maleimide that cyanamide and melamine are modified.
2. a kind of lithium battery maleimide additive according to claim 1, it is characterized in that: described additive can be applicable to the anode formula composition material of lithium ion battery or lithium macromolecule battery.
3. described lithium battery anode prescription that contains the modified maleimide additive of claim 2, it is characterized in that: described prescription contains the material of following percentage by weight:
(ⅰ) 0.1 ~ 5% by cyanamide and cyanurotriamide modified bismaleimides or/and single maleimide reaction products therefrom;
(ⅱ) 0.1 ~ 15% Kynoar, acrylic resin and butadiene-styrene rubber;
(ⅲ) positive active material;
(ⅳ) 0.1 ~ 5% conductive additive: such as KS6 or CGCF or SP or VGCF.
4. anode formula material according to claim 3, it is characterized in that: described positive active material is: LiCoO
2Or LiMnO
2Or LiFePO
4Or LNCM or NCA, or its mixture.
5. anode formula material according to claim 3, it is characterized in that: described bismaleimide structure is:
Wherein, m, n, o are 1,2,3,4,5
Or
Wherein, R can be a kind of in the following group :-(CH
2)
2-,-(CH
2)
6-,-(CH
2)
8-,-(CH
2)
12-,
,
,
,
,
,
6. anode formula material according to claim 3 is characterized in that: described single maleimide can be a kind of in the following material:
(1) phenyl maleimide
(2). N-(to methylbenzene) maleimide
(3). N-(o-methyl-benzene) maleimide
(4). N-(methylbenzene) maleimide
(5). the N-CYCLOHEXANE maleimide
(6). maleimide
(7). dimaleoyl imino phenol
(8). the dimaleoyl imino benzocyclobutene
(9). phosphorous maleimide
(10). phosphatic maleimide
(11). the maleimide of silicone-containing
(12). N-(4-THP trtrahydropyranyl-hydroxyphenyl) maleimide
(13). 2,6-benzhydryl-maleimide.
7. anode formula material according to claim 3 is characterized in that: described melamine or derivatives thereof, and its structure can be:
Wherein, H can be by R
1, R
2, R
3, R
4, R
5, R
6Replace.Wherein, R
1, R
2, R
3, R
4, R
5, R
6Can be linearity or branched alkyl.
8. anode formula material according to claim 3, it is characterized in that: described cyanamide is:
Wherein, R
1, R
2Be H or linearity or branched alkyl.
9. anode formula material according to claim 3 is characterized in that: can add reaction initiator in the described anode formula material.
10. anode formula material according to claim 9, it is characterized in that: the reaction initiator in the described anode formula material is peroxide or azodiisobutyronitrile.
11. anode formula material according to claim 3 is characterized in that: conductive additive can carry out surface treatment (ⅳ).
12. anode formula material according to claim 11 is characterized in that: the surface treatment of conductive additive can be used following coupling agent (ⅳ):
(1) with the oxosilane coupling agent of vinyl-functional;
(2) unsaturated linear chain hydrocarbon carboxylic acids, its structural formula is:
CH
3(CH
2)
nCH=CH (CH
2)
nCOOH; N is 1 ~ 14 integer.
13. anode formula material according to claim 11 is characterized in that: unsaturated linear chain hydrocarbon carboxylic acids is oleic acid.
14. anode formula material according to claim 3 is characterized in that: the mol ratio of bismaleimides (ⅰ) or single maleimide and melamine or derivatives thereof is 25:1 ~ 1:1.
15. anode formula material according to claim 3 is characterized in that: the mol ratio of the or derivatives thereof of melamine (ⅰ) and amino nitrile is 1.0:1.0 ~ 1.0:0.1.
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| CN105304934A (en) * | 2015-11-02 | 2016-02-03 | 中国第一汽车股份有限公司 | Positive electrode modified high-safety lithium ion battery |
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| EP3211706A4 (en) * | 2014-10-22 | 2018-07-04 | Mitsui Chemicals, Inc. | Lithium secondary battery |
| CN105304934A (en) * | 2015-11-02 | 2016-02-03 | 中国第一汽车股份有限公司 | Positive electrode modified high-safety lithium ion battery |
| CN105244551B (en) * | 2015-11-02 | 2017-11-21 | 中国第一汽车股份有限公司 | Negative pole is modified high security lithium ion battery |
| CN105304934B (en) * | 2015-11-02 | 2017-11-21 | 中国第一汽车股份有限公司 | Positive pole is modified high security lithium ion battery |
| CN105390737A (en) * | 2015-11-02 | 2016-03-09 | 中国第一汽车股份有限公司 | Lithium ion battery with thermodynamic protection effect |
| CN105244551A (en) * | 2015-11-02 | 2016-01-13 | 中国第一汽车股份有限公司 | Cathode modified high security lithium ion battery |
| CN105742706A (en) * | 2016-04-01 | 2016-07-06 | 朱政 | Positive electrode additive of lithium battery |
| CN105742706B (en) * | 2016-04-01 | 2018-06-29 | 朱政 | A kind of lithium battery anode additive |
| WO2019000861A1 (en) * | 2017-06-30 | 2019-01-03 | 福建猛狮新能源科技有限公司 | Lithium-ion battery positive electrode and preparation method therefor and method for preparing lithium-ion battery |
| CN109988330A (en) * | 2018-10-18 | 2019-07-09 | 国联汽车动力电池研究院有限责任公司 | One kind coating modified diaphragm resistant to high temperature and the preparation method and application thereof |
| CN109988330B (en) * | 2018-10-18 | 2021-10-26 | 国联汽车动力电池研究院有限责任公司 | High-temperature-resistant coating modified diaphragm and preparation method and application thereof |
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| CN103050706B (en) | 2015-06-17 |
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