CN105153974B - A kind of aqueous compound binding agent and its prepare aqueous positive-pole slurry methods - Google Patents
A kind of aqueous compound binding agent and its prepare aqueous positive-pole slurry methods Download PDFInfo
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Abstract
The present invention provides a kind of aqueous compound binding agent and its aqueous positive-pole slurry methods are prepared, including with the water-soluble polymer of the functional group Han-COOLi, water-soluble class containing lithium silicates or can be with free Li+The water-soluble binder for forming complex compound is ionic binder；Using the long-chain water-soluble polymer with adsorption-flocculation effect as flexibility agent；Using water-soluble polymer as main binder, three is blended to form aqueous compound binding agent；Respectively constituent presses mass fraction for its are as follows: 65-70 parts of main binder；30-35 parts of ionic binder；1.5 parts of flexibility agent.The present invention can effectively solve spinel lithium manganate battery in cyclic process the problem of Mn dissolution, and the battery of preparation is more environmentally friendly, charge-discharge performance is more preferable.
Description
Technical field
The present invention relates to materials chemistry and new energy fields, and in particular to aqueous compound binding agent and preparation method thereof makes
The aqueous compound binding agent made from this method is applied in the preparation of based lithium-ion battery positive plate.
Background technique
Lithium ion battery, as the first march of contemporary battery industry, the main charging applied in portable electronic product
Battery, electric tool and electric car etc..Domestic and external electric automobile market constantly expands, the demand of lithium ion battery
Amount also will constantly increase.Prepare lithium ion battery and need auxiliary material binder, it be also influence battery constitute and its it is comprehensive
An important factor for energy.Manganese-based anode material is to study lithium electricity positive electrode earlier, with cheap, safety is good, resistance to mistake
Filling property is good, the advantages that being readily synthesized, and is one of power lithium battery positive electrode of most development prospect.
But there is also following disadvantages: first is that, such positive electrode is mostly semiconductor structure, and electronics, ionic conductivity are low；
Second is that in electrolyte lithium salts decomposition, cause manganese to dissolve, two of dissolution zone gradually become individual event structure, electrolyte decomposition
Product will cause electrode polarization impedance increase.Lithium ion is embedded in the expansion and contraction for causing structure with abjection repeatedly, or even goes out
It now collapses, structural symmetry is caused to reduce, crystal structure is converted into tetragonal crystal system by cubic system.Structure when being coexisted due to two
It is incompatible, it cannot be contacted well between electrode material particles, Li+Diffusion is difficult, and polarization increases, and irreversible capacity loss is caused to increase
Add, be unable to satisfy the biggish charging and discharging currents of battery and cycle life, the conduction of lithium ion, electronics also relies on binder and activity
Material junction.
Summary of the invention
The aqueous compound of spinel manganese base anode material cyclical stability can be improved the purpose of the present invention is to provide a kind of
Binder and its aqueous positive-pole slurry methods are prepared, and its application in lithium ion battery is provided.It is aqueous compound viscous using this
Lithium ion battery internal resistance made from knot agent is small, and charge-discharge performance is excellent.
The purpose of the present invention is what is be achieved through the following technical solutions.
A kind of aqueous compound binding agent, including with the water-soluble polymer of the functional group Han-COOLi, water-soluble silicic acid containing lithium
Salt can be with free Li+The water-soluble binder for forming complex compound is ionic binder；With adsorption-flocculation effect
Long-chain water-soluble polymer be flexibility agent；Using water-soluble polymer as main binder, three is blended to form aqueous compoiste adhering
Agent；Respectively constituent presses mass fraction for its are as follows: 65-70 parts of main binder；30-35 parts of ionic binder；Flexibility agent 1.5
Part.
It is further preferred that the water-soluble polymer that the ionic binder is the functional group containing-COOLi is selected from carboxymethyl
At least one of cellulose lithium, Lithium polyacrylate, polymethylacrylic acid lithium and its derivative.
It is further preferred that the water-soluble lithium silicates that contain are lithium metasilicate.
It is further preferred that described can be with free Li+The water-soluble binder for forming complex compound is polyethylene glycol oxide.
It is further preferred that the ionic binder is carboxymethyl cellulose lithium, preparation method is specifically included: by carboxylic
Sodium carboxymethylcellulose pyce is scattered in ethyl alcohol, stirs lower acid adding dissolution, and 90% ethyl alcohol, precipitating, mistake is added in insoluble matter precipitation to be had
Filter, washing, dry carboxymethyl cellulose；It disperses carboxymethyl cellulose in ethyl alcohol, lithium hydroxide solution is added, stirring is extremely
Carboxymethyl cellulose all dissolves, and 90% ethyl alcohol is added, precipitates, be filtered, washed, dry carboxymethyl cellulose lithium, dissolution
The aqueous solution that mass fraction is 2% is formed in deionized water.
It is further preferred that the flexibility agent is partially hydrolyzed polyacrylamide (PHPA), polyacrylamide, polyethylene glycol oxide, gathers
One or more of vinylpyrrolidone and polyvinyl alcohol.
It is further preferred that the flexibility agent is partially hydrolyzed polyacrylamide (PHPA), preparation method is specifically included: by poly- third
Acrylamide is soluble in water, and lithium hydroxide is added, and is heated to 40~90 DEG C, stirs 2~8h, is cooled to room temperature, and organic solvent is added
It if ethyl alcohol is to there is solid precipitation, stands, filters, wash, drying, drying temperature is 50~80 DEG C, is dissolved in deionized water, is formed
The aqueous solution that mass fraction is 0.15%.
It is further preferred that the main binder is polyvinyl alcohol, solution is specially heated to 50~80 DEG C, until poly- second
Enol all dissolves, and forms the aqueous solution that mass fraction is 10%.
It is a kind of to prepare aqueous positive-pole slurry methods using the upper aqueous compound binding agent, comprising: to be weighed by mass fraction
8 parts of aqueous compound binding agent, 10 parts of conductive agent, 82 parts of positive electrode, 200-250 parts of deionized water；Above-mentioned each component is aqueous
Deionized water is added in agitating device dissolution and obtains Polymer Solution compound binding agent respectively；Conductive agent is added to macromolecule
In solution, quickly stir at least 1 hour；Positive electrode is added, stirs at least 3 hours, a small amount of ethyl alcohol defoaming is added, obtains anode
Slurry.
It is further preferred that the positive electrode is aluminium doped spinel LiMn2O4, preparation method is as follows: first by change
It is Li more anhydrous than accurate weighing to learn metering2CO3, electrolysis MnO2With γ-Al2O3, then it is fully ground and is moved back to oxygen in the agate mortar
Change in aluminium crucible, in air atmosphere, be warming up to 800 DEG C with the rate of 10 DEG C/min, keep the temperature 12h, after cooled to room temperature
It can take out, obtain target product.
Compared with prior art, the present invention beneficial effect is: the present invention is replaced traditional using aqueous compound binding agent
After Kynoar is as lithium ion battery binder, adhesive property more more superior than conventional binders is realized, is made simultaneously
Standby battery has excellent performance outstanding.1) functional groups such as amide, carboxyl, hydroxyl introduced due to aqueous compound binding agent tool
There is good interfacial adhesion to act on, is effectively guaranteed binder to the adhesive attraction of active material, while these functional groups
Chemical bond can be formed with the hydroxyl of active material, conductive agent, to enhance the binding force of active material and conductive carbon, other carboxylic
Base and collector complexing easy to form improve the bonding to collector, to ensure that battery in repeated charge-discharge cycles
Enough fatigue resistances reduce the change rate of thickness of the battery in cyclic process.2) in electrocondution slurry preparation process, by
There is suitable surface tension in aqueous compound binding agent, be easy to sprawl in active material surface or collector, and dry
A continuous film is formed after dry on active material, there are good adhesion characteristics, in cyclic process, active matter to active material
The part of the surface of matter is preferably covered by binder, and the surface area of exposure in the electrolytic solution greatly reduces, to reduce electrolysis
Liquid guarantees the charge-discharge performance of battery in the irreversible consumption of active material surface.3) had using anode prepared by the present invention
Smaller impedance, better dynamic property performance, can effectively solve spinel lithium manganate battery in cyclic process Mn dissolve ask
Topic, the battery of preparation is more environmentally friendly, charge-discharge performance is more preferable.
Detailed description of the invention
Fig. 1 is PVDF and the LiMn of aqueous compound binding agent preparation2O4The cycle performance of battery compares；
Fig. 2 is PVDF and the LiMn of aqueous compound binding agent preparation2O4The specific capacity of battery and the relationship of voltage；
Fig. 3 LiMn2O4The AC impedance figure of battery；
Fig. 4 is PVDF and the LiAl of aqueous compound binding agent preparation0.04Mn1.96O4The cycle performance of battery compares；
Fig. 5 is PVDF and the LiAl of aqueous compound binding agent preparation0.04Mn1.96O4The specific capacity of battery and the relationship of voltage；
Fig. 6 LiAl0.04Mn1.96O4The AC impedance figure of battery；
The LiAl of two kinds of binders of Fig. 7 preparation0.04Mn1.96O4The scanning electron microscope (SEM) photograph (a) (b) (c) of positive plate is PVDF/
LiAl0.04Mn1.96O4Pole piece is respectively in 1000,10000,50000 times of scanning electron microscope (SEM) photograph；(d) (e) (f) is WSCB/
LiAl0.04Mn1.96O4Pole piece is respectively in 1000,10000,50000 times of scanning electron microscope (SEM) photograph.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
In the present invention, a kind of aqueous compound binding agent that can improve spinel manganese base anode material cyclical stability, it is
With the water-soluble polymer of the functional group Han-COOLi, water-soluble class containing lithium silicates or can be with free Li+Form complex compound
Water-soluble binder is ionic binder；Using the long-chain water-soluble polymer with adsorption-flocculation effect as flexibility agent；With water
Soluble polymer is main binder, and three is blended to form aqueous compound binding agent.
In the following, implementation result of the invention is described in detail by specific embodiment.
The preparation of [embodiment 1] anode
Include following component using the aqueous compound binding agent: being shown in Table 1
| Water-soluble polymer | Polyvinyl alcohol | 65-70 parts |
| Ionic binder | Carboxymethyl cellulose lithium | 30-35 parts |
| Flexibility agent | Partially hydrolyzed polyacrylamide (PHPA) | 1.5 part |
Table 1
Include following component using aqueous positive-pole slurry prepared by the aqueous compound binding agent: being shown in Table 2
| Aqueous compound binding agent | 8 parts |
| Conductive agent acetylene black | 10 parts |
| Positive electrode | 82 parts |
| Deionized water | 200-250 parts |
Table 2
In the above aqueous compound binding agent, partially hydrolyzed polyacrylamide (PHPA) is prepared by such method: by polyacrylamide
Amine is soluble in water, and lithium hydroxide is added, and is heated to 40~90 DEG C, stirs 2~8h, is cooled to room temperature, and organic solvent such as second is added
Alcohol is stood to there is solid precipitation, is filtered, and is washed, drying, and drying temperature is 50~80 DEG C, is dissolved in deionized water, forms quality
The aqueous solution that score is 0.15%.
Polyvinyl alcohol is dissolved in solution using such preparation method, solution is heated to 50~80 DEG C, until polyethylene
Alcohol all dissolves, and forms the aqueous solution that mass fraction is 10%.
Carboxymethyl cellulose lithium uses such preparation method, disperses sodium carboxymethylcellulose in ethyl alcohol, under stirring
Acid adding (hydrochloric acid or sulfuric acid) dissolution, insoluble matter precipitation to be had is added 90% ethyl alcohol, precipitates, is filtered, washed, dry carboxylic first
Base cellulose；It disperses carboxymethyl cellulose in ethyl alcohol, lithium hydroxide solution is added, stir all molten to carboxymethyl cellulose
Solution, is added 90% ethyl alcohol, precipitates, is filtered, washed, and dry carboxymethyl cellulose lithium is dissolved in deionized water and forms matter
Measure the aqueous solution that score is 2%.
Partially hydrolyzed polyacrylamide (PHPA), polyvinyl alcohol, carboxymethyl cellulose lithium form aqueous multiple according to above-mentioned component blend
Close binder, specifically, by main binder, ionic binder, flexibility agent respectively deionized water be added to it is molten in agitating device
Solution, obtains the solution of each component, these three solution is blended to obtain Polymer Solution by formula ratio；The conductive agent of formula ratio is added
Enter into Polymer Solution, quickly stirring at least 1 hour；The active material of formula ratio is added, stirs at least 3 hours, is added few
Ethyl alcohol defoaming is measured, anode sizing agent is obtained；Anode sizing agent is uniformly coated on collector single side aluminium foil, naturally dry, then dried
It is dry to obtain lithium ion cell positive.
Relative to aqueous compound binding agent, solvent is free of, the weight percent of part of hydrolyzed polyacrylamide is
0.15%, polyvinyl alcohol: carboxymethyl cellulose lithium is 2: 1.
The positive electrode is aluminium doped spinel LiMn2O4, and preparation method is as follows:
Doped spinel type LiMn2O4 LiAl0.04Mn1.96O4It is to be prepared by high temperature solid-state method, main method and condition
It is as described below: the first stoichiometrically anhydrous Li of accurate weighing2CO3, electrolysis MnO2With γ-Al2O3, then in the agate mortar
It is fully ground and moves back into alumina crucible, in air atmosphere, be warming up to 800 DEG C with the rate of 10 DEG C/min, keep the temperature 12h,
It can be taken out after cooled to room temperature, obtain target product.
Lithium manganate having spinel structure LiMn2O4Preparation method it is same as mentioned above, be a difference in that stoichiometrically smart
Really weigh anhydrous Li2CO3With electrolysis MnO2。
(1) coating method of anode sizing agent
It with the slurry prepared above, is coated with scraper, using the single side aluminium foil with a thickness of 20um as collector, coating is thick
Degree is 400um, obtains positive plate after natural drying.
(2) battery assembly
It is above-mentioned dry after positive plate, be cut into diameter be 14mm sequin, be placed in baking oven 80 DEG C, bake 8h, then very
Dry 12h, weighs, using lithium piece as negative electrode tab, button cell is assembled into glove box at 120 DEG C empty, seals, and carries out electrically
It can test.
(3) battery testing
The battery sealed is placed on LAND indigo plant electrical measurement test system, 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.
[embodiment 2] method and step is same as above, the difference is that active material changes LiMn into2O4, binder, conductive agent, active matter
The ratio of matter three is 7: 10: 83.
[embodiment 3] 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 LiMn2O4, binder, conductive agent, active material three ratio be 7: 10:
83。
[embodiment 4] method and step is same as above, the difference is that compound binding agent is by polyethylene glycol oxide, polyvinyl alcohol, lithium metasilicate
Aqueous solution composition, active material LiMn2O4, binder, conductive agent, active material three ratio be 7: 10: 83.
[embodiment 5] method and step is same as above, unlike compound binding agent by polyethylene glycol oxide, polyvinylpyrrolidone,
Lithium silicate aqueous solution composition, active material LiMn2O4, binder, conductive agent, active material three ratio be 7: 10: 83.
[embodiment 6] method and step is same as above, the difference is that compound binding agent is by polyacrylamide, polyethylene glycol, lithium metasilicate
Aqueous solution composition, active material LiMn2O4, binder, conductive agent, active material three ratio be 7: 10: 83.
[embodiment 7] method and step is same as above, the difference is that compound binding agent is by polyacrylamide, polyvinyl alcohol, carboxymethyl
Cellulose lithium composition, active material LiMn2O4, binder, conductive agent, active material three ratio be 7: 10: 83.
[embodiment 8] method and step is same as above, the difference is that compound binding agent is by polyvinyl alcohol, carboxymethyl chitosan, silicic acid
Lithium aqueous solution composition, active material LiMn2O4, binder, conductive agent, active material three ratio be 7: 10: 83.
[embodiment 9] method and step is with embodiment 3,4,5,6,7,8, the difference is that active material is LiAl0.04Mn1.96O4,
Binder, conductive agent, active material three ratio be 8: 10: 82.
Comparative example: respectively with LiMn2O4、LiAl0.04Mn1.96O4For positive electrode, Kynoar (PVDF) be binder,
N-Methyl pyrrolidone (NMP) is that positive plate, positive plate composition is made in solvent are as follows: 80 parts of positive electrode, 10 parts of acetylene black, and PVDF
10 parts, 100 parts of NMP.Battery is made by above-mentioned steps, the difference is that, when PVDF is dissolved in NMP, 45 DEG C need to be heated to, is added
The hot time is 3-5h；It is placed directly in baking oven after the completion of slurry coating dry.
Show that compared with PVDF system, when using aqueous compound system, the specific discharge capacity of electrode is bright by Fig. 1-7 test
Aobvious to be improved, the distance between charging and discharging curve is smaller, and charge transfer resistance is lower, polarizes smaller.First is that since battery exists
For the first time in circulation, part Li+The generation for taking part in solid liquid interface oxide layer SEI film will lead to the irreversibility enhancing of battery, water
Ionic binder in sex camplex system can provide lithium ion, reduce the irreversibility for the first time of battery, therefore aqueous compound
The first discharge specific capacity of system is higher.Second is that since conductive agent and binder interaction are equably wrapped in positive electrode
When on particle, foring good conductive network, and using PVDF as binder, conductive agent be then located at positive electrode particle it
Between, and there are serious agglomerations, and part positive electrode is not contacted with conductive agent, binder, thus electric conductivity is poor.
Third is that active material occurs to need when reduction reaction since aqueous compound system improves the interface property between electrode and electrolyte
Lithium ion, and this part lithium ion can be by the Ionomer in the aqueous compound binding agent close to reaction center
Lithium ion provides.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of aqueous compound binding agent, which is characterized in that including with the water-soluble polymer of the functional group Han-COOLi, water solubility
Class containing lithium silicates can be with free Li+The water-soluble binder for forming complex compound is ionic binder；To have absorption
The long-chain water-soluble polymer of flocculation is flexibility agent；Using water-soluble polymer as main binder, three be blended to be formed it is aqueous
Compound binding agent；Respectively constituent presses mass fraction for its are as follows: 65-70 parts of main binder；30-35 parts of ionic binder；It is soft
Tough dose 1.5 parts.
2. aqueous compound binding agent as described in claim 1, which is characterized in that the ionic binder is containing-COOLi official
The water-soluble polymer that can be rolled into a ball is in carboxymethyl cellulose lithium, Lithium polyacrylate, polymethylacrylic acid lithium and its derivative
It is at least one.
3. aqueous compound binding agent as described in claim 1, which is characterized in that the water-soluble lithium silicates that contain are silicic acid
Lithium.
4. aqueous compound binding agent as described in claim 1, which is characterized in that it is described can be with free Li+Form the water of complex compound
Soluble binder is polyethylene glycol oxide.
5. aqueous compound binding agent as claimed in claim 2, which is characterized in that the ionic binder is carboxymethyl cellulose
Plain lithium, preparation method specifically include: it disperses sodium carboxymethylcellulose in ethyl alcohol, stirs lower acid adding dissolution, it is insoluble wait have
Object is precipitated, and 90% ethyl alcohol is added, precipitates, be filtered, washed, dry carboxymethyl cellulose；It disperses carboxymethyl cellulose in
In ethyl alcohol, addition lithium hydroxide solution, stirring to carboxymethyl cellulose is all dissolved, and 90% ethyl alcohol is added, precipitate, filter,
Washing, dry carboxymethyl cellulose lithium are dissolved in the aqueous solution for forming that mass fraction is 2% in deionized water.
6. aqueous compound binding agent as described in claim 1, which is characterized in that the flexibility agent is partial hydrolysis polyacrylamide
One or more of amine, polyacrylamide, polyethylene glycol oxide, polyvinylpyrrolidone and polyvinyl alcohol.
7. aqueous compound binding agent as claimed in claim 6, which is characterized in that the flexibility agent is partial hydrolysis polyacrylamide
Amine, preparation method specifically include: polyacrylamide is soluble in water, lithium hydroxide is added, is heated to 40~90 DEG C, stirring 2
~8h, is cooled to room temperature, and organic solvent such as ethyl alcohol is added to there is solid precipitation, stands, filters, wash, drying, and drying temperature is
It 50~80 DEG C, is dissolved in deionized water, forms the aqueous solution that mass fraction is 0.15%.
8. aqueous compound binding agent as described in claim 1, which is characterized in that the main binder is polyvinyl alcohol, specifically
For solution is heated to 50~80 DEG C, until polyvinyl alcohol all dissolves, the aqueous solution that mass fraction is 10% is formed.
9. the method that aqueous compound binding agent described in a kind of right to use 1 prepares aqueous positive-pole slurry characterized by comprising press
Mass fraction weighs 8 parts of aqueous compound binding agent, 10 parts of conductive agent, 82 parts of positive electrode, 200-250 parts of deionized water；It will lead
Binder, ionic binder, flexibility agent are added in agitating device with deionized water dissolve respectively, obtain the molten of each component
Liquid, these three solution are blended to obtain Polymer Solution by formula ratio: conductive agent being added in Polymer Solution, is quickly stirred
At least 1 hour: positive electrode is added, stirs at least 3 hours, a small amount of ethyl alcohol defoaming is added, obtains anode sizing agent.
10. aqueous compound binding agent as claimed in claim 9 prepares aqueous positive-pole slurry methods, which is characterized in that it is described just
Pole material is aluminium doped spinel LiMn2O4, and preparation method is as follows: the first stoichiometrically anhydrous Li of accurate weighing2CO3、
It is electrolysed MnO2With γ-Al2O3, it is then fully ground and is moved back into alumina crucible in the agate mortar, in air atmosphere, with
The rate of 10 DEG C/min is warming up to 800 DEG C, keeps the temperature 12h, can take out after cooled to room temperature, obtain target product.
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| CN110690451B (en) * | 2018-07-05 | 2022-09-13 | 贝特瑞新材料集团股份有限公司 | Conductive aqueous adhesive for lithium ion battery and preparation method and application thereof |
| CN109309232A (en) * | 2018-09-13 | 2019-02-05 | 深圳市电科电源股份有限公司 | A kind of preparation method of lithium ion battery with high energy density |
| CN111668483B (en) * | 2019-03-09 | 2022-04-15 | 江苏道赢科技有限公司 | Battery electrode binder and preparation method thereof |
| CN110911644A (en) * | 2019-10-30 | 2020-03-24 | 深圳市卓能新能源股份有限公司 | Lithium ion positive coating and lithium ion battery |
| CN112968177B (en) * | 2021-03-01 | 2022-02-22 | 广州鹏辉能源科技股份有限公司 | Water-based anode slurry composition, water-based anode slurry, preparation method of water-based anode slurry, anode plate, lithium ion battery and power utilization equipment |
| CN113725438B (en) * | 2021-09-02 | 2022-10-14 | 广州市乐基智能科技有限公司 | Water-based composite binder for solid lithium battery and application thereof |
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| CN114335422A (en) * | 2021-12-30 | 2022-04-12 | 珠海冠宇电池股份有限公司 | Negative plate and lithium ion battery comprising same |
| CN115425226B (en) * | 2022-08-18 | 2023-04-14 | 楚能新能源股份有限公司 | Ternary material flexible positive electrode and preparation method thereof |
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| CN105153974A (en) | 2015-12-16 |
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Denomination of invention: The invention relates to a water-based composite binder and a method for preparing water-based positive paste Effective date of registration: 20201229 Granted publication date: 20190115 Pledgee: Shenzhen hi tech investment small loan Co.,Ltd. Pledgor: Shenzhen Tenglongyuan Industrial Co.,Ltd. Registration number: Y2020980010201 |