CN104752729B - The preparation method of the water-based compound binding agent of lithium ion battery with electronics and ionic conductivity general character - Google Patents

The preparation method of the water-based compound binding agent of lithium ion battery with electronics and ionic conductivity general character Download PDF

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CN104752729B
CN104752729B CN201510102142.3A CN201510102142A CN104752729B CN 104752729 B CN104752729 B CN 104752729B CN 201510102142 A CN201510102142 A CN 201510102142A CN 104752729 B CN104752729 B CN 104752729B
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binding agent
water
ion battery
lithium
agent
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CN104752729A (en
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李国富
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Teng Longyuan Industrial Co Ltd Of Shenzhen
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H01M4/622—Binders being polymers
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses a kind of preparation method of the water-based compound binding agent of lithium ion battery with electronics and ionic conductivity general character, it is blended by flexibility agent, ionic binding agent, water-soluble polymer and is formed polymeric matrix, its ionic binding agent provides lithium source, and polymeric matrix can be with conducting lithium ions；Conductive agent is dispersed in polymeric matrix and forms conductive polymer composites, filler forms conductive network in polymerization system.Water-based compound binding agent prepared by the present invention is both electronic conductor, and ion conductor, can be effectively increased the content of lithium ion in positive plate, improves the cyclical stability of battery.

Description

The water-based compound binding agent of lithium ion battery with electronics and ionic conductivity general character Preparation method
Technical field
The present invention relates to materials chemistry and new energy field, and in particular to a kind of preparation method of water-based compound binding agent and It is applied to using water-based compound binding agent made from this method in the preparation of based lithium-ion battery positive plate.
Background technology
Lithium ion battery, as the first march of contemporary battery industry, the main charging applied in portable type electronic product Battery, electric tool and electric automobile etc..Domestic and external electric automobile market constantly expands, the demand of lithium ion battery Amount also will constantly increase.Preparing lithium ion battery needs auxiliary material binding agent, it be also influence battery form and its it is comprehensive An important factor for energy.
The charge and discharge process of lithium ion battery is the cyclic process that lithium ion and electronics participate in jointly, to ensure larger fill Discharge current and cycle life, the electrode material for just necessarily requiring lithium ion battery are the good mixed conductors of ion and electronics. But commercialized positive and negative pole material is generally all semi-conducting material, its intrinsic electronic conductivity is all 10-1-10-9S/cm, electricity Conductive performance of the son between active material particle is poor, depend merely on the electric conductivity of active material in itself be it is far from being enough, lithium from Son conduction relies on binding agent and active material junction.
In the industrial production, anode material for lithium-ion batteries is generally using Kynoar PVDF as binding agent, still Its electronics and ionic conductivity are poor, be unfavorable for lithium ion inside pole piece and interface migration, increase battery polarization and internal resistance, lead The problems such as poor circulation, capacity are rapidly decayed in the case of cause high rate charge-discharge；It is and organic molten used in dissolving PVDF Agent such as N-methyl pyrrolidones NMP is harmful to environment and human body, and expensive, in order to reduce the harm to environment, reclaims NMP Further increase the manufacturing cost of lithium ion battery.Aqueous binders use water as solvent, not only cheap, Er Qiewu Pollution.
When preparing graphite cathode piece, CMC (sodium carboxymethylcellulose) and SBR (butadiene-styrene rubber) glue are industrially used The water-based compound binding agent system that both breasts are combined, this kind of binding agent are that point contacts with active material, and faying face is small, manufacture Lack long-range connection between electrode particle, be unfavorable for the conduction of ion and electronics.
In the prior art, someone using water-based compound system as lithium ion battery electrode material binding agent.Example Such as, Chinese patent application CN200410050866.X disclose be made up of polytetrafluoroethylene (PTFE) (PTFE) and cellulose ethers it is water-based Composite adhesive system prepares anode sizing agent, lithium battery and its preparation method.But this kind of compound system and active material are a little Contact, faying face is small, and long-range connection is lacked between the electrode particle of manufacture, is unfavorable for the conduction of ion and electronics, causes what is prepared Anode sizing agent is coated on aluminium foil, and after drying, cathode film fully can not be attached in aluminum foil current collector, especially one side aluminium Paper tinsel, binder system are inadequate to the adhesive force of collector；And the battery polarization prepared is big, electrical property is bad, can not be applied to In industry.
The content of the invention
It is an object of the invention to provide a kind of lithium ion battery with electronics and ionic conductivity general character with water-based compound The preparation method of binding agent, conductive agent is filled into polymeric matrix and forms composite conducting material, applied to lithium ion battery In electrode material, make it that both there is ionic conductivity, there is electron conduction again, reduce battery polarization and internal resistance, avoid battery The problems such as poor circulation, capacity are decayed rapidly under charge status；The present invention is cheap using water as solvent, avoids Harm of the organic solvent to environment.
A kind of lithium ion battery electrode material preparation method of water-based compound binding agent, comprises the following steps：
(1) flexibility agent is dissolved in the water；
(2) toward adding water-soluble polymer in above-mentioned solution, stirring is to dissolving；
(3) ionic binding agent and then into the solution of step (2) is added, stirs to being completely dissolved, obtains polymer matrix Body；
(4) conductive agent is added into above-mentioned polymeric matrix, be uniformly dispersed.
Wherein it is preferred to flexibility agent is partially hydrolyzed polyacrylamide (PHPA)；Water-soluble polymer is polyvinyl alcohol；Ionic Binding agent is carboxymethyl cellulose lithium；Conductive agent is in carbon system filler such as acetylene black, graphite, graphene, carbon black, CNT Any one or a few.
Preferably, relative to obtained positive plate, without solvent, the percentage by weight of the water-soluble polymer is 1%~10%, the percentage by weight of ionic binding agent is 1%~5%, the percentage by weight of flexibility agent for 0.01%~ 0.5%, the percentage by weight of conductive agent is 1%~12%.
It may further be preferable that the percentage by weight of water-soluble polymer is 2%~7%.
It may further be preferable that the percentage by weight of ionic binding agent is 1%~3.5%.
It may further be preferable that the percentage by weight of flexibility agent is 0.01%~0.3%.
It may further be preferable that the percentage by weight of conductive agent is 2%~10%.
In above-mentioned preparation method, preferred partially hydrolyzed polyacrylamide (PHPA) is prepared by such method in step (1)：Will Polyacrylamide is soluble in water, adds lithium hydroxide, is heated to 40~90 DEG C, stirs 2~8h, is cooled to room temperature, adds organic Solvent such as ethanol is stood to there is solid precipitation, is filtered, and is washed, drying, and drying temperature is 50~80 DEG C.
Preferably polyvinyl alcohol is dissolved in solution using such preparation method in step (2), solution is heated to 50 ~80 DEG C, polyvinyl alcohol is added while stirring, is then stirred to polyvinyl alcohol and is all dissolved, stops heating, be cooled under stirring Room temperature, it is eventually adding ionic binding agent.
Preparation method as the use of preferably carboxymethyl cellulose lithium, sodium carboxymethylcellulose is scattered in step (3) In ethanol, acid adding (hydrochloric acid or sulfuric acid) dissolves under stirring, insoluble matter precipitation to be had, and adds 90% ethanol, precipitates, filters, washes Wash, dry carboxymethyl cellulose；Carboxymethyl cellulose is scattered in ethanol, lithium hydroxide solution is added, stirs to carboxylic first Base cellulose all dissolves, and adds 90% ethanol, precipitation, filtering, washing, dry carboxymethyl cellulose lithium.
The preparation flow of water-based compoiste adhering agent solution：Partially hydrolyzed polyacrylamide (PHPA) is soluble in water, stirring to dissolving, Solution is heated to 50~80 DEG C, adds polyvinyl alcohol while stirring, then stirs to polyvinyl alcohol and all dissolves, stops adding Heat, room temperature is cooled under stirring, is eventually adding ionic binding agent, stirring to dissolving.
Water-based compound binding agent produced by the present invention can be applied in the preparation of based lithium-ion battery positive plate and contain this In the preparation of the lithium ion battery of positive plate.
Brief description
Fig. 1 is the LiAl that PVDF is prepared with water-based compound binding agent0.04Mn1.96O4The specific capacity of battery and the relation of voltage；
Fig. 2 is the LiFePO that PVDF is prepared with water-based compound binding agent4The specific capacity of battery and the relation of voltage；
Fig. 3 is the LiFePO that PVDF is prepared with water-based compound binding agent4AC impedance after circulating battery.
Embodiment
Below by embodiment and with reference to accompanying drawing, the present invention is described in further detail.Using existing skill Art, using positive plate made of the water-based compound binding agent of the present invention, and battery is further assembled into, passes through the painting to positive plate Chemical property of cloth performance and battery etc. carries out test investigation, to illustrate the application effect of the present invention.
Material source：Unless otherwise instructed, all material is by commercially available.
The water-based compound binding agent of the present invention is prepared by following methods：
(1) flexibility agent is dissolved in the water；
(2) toward adding water-soluble polymer in above-mentioned solution, heating stirring is to dissolving；
(3) ionic binding agent and then into the solution of step (2) is added, stirs to being completely dissolved, obtains polymer matrix Body；
(4) conductive agent is added into above-mentioned polymeric matrix, be uniformly dispersed.
It is because one it is preferred that partially hydrolyzed polyacrylamide (PHPA) increases the pliability of pole piece, and non-selected polyacrylamide Lithium source content can then be improved；Second amount of hydrolysis of the polyacrylamide in water is reduced.50~90 DEG C are heated in preparation process In favor of hydrolysis of polyacrylamide, when its content is too low (＜ 0.01%), it is impossible to the effective pliability for improving pole piece；Content mistake When high (＞ 0.5%), after the pole piece of preparation is assembled into battery, battery capacity is not high.It is preferred that polyvinyl alcohol and carboxymethyl cellulose Lithium is used in mixed way, if first, being single use polyvinyl alcohol or carboxymethyl cellulose lithium, the positive plate hardness of preparation is excessive, easily Aliquation；Two be that of avoiding be used alone polyvinyl alcohol viscosity it is too low, be used alone carboxymethyl cellulose lithium viscosity it is too high.Both institutes The percentage composition accounted for is too high, and battery capacity is not high, and the Painting effect of too low anode sizing agent on the current collector is bad.
Below, the implementation result of the present invention is described in detail by specific embodiment.
【Embodiment 1】In agitator, 100 parts of water are added, are placed on magnetic stirring apparatus, add partial hydrolysis polyacrylamide Amine powder, stir to being completely dissolved, be heated to 50~80 DEG C, add polyvinyl alcohol, stirring stops heating to dissolving, to be cooled Carboxymethyl cellulose lithium is added after to room temperature, continues stirring and is all dissolved to it, the water-based compound binding agent of three's composition is 10 Part, relative to water-based compound binding agent, without solvent, the percentage by weight of which part hydrolyzed polyacrylamide is 0.1%, 0.15%th, 0.3%, polyvinyl alcohol：Carboxymethyl cellulose lithium is 20:1、10:1、2:1.10 parts of conductions are added into above-mentioned solution Agent acetylene black, after being sufficiently stirred 1~3h, add active material LiFePO480 parts, it is sufficiently stirred 3~24h.If in pulping process Middle generation bubble, a small amount of ethanol (de-airing mixer industrially may be selected to eliminate bubble) can be added, to the pitch-black light of slurry color and luster Bright, good fluidity, bubble-free, then slurry prepare, can be coated with.
【Embodiment 2】Method and step is same as above, the difference is that binding agent, conductive agent, the ratio of active material three are 8:10: 82。
【Embodiment 3】Method and step is same as above, the difference is that binding agent, conductive agent, the ratio of active material three are 6:10: 84。
【Embodiment 4】Method and step is same as above, the difference is that active material changes LiAl into0.04Mn1.96O4, binding agent, conduction Agent, the ratio of active material three are 8:10:82.
【Embodiment 5】Method and step is same as above, the difference is that compound binding agent is by partially hydrolyzed polyacrylamide (PHPA), polyethylene Alcohol, lithium silicate aqueous solution composition, active material LiFePO4, binding agent, conductive agent, the ratio of active material three are 10: 10:80。
【Embodiment 6】Method and step is same as above, the difference is that compound binding agent is by polyethylene glycol oxide, polyvinyl alcohol, lithium metasilicate The aqueous solution forms, active material LiFePO4, binding agent, conductive agent, the ratio of active material three are 10:10:80.
【Embodiment 7】Method and step is same as above, unlike compound binding agent by polyethylene glycol oxide, polyvinylpyrrolidone, Lithium silicate aqueous solution forms, active material LiFePO4, binding agent, conductive agent, the ratio of active material three are 10:10: 80。
【Embodiment 8】Method and step is same as above, the difference is that compound binding agent is by polyacrylamide, polyethylene glycol, lithium metasilicate The aqueous solution forms, active material LiFePO4, binding agent, conductive agent, the ratio of active material three are 10:10:80.
【Embodiment 9】Method and step is same as above, the difference is that compound binding agent is by polyacrylamide, polyvinyl alcohol, carboxymethyl Cellulose lithium forms, active material LiFePO4, binding agent, conductive agent, the ratio of active material three are 10:10:80.
【Embodiment 10】Method and step is same as above, the difference is that compound binding agent is by polyvinyl alcohol, carboxymethyl chitosan, silicic acid The lithium aqueous solution forms, active material LiFePO4, binding agent, conductive agent, the ratio of active material three are 10:10:80.
(1) preparation of positive plate
With the slurry prepared above, it is coated with scraper, the one side aluminium foil using thickness as 20um is collector, and coating is thick Spend for 400um, positive plate is obtained after naturally dry.
(2) positive plate coating performance is tested
Positive plate after drying respectively according to national standard GB/T9286-1998 and GB/T1731-1993 test its adhesive force and Pliability.
(3) battery assembles
It is above-mentioned dry after positive plate, be cut into a diameter of 14mm sequin, be placed in baking oven 80 DEG C, bake 8h, then very 12h is dried at empty 120 DEG C, weighs, using lithium piece as negative plate, button cell is assembled into glove box, is sealed, is carried out electrical Can test.
(4) battery testing
The battery sealed is placed on LAND indigo plant electrical measurement test systems, 3h is stood, first charges to required voltage, then constant pressure is filled Electric 0.5h, finally with required multiplying power discharging to required voltage.
Comparative example：Respectively with LiFePO4、LiAl0.04Mn1.96O4It is to bond for positive electrode, Kynoar (PVDF) Agent, 1-METHYLPYRROLIDONE (NMP) are that positive plate is made in solvent, and positive plate composition is：80 parts of positive electrode, 10 parts of acetylene black, 100 parts of 10 parts of PVDF, NMP.Battery is made by above-mentioned steps, difference is, when PVDF is dissolved in NMP, need to be heated to 45 DEG C, heat time 3-5h；It is placed directly within baking oven and dries after the completion of slurry coating.
Test shows, LiFePO prepared by water-based compound binding agent4Positive plate film forming is good, pole piece is flawless, positive plate Pliability and adhesive force are qualified；The LiFePO of preparation4The battery that the chemical property of battery is prepared close to PVDF, after circulation Compound system polarization is smaller, and impedance is smaller；The LiAl prepared using water-based compound binding agent system0.04Mn1.96O4The electrification of battery The battery that performance is slightly prepared better than PVDF is learned, specific discharge capacity is respectively after 50 circulations of battery prepared by two kinds of systems 93.1mAh/g, 87.5mAh/g, the capability retention after 50 circulations is respectively 83.9%, 79.5%, water-based compound system table Reveal more preferable cyclical stability.
Test result is shown in Table 1~table 2, Fig. 1~Fig. 3.
LiFePO of each component to preparation in 1 water-based compound binding agent of table4The influence of the coating performance of pole piece
LiFePO of each component percentage composition to preparation in 2 water-based compound binding agent of table4The shadow of the specific discharge capacity of battery Ring
Note 1：The percentage composition of water-based compound binding agent is relative to the quality of positive plate after drying, without solvent；
Note 2：The percentage composition and polyvinyl alcohol of partially hydrolyzed polyacrylamide (PHPA)：Carboxymethyl cellulose lithium is relative to water-based The quality of compound binding agent, without solvent.

Claims (7)

1. a kind of preparation method of the water-based compound binding agent of lithium ion battery with electronics and ionic conductivity general character, including Following steps：
(1) flexibility agent is dissolved in the water；
(2) toward adding water-soluble polymer in above-mentioned solution, stirring is to dissolving；
(3) ionic binding agent and then into the solution of step (2) is added, stirs to being completely dissolved, obtains polymeric matrix；
(4) conductive agent is added into above-mentioned polymeric matrix, be uniformly dispersed；
Wherein, described flexibility agent is partially hydrolyzed polyacrylamide (PHPA), and its percentage by weight is 0.01%~0.5%；Described Water-soluble polymer is polyvinyl alcohol, and its percentage by weight is 1%~10%；Described ionic binding agent is carboxymethyl cellulose Plain lithium, its percentage by weight are 1%~5%；Described conductive agent is in acetylene black, graphite, graphene, CNT Any one or a few, its percentage by weight is 1%~12%.
2. a kind of based lithium-ion battery positive plate, it is characterised in that used the water-based of preparation according to the method for claim 1 Compound binding agent.
3. based lithium-ion battery positive plate according to claim 2, it is characterised in that：The percentage by weight of the flexibility agent is 0.01%~0.3%.
4. based lithium-ion battery positive plate according to claim 2, it is characterised in that：The weight hundred of the water-soluble polymer Divide than being 2%~7%.
5. based lithium-ion battery positive plate according to claim 2, it is characterised in that：The weight hundred of the ionic binding agent Divide than being 1%~3.5%.
6. based lithium-ion battery positive plate according to claim 2, it is characterised in that：The percentage by weight of the conductive agent is 2%~10%.
7. a kind of lithium ion battery, including the based lithium-ion battery positive plate described in claim 2~6 any one.
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CN106356534A (en) * 2015-07-18 2017-01-25 宁波大学 Adhesive for lithium ion battery and preparation method of adhesive
CN105489897B (en) * 2015-11-27 2018-05-04 中航锂电（洛阳）有限公司 Ternary cathode material of lithium ion battery conduction liquid and preparation method thereof, lithium ion battery
CN105336961A (en) * 2015-11-30 2016-02-17 四川北方硝化棉股份有限公司 Lithium battery anode and preparation method thereof
CN105428658B (en) * 2015-12-21 2018-01-09 中盐安徽红四方锂电有限公司 A kind of aqueous binders positive electrode of ferric phosphate lithium cell and preparation method thereof
CN107732169B (en) * 2017-09-17 2021-02-12 亚士创能科技(上海)股份有限公司 Silicon-based negative electrode material of lithium battery, preparation method of silicon-based negative electrode material, battery negative electrode and lithium battery
CN109167064B (en) * 2018-08-21 2021-08-27 李国富 Composite binder applied to lithium ion battery anode material and preparation method thereof
CN111129499A (en) * 2019-12-30 2020-05-08 宣城研一新能源科技有限公司 Water-based conductive adhesive for lithium battery and preparation method thereof
CN111668485B (en) * 2020-05-22 2021-11-02 远景动力技术(江苏)有限公司 Binder for lithium ion battery and preparation method and application thereof
CN112029452B (en) * 2020-09-10 2022-04-15 华鼎国联四川电池材料有限公司 Preparation method and application of adhesive capable of improving battery rate performance
CN113644273A (en) * 2021-08-13 2021-11-12 中科检测技术服务(重庆)有限公司 Ionic-electronic co-conductive material and preparation method and device thereof
CN114805823A (en) * 2022-04-25 2022-07-29 惠州锂威新能源科技有限公司 Crosslinked composite binder, preparation method thereof, pole piece and secondary battery
CN117117077A (en) * 2023-01-13 2023-11-24 荣耀终端有限公司 Negative electrode plate, preparation method of negative electrode plate and lithium ion battery

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