CN103346328A - High-potential-resistant window lithium-ion secondary battery binder and preparation method thereof - Google Patents
High-potential-resistant window lithium-ion secondary battery binder and preparation method thereof Download PDFInfo
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- CN103346328A CN103346328A CN2013102993391A CN201310299339A CN103346328A CN 103346328 A CN103346328 A CN 103346328A CN 2013102993391 A CN2013102993391 A CN 2013102993391A CN 201310299339 A CN201310299339 A CN 201310299339A CN 103346328 A CN103346328 A CN 103346328A
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- adhesive
- lithium
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- polymerization
- positive plate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a high-potential-resistant window lithium-ion secondary battery binder and a preparation method thereof. The fluorine-containing acrylate, butadiene, styrene and acrylate are used as a polymerization starting monomer, the polymerization of free radicals is carried out under the initiation condition of the peroxysulphate heat free radical initiator, and the uniform and stable emulsion binder is prepared. By utilizing the electrode binder, the advantages such as high mechanical and chemical stability and high electrochemical stable window value resistance can be realized. The binder is applicable to the high-power density and high-energy density lithium-ion secondary battery and particularly applicable to the high-potential window positive materials such as LiNi0.5Mn1.504 which is developed at present. Compared with the traditional polyvinylidene fluoride and styrene-butadiene latex binder, the binder also has the advantages of environmental protection and moderate cost.
Description
Technical field
The present invention relates to a kind of window of anti-high potential lithium rechargeable battery adhesive and preparation method thereof.
Background technology
Lithium rechargeable battery is with its height ratio capacity, high voltage, and volume is little, and is in light weight, advantages such as memoryless property, recent two decades has obtained huge development.Battery is mainly by positive pole, negative pole, compositions such as barrier film and organic electrolyte; Positive and negative electrode is generally by the powdery electroactive material, as lithium metal oxide, the carbon element negative material, adhesive, conductive agent and collector body are formed, the preparation method is active material, conductive agent, binder solution etc. mix and grind to distributed slurry, coat on the collector electrodes such as Copper Foil or aluminium foil, drying technology such as rolls and is prepared from.The operable adhesive of the adhesive of electrode material of secondary lithium ion battery such as ethylene-propylene rubber, fluorine-containing polyolefin etc.Generally adopt expensive fluorinated polymer as the adhesive of cell positive material at present, as Kynoar (PVDF) etc. (as Japanese patent laid-open 7-220722,7-78056 and 7-78057), and with organic solvent N-methyl pyrrolidone (NMP) as dispersant, be aided with a small amount of conductive agent, obtain the anode sizing agent of organic system.The anodal oar material coating smoothness of organic system is low, and the difficult oven dry of pole piece had not only increased cost but also the contaminated environment made.
In order to address the above problem, people have also developed the lithium rechargeable battery aqueous binder, as acrylic acid-styrene polymer, and acrylic acid-silicon-oxygen polymer, cinnamic acrylic ester polymer (JP2000294230); Styrene-butadiene polymer (JP2000106198); Butadiene-acrylonitrile polymer waterborne polymeric latex such as (EP100905), this base polymer viscosity is too low to contain more surfactant simultaneously, and processing and the battery performance of battery pole piece produced adverse influence.CN1328104A and CN1328102A etc. disclose acrylic acid, and acrylate, monomer copolymerizations such as acrylamide and acrylonitrile obtain the aqueous binder that the mode of emulsifier-free emulsion polymerization obtains having good adhesion.Along with the progress of lithium rechargeable battery material technology, power lithium-ion rechargeable battery need have higher energy density and power density, thereby need develop the positive electrode of high potential window more or the positive electrode of height ratio capacity more.The LiNiPO of the positive electrode of high potential window such as olivine-type wherein
4(5.1V), LiCoPO
4(4.8V), and spinel-type LiNi
0.5Mn
1.5O
4(4.8V) and LiCoMnO
4(5.1V), the positive electrode of these high potential windows need have the corresponding window of anti-high potential electrolyte and adhesive to mate.Above-described aqueous binder material also mainly is applicable at present traditional cobalt acid lithium, bonding and the coating of positive electrode such as LiMn2O4 and LiFePO4, the performance of its anti-high potential does not also reach the requirement of 5V, thereby needs to adopt the macromolecular material exploitation of the window of anti-the high potential to prepare the window of anti-high potential the and the moderate high performance adhesive of cost.
Fluorine is the element of the electronegativity maximum known to up to now, its atom covalence radius (0. 064nm) is only big slightly than hydrogen atom, so after the hydrogen on the hydrocarbon key (C-H) was replaced by fluorine, the bond energy of the carbon-fluorine bond (C-F) that fluorine atom and carbon atom form had increased by 63 kJ/mol.Fluorinated acrylate polymer is to introduce fluoro-containing group at the side chain of original copolymer; because fluorine side chain orientation outwardly; main chain and interior molecules are formed shielding and protection; the electron cloud of fluorine atom shields carbon carbon major key well; guaranteed the stability of carbon-carbon bond; make the stable performance of acrylate containing fluorine polymer physics, durability and chemical proof are good, and especially electrochemical stability window improves.So the present invention under the suitable proportioning condition, is prepared into excellent performance to fluorine-containing acrylate monomer and traditional monomer by modification by copolymerization, the battery adhesive that cost is moderate is to satisfy lithium rechargeable battery technology requirement of future generation.
The purpose of this invention is to provide a kind of window of anti-high potential lithium ion secondary battery anode material adhesive.Another object of the present invention provides a kind of preparation method of the window of anti-high potential lithium ion secondary battery anode material adhesive.
Summary of the invention
The present invention has introduced a kind of window of anti-high potential lithium rechargeable battery adhesive and preparation method thereof.Use electrode adhesive of the present invention, have machinery and chemical stability height, the advantage that anti-electrochemical stability window is high is applicable to high power density and high energy density lithium ion secondary battery, is particularly useful for high potential window positive electrode such as the LiNi of exploitation recently
0.5Mn
1.5O
4Deng.
A kind of window of anti-high potential lithium rechargeable battery adhesive and preparation method thereof, it is characterized in that adopting fluorinated acrylate, butadiene, styrene and acrylates are the polymerization initial monomers, under the condition that the persulfate thermal free radical initiator causes, carry out radical polymerization, make uniform and stable emulsion form adhesive; Wherein above-mentioned fluorinated acrylate is selected from acrylic acid hexafluoro butyl ester, methacrylic acid hexafluoro butyl ester, acrylic acid five fluorine ethyl esters, methacrylic acid five fluorine ethyl esters, dodecafluorhe-ptylacrylate, methacrylic acid ten difluoro heptyl esters, a kind of among perfluoro hexyl ethyl propylene acid esters or the perfluorobutyl ethylene; Above-mentioned fluorinated acrylate wherein, butadiene, the consumption of styrene and acrylates polymerization single polymerization monomer is 30 ~ 60:20 ~ 35:15 ~ 25:5 ~ 10; Above-mentioned fluorinated acrylate wherein, butadiene, the total amount of styrene and acrylates polymerization single polymerization monomer is the 10-50% of adhesive total amount; Wherein the persulfate thermal free radical initiator that adopts among the above-mentioned preparation method is ammonium persulfate, a kind of in potassium peroxydisulfate and the hydrogen peroxide; Wherein the persulfate thermal free radical initiator consumption that adopts among the above-mentioned preparation method is 0.1-2% of amount of monomer.
The positive plate that above-mentioned battery adhesive is made is characterized in that being applied to LiCoO
2, LiMnO
2And LiFePO
4In the positive plate made of one or both grades.
The positive plate that above-mentioned battery adhesive is made is characterized in that being applied to positive electrode such as the LiNiPO of high potential window
4, LiCoPO
4, LiNi
0.5Mn
1.5O
4And LiCoMnO
4In the positive plate made of one or both grades.
The lithium rechargeable battery of above-mentioned battery adhesive and the assembling of the positive plate of making thereof is characterized in that adopting above-mentioned high potential window positive electrode as positive plate, and again with cathode of lithium, graphite or carbonaceous mesophase spherules are the battery of the high potential of negative plate assembling.
Electrode material adhesive of the present invention, its stable electrochemical property window be with the method for this area routine, namely three electrode method (stainless steel is work electrode, the lithium sheet be reference and to electrode) test investigation.Wherein electrolyte adopts the perfluorocarbon acid vinyl acetate, and lithium salts is polymerization boric acid lithium salts.
Electrode material adhesive of the present invention, its battery performance and application with the method for this area routine, namely are assembled into button cell (2032 type) and carry out the charge-discharge test investigation.Preparation and test process are as follows:
At first with 5.70 gram positive active material LiNi
0.5Mn
1.5O
4, 0.30 gram conductive agent acetylene black mixes, and then adds 6.30 gram mass marks again and be 5% binder solution, stirs the uniform anodal slip of formation.This slip is coated on the aluminium foil uniformly, 120 ℃ of oven dry down then, it is 12 millimeters that roll-in, punching make radius, thickness is 80 microns circular positive plate, wherein contains 17.6 milligrams of active component LiNi
0.5Mn
1.5O
4After vacuumize under the temperature of 120 degree, place the glove box of dry argon gas atmosphere, dress up Li/LiNi with the metal lithium electrode matched group respectively
0.5Mn
1.5O
4Button cell, electrolyte adopt polymerization lithium borate gel-type electrolyte, and battery charging and discharging is constant flow method, and charge condition is: 0.3-1.1mA/cm
2Discharging current is 0.5-1.1mA/cm
2Be the Li/Li of 2.50-5.20V(by voltage range
+); Discharging and recharging instrument by the LAND of computer control tests.
Description of drawings
The electrochemical stability window resolution chart of composite adhesives among accompanying drawing 1 embodiment 1.
Embodiment
Be embodiments of the invention below.
In stainless steel reactor, add 30 parts of methacrylic acid hexafluoro butyl esters, 13 parts of butadiene, 12 parts of styrene, 5 parts acrylic acid lithium and 240 parts of distilled water, be to be warmed up to 75 ° of C gradually under 150 rev/mins the mixing speed at rotating speed, add 0.9 part of ammonium persulfate initiator initiation reaction then, afterreaction was finished in 3 hours, made solids content and be 20% lithium ion secondary battery anode material adhesive.
In stainless steel reactor, add 30 parts of perfluoro hexyl ethyl propylene acid esters, 15 parts of butadiene, 10 parts of styrene, 5 parts acrylic acid lithium and 240 parts of distilled water, be to be warmed up to 75 ° of C gradually under 150 rev/mins the mixing speed at rotating speed, add 0.9 part of ammonium persulfate initiator initiation reaction then, afterreaction was finished in 3 hours, made solids content and be 20% lithium ion secondary battery anode material adhesive.
In stainless steel reactor, add 25 parts of methacrylic acid ten difluoro heptyl esters, 20 parts of butadiene, 10 parts of styrene, 5 parts acrylic acid lithium and 240 parts of distilled water, be to be warmed up to 75 ° of C gradually under 150 rev/mins the mixing speed at rotating speed, add the initiation reaction of 0.9 part of potassium peroxydisulfate initator then, afterreaction was finished in 3 hours, made solids content and be 20% lithium ion secondary battery anode material adhesive.
In stainless steel reactor, add 25 parts of methacrylic acid ten difluoro heptyl esters, 20 parts of butadiene, 10 parts of styrene, 5 parts acrylic acid lithium and 240 parts of distilled water, be to be warmed up to 75 ° of C gradually under 150 rev/mins the mixing speed at rotating speed, add the initiation reaction of 0.9 part of potassium peroxydisulfate initator then, afterreaction was finished in 3 hours, made solids content and be 20% lithium ion secondary battery anode material adhesive.
The application of adhesive of the present invention in the high temperature modification lithium rechargeable battery.
At first with 5.70 gram positive active material LiNi
0.5Mn
1.5O
4, 0.30 gram conductive agent acetylene black mixes, and then adds 6.30 gram mass marks again and be 5% binder solution, stirs the uniform anodal slip of formation.This slip is coated on the aluminium foil uniformly, 120 ℃ of oven dry down then, it is 12 millimeters that roll-in, punching make radius, thickness is 80 microns circular positive plate, wherein contains 17.6 milligrams of active component LiNi
0.5Mn
1.5O
4After vacuumize under the temperature of 120 degree, place the glove box of dry argon gas atmosphere, dress up Li/LiNi with the metal lithium electrode matched group respectively
0.5Mn
1.5O
4Button cell, electrolyte adopt polymerization lithium borate gel-type electrolyte, and battery charging and discharging is constant flow method, and charge condition is 0.5C, observe discharge capacity of the cell and still remain on more than 90% after 50 circulations.
Claims (4)
1. the window of anti-high potential lithium rechargeable battery adhesive and preparation method thereof, it is characterized in that adopting fluorinated acrylate, butadiene, styrene and acrylates are the polymerization initial monomers, under the condition that the persulfate thermal free radical initiator causes, carry out radical polymerization, make uniform and stable emulsion form adhesive;
Wherein above-mentioned fluorinated acrylate is selected from acrylic acid hexafluoro butyl ester, methacrylic acid hexafluoro butyl ester, acrylic acid five fluorine ethyl esters, methacrylic acid five fluorine ethyl esters, dodecafluorhe-ptylacrylate, methacrylic acid ten difluoro heptyl esters, a kind of among perfluoro hexyl ethyl propylene acid esters or the perfluorobutyl ethylene;
Above-mentioned fluorinated acrylate wherein, butadiene, the consumption of styrene and acrylates polymerization single polymerization monomer is 30 ~ 60:20 ~ 35:15 ~ 25:5 ~ 10;
Above-mentioned fluorinated acrylate wherein, butadiene, the total amount of styrene and acrylates polymerization single polymerization monomer is the 10-50% of adhesive total amount;
Wherein the persulfate thermal free radical initiator that adopts among the above-mentioned preparation method is ammonium persulfate, a kind of in potassium peroxydisulfate and the hydrogen peroxide;
Wherein the persulfate thermal free radical initiator consumption that adopts among the above-mentioned preparation method is 0.1-2% of amount of monomer.
2. the positive plate of the described battery adhesive making of claim 1 is characterized in that being applied to LiCoO
2, LiMnO
2And LiFePO
4In the positive plate made of one or both grades.
3. the positive plate made of the described battery adhesive of claim 1 is characterized in that being applied to positive electrode such as the LiNiPO of high voltage window
4, LiCoPO
4, LiNi
0.5Mn
1.5O
4And LiCoMnO
4In the positive plate made of one or both grades.
4. the lithium rechargeable battery of the positive plate described in the claim 2 or 3 assembling is characterized in that the positive plate that adopts the described adhesive of claim 1 to make adopting cathode of lithium, and graphite or carbonaceous mesophase spherules are the battery of negative plate assembling.
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|---|---|---|---|
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|---|---|---|---|
| CN2013102993391A CN103346328A (en) | 2013-07-16 | 2013-07-16 | High-potential-resistant window lithium-ion secondary battery binder and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905475A (en) * | 2017-03-10 | 2017-06-30 | 湖南高瑞电源材料有限公司 | The ceramic diaphragm that a kind of lithium battery ceramic diaphragm is prepared with the preparation method of fluorine-containing adhesive and using the adhesive |
| CN109768280A (en) * | 2018-12-20 | 2019-05-17 | 中国科学院青岛生物能源与过程研究所 | A kind of lithium battery anode with free radical capture function |
| CN112321761A (en) * | 2020-11-04 | 2021-02-05 | 深圳港池科技有限公司 | Preparation method of adhesive for lithium ion battery |
| CN112467142A (en) * | 2020-11-25 | 2021-03-09 | 湖南高瑞电源材料有限公司 | Aqueous solution type lithium iron phosphate anode adhesive, preparation method and application thereof |
| CN114597367A (en) * | 2022-03-14 | 2022-06-07 | 广西卓能新能源科技有限公司 | Preparation and use methods of lithium ion battery anode material and multi-element hydrosol |
| CN116536003A (en) * | 2023-07-06 | 2023-08-04 | 深圳海辰储能控制技术有限公司 | Adhesive and preparation method thereof, pole piece, battery and power utilization device |
| WO2023240681A1 (en) * | 2022-06-15 | 2023-12-21 | 天津力神电池股份有限公司 | Mass transfer acceleration and expansion reduction material for negative electrode and use |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106905475A (en) * | 2017-03-10 | 2017-06-30 | 湖南高瑞电源材料有限公司 | The ceramic diaphragm that a kind of lithium battery ceramic diaphragm is prepared with the preparation method of fluorine-containing adhesive and using the adhesive |
| CN106905475B (en) * | 2017-03-10 | 2020-09-25 | 湖南高瑞电源材料有限公司 | Preparation method of fluorine-containing adhesive for lithium battery ceramic diaphragm and ceramic diaphragm prepared by using adhesive |
| CN109768280A (en) * | 2018-12-20 | 2019-05-17 | 中国科学院青岛生物能源与过程研究所 | A kind of lithium battery anode with free radical capture function |
| CN112321761A (en) * | 2020-11-04 | 2021-02-05 | 深圳港池科技有限公司 | Preparation method of adhesive for lithium ion battery |
| CN112467142A (en) * | 2020-11-25 | 2021-03-09 | 湖南高瑞电源材料有限公司 | Aqueous solution type lithium iron phosphate anode adhesive, preparation method and application thereof |
| CN114597367A (en) * | 2022-03-14 | 2022-06-07 | 广西卓能新能源科技有限公司 | Preparation and use methods of lithium ion battery anode material and multi-element hydrosol |
| WO2023240681A1 (en) * | 2022-06-15 | 2023-12-21 | 天津力神电池股份有限公司 | Mass transfer acceleration and expansion reduction material for negative electrode and use |
| CN116536003A (en) * | 2023-07-06 | 2023-08-04 | 深圳海辰储能控制技术有限公司 | Adhesive and preparation method thereof, pole piece, battery and power utilization device |
| CN116536003B (en) * | 2023-07-06 | 2023-09-19 | 深圳海辰储能控制技术有限公司 | Adhesive and preparation method thereof, pole piece, battery and power utilization device |
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Application publication date: 20131009 |