CN106207190B - A kind of anode material for lithium-ion batteries compound binding agent and preparation method thereof - Google Patents
A kind of anode material for lithium-ion batteries compound binding agent and preparation method thereof Download PDFInfo
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- CN106207190B CN106207190B CN201610852754.9A CN201610852754A CN106207190B CN 106207190 B CN106207190 B CN 106207190B CN 201610852754 A CN201610852754 A CN 201610852754A CN 106207190 B CN106207190 B CN 106207190B
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- polyacrylic acid
- binding agent
- epoxy resin
- compound binding
- kynoar
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- H01M4/622—Binders being polymers
- H01M4/623—Binders being polymers fluorinated polymers
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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
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- Engineering & Computer Science (AREA)
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- Manufacturing & Machinery (AREA)
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Abstract
The invention belongs to technical field of lithium ion, a kind of anode material for lithium-ion batteries composite caking agent and preparation method are disclosed.Compound binding agent its be prepared by the component of following mass percent: polyacrylic acid grafted modified epoxy be 1~10%；Molecular weight 6 × 105Kynoar be 30~48%, N-Methyl pyrrolidone be 51~62%.Its preparation step are as follows: first by solution graft polymerization method, preparation synthesizes polyacrylic acid grafted modified epoxy and obtains compound binding agent then by the N-Methyl pyrrolidone solution blending of itself and Kynoar.The compound binding agent adhesive force with higher and good solvent-resisting prepared using method of the invention, is significantly reduced the internal resistance of lithium ion battery, improves the cycle performance of battery.
Description
Technical field
The invention belongs to the technical fields of new energy materials, and in particular to a kind of anode material for lithium-ion batteries is with compound viscous
Tie agent and preparation method.
Background technique
For lithium ion battery due to its operating voltage height, specific energy is big, quickly-chargeable and many advantages, such as having extended cycle life,
It has been widely used as mobile phone, computer, the power supply of the mobile devices such as electric car at present.It is mainly by positive and negative anodes, electrolyte, diaphragm and
Shell composition.Wherein electrode is mainly by active material, conductive agent, binder and collector composition.The performance of lithium ion battery with
Fabrication Technology of Electrode has very big relationship, such as the performance of binder, active material, conductive agent, the ratio of binder etc..Lithium at present
The common binder of ion battery is the N-Methyl pyrrolidone solution of Kynoar.Kynoar is due to higher
Dielectric constant, stable electrochemical window, and slurry is easily formed, it is widely used in commodity lithium ion battery.But
There is also some defects at present for Kynoar binder, such as in the battery pole piece for making binder preparation with Kynoar,
It is easily swollen by electrolyte, and pole piece structure is caused to change, and electrode material and current collector adhesion force is caused to decline and make circulating battery
Performance decline；Also, electrode active material is coated by the Kynoar of semicrystalline structure, the Kynoar suppression of crystal region
The abjection or insertion of preparing lithium ion, and the weak interaction of active material and Kynoar causes active material to be unevenly distributed,
Easy cluster.
Summary of the invention
Goal of the invention of the invention is to reduce internal resistance of the conventional binders in lithium ion battery and improve its adherency
Power performance etc. provides a kind of anode material for lithium-ion batteries compound binding agent and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of anode material for lithium-ion batteries compound binding agent, is prepared by the component of following mass percent:
Polyacrylic acid grafted modified epoxy is 1~10%；Molecular weight 6 × 105Kynoar be 30~48%, N- methyl pyrrole
Pyrrolidone is 51~62%；
Wherein, the polyacrylic acid grafted modified epoxy is prepared via a method which to obtain: by benzoyl peroxide first
Acyl is mixed with acrylic acid, then the mixing and epoxy resin are mixed in n-butanol, and heat up graft reaction, is obtained polyacrylic acid and is connect
Branch modified epoxy.
Preferably, the number-average molecular weight of the Kynoar is Mn=6 × 105。
Preferably, the epoxy resin is epoxy resin 601.
A kind of anode material for lithium-ion batteries compound binding agent preparation method comprising following steps:
(1) first initiator benzoyl peroxide is mixed with acrylic monomers, obtains mixing A,
(2) above-mentioned mixing A is added in n-butanol, then epoxy resin is added in the n-butanol, be uniformly mixed, risen
Polyacrylic acid grafted modified epoxy is made in warm graft copolymerization；
(3) Kynoar powder is dissolved in N-Methyl pyrrolidone solution, adds polyacrylic acid above-mentioned and connects
Compound binding agent is prepared in branch modified epoxy, reaction.
Preferably, in the step (1), benzoyl peroxide and acrylic monomers are 1: 10~1: 20 progress in mass ratio
Mixing.
Preferably, in the step (2), mixing A and epoxy resin mass ratio are 1: 3~1: 6.
Preferably, in the step (2), by above-mentioned mixing A be added n-butanol in, then by epoxy resin be added to it is described just
In butanol, 100~120 DEG C are warming up to, graft copolymerization 3~6 hours, polyacrylic acid grafted modified ring was made in high speed centrifugation, drying
Oxygen resin.
Preferably, in the step (3), Kynoar powder is dissolved in N-Methyl pyrrolidone solution, in room
Polyacrylic acid grafted modified epoxy is added after lower stirring 12~18 hours in temperature, is stirred for 3~6 hours, so that be completely dissolved,
Compound binding agent is made.
Preferably, the molecular weight of the Kynoar is equal Mn=6 × 10 of number5。
Preferably, the epoxy resin is epoxy resin 601.
In order to achieve the above object, another technical solution that the present invention takes is:
A kind of anode material for lithium-ion batteries compound binding agent preparation method, includes the following steps:
Step 1 prepares polyacrylic acid grafted modified epoxy: first by initiator benzoyl peroxide and acrylic acid list
Body in mass ratio 1: 10~1: 20 mixes, then mixing and epoxy resin 601 are mixed according to the ratio of mass ratio 1: 3~1: 6
In n-butanol, 100~120 DEG C are warming up to, graft copolymerization 3~6 hours, polyacrylic acid grafted modification was made in high speed centrifugation, drying
Epoxy resin；
Step 2 prepares compound binding agent: by molecular weight Mn=6 × 105Kynoar powder be dissolved in N- methyl pyrrole
In pyrrolidone solution, polyacrylic acid grafted modified epoxy is added after stirring 12~18 hours at room temperature, it is small to be stirred for 3~6
When, so that being completely dissolved, compound binding agent is made.
Present invention design synthesizes a kind of composition polymer that caking property is good, and electrolyte resistance corrodes: polyacrylic acid grafted modification
Binder is made with polyvinylidene blending in it by epoxy resin.Using compound binding agent obtained by positive electrode active materials, lead
Electric agent, which is adhered on aluminium foil, is made anode pole piece.Since its compound binding agent contains corrosion resistant acrylated epoxy group, increase
The adhesion strength of pole piece and active material is added, it is suppressed that the excessive swelling of Kynoar improves the mechanics of Kynoar
Supporting role；On the other hand, modified epoxy resin contains a large amount of carboxyl groups, generates electrostatic repulsion and promotes conductive agent and activity
The dispersion of material.
Of the invention is a little with beneficial effect:
1, the present invention by using polyacrylic acid grafted modified epoxy blend polyvinylidene fluoride as lithium ion battery just
Pole binder is conducive to the stability for keeping electrode structure since epoxy itself has stronger adhesion strength, prevents electrode de-
It falls；
2, polyacrylic acid grafted modified epoxy contains a large amount of carboxyl groups, and the carboxyl to dissociate in the electrolytic solution generates one
Kind of electrostatic repulsion field, it is suppressed that conductive agent with or active material cluster, improve its dispersibility.Changed using polyacrylic acid grafted
Property epoxy blend Kynoar as the dispersibility of lithium ion cell positive made from binder, caking property and solvent resistance
Improved；
3, using polyacrylic acid grafted modified epoxy blend polyvinylidene fluoride as binder, be conducive to improve battery
Chemical property.
With active material LiCo2Content is 80%, conductive agent conductive black content be 10% made from lithium ion battery just
Pole pole piece is washed into the sequin of diameter 1cm, as anode, using metal lithium sheet as cathode, and import polyethylene/polypropylene/poly- second
Three layers of microporous barrier (celgard 2325) of alkene are diaphragm, 1M LiPF6/ ethylene carbonate (EC)+dimethyl carbonate (DMC)+carbonic acid
The mixed solution of diethylester (DEC) (mass ratio 1: 1: 1) is electrolyte, is assembled into button in the glove box of argon hydrogen gaseous mixture
The chemical property of battery 2032, battery is improved significantly.It is assembled into the charge and discharge under room temperature 0.5C multiplying power after battery, battery
First discharge specific capacity is 178.9mAh/g, and capacity is maintained at 161.5mAh/g after circulation 50 times, and capacity retention ratio reaches
90.27%, and using Kynoar for capacity after circulating battery 50 times of binder is 112.9mAh/g, capacity retention ratio is only
It is 67.8%.
Detailed description of the invention:
Fig. 1 is that the polyacrylic acid grafted modified epoxy blend polyvinylidene fluoride of the present invention gathers as binder and traditional
Cycle performance of battery test comparison chart of the vinylidene as binder.
Fig. 2 is that the polyacrylic acid grafted modified epoxy blend polyvinylidene fluoride of the present invention gathers as binder and traditional
Circulating battery volt-ampere performance test comparison diagram of the vinylidene as binder.
Fig. 3 is that the polyacrylic acid grafted modified epoxy blend polyvinylidene fluoride of the present invention prepares anode as binder and fills
The pole piece shape appearance figure of the circle of discharge cycles 50 front and back；Fig. 3 A is the pole piece shape appearance figure before charge and discharge cycles 50 are enclosed, and Fig. 3 B is charge and discharge
Pole piece shape appearance figure after 50 circle of circulation.
Fig. 4 is the pole piece pattern that traditional Kynoar prepares the positive circle of charge and discharge cycles 50 front and back as binder
Figure, Fig. 4 A are the pole piece shape appearance figure before charge and discharge cycles 50 are enclosed, and Fig. 4 B is the pole piece shape appearance figure after charge and discharge cycles 50 are enclosed.
Specific embodiment
The following examples are of the invention to be further described, but the contents of the present invention are without being limited thereto.Present invention explanation
Embodiment in book is only used for that the present invention will be described, does not play restriction effect to protection scope of the present invention.This
The protection scope of invention is only defined by the claims, and those skilled in the art are in embodiment disclosed by the invention on the basis of institute
Any omission, replacement or the modification made fall within protection scope of the present invention.
Embodiment 1
(1) acrylic monomers is mixed with initiator benzoyl peroxide in mass ratio 1: 10, then by mixing and asphalt mixtures modified by epoxy resin
Rouge 601, with n-butanol, using benzoyl peroxide as initiator, is warming up to 120 DEG C, connects according to the ratio mixing of mass ratio 1: 3
Branch copolymerization 3 hours, polyacrylic acid grafted modified epoxy is made in high speed centrifugation, drying.
(2) by molecular weight Mn=1 × 105Kynoar powder be dissolved in N-Methyl pyrrolidone solution, room temperature
Polyacrylic acid grafted modified epoxy is added after 12 hours in stirring, is stirred for 3 hours that it is molten to obtain binder so that being completely dissolved
Liquid, polyacrylic acid grafted modified epoxy in compound binding agent system: Kynoar: N-Methyl pyrrolidone mass ratio is
1∶48∶51。
Embodiment 2
(1) acrylic monomers is mixed with initiator benzoyl peroxide in mass ratio 1: 20, then by mixing and asphalt mixtures modified by epoxy resin
Rouge 601, with n-butanol, using benzoyl peroxide as initiator, is warming up to 100 DEG C, connects according to the ratio mixing of mass ratio 1: 6
Branch copolymerization 6 hours, polyacrylic acid grafted modified epoxy is made in high speed centrifugation, drying.
(2) by molecular weight Mn=1 × 105Kynoar powder be dissolved in N-Methyl pyrrolidone solution, room temperature
Polyacrylic acid grafted modified epoxy is added after 18 hours in stirring, is stirred for 6 hours that it is molten to obtain binder so that being completely dissolved
Liquid, polyacrylic acid grafted modified epoxy in compound binding agent system: Kynoar: N-Methyl pyrrolidone mass ratio is
2∶36∶62。
Embodiment 3
(1) acrylic monomers is mixed with initiator benzoyl peroxide in mass ratio 3: 40, then by mixing and asphalt mixtures modified by epoxy resin
Rouge 601, with n-butanol, using benzoyl peroxide as initiator, is warming up to 110 DEG C, connects according to the ratio mixing of mass ratio 1: 4
Branch copolymerization 4.5 hours, polyacrylic acid grafted modified epoxy is made in high speed centrifugation, drying.
(2) by molecular weight Mn=1 × 105Kynoar powder be dissolved in N-Methyl pyrrolidone solution, room temperature
Polyacrylic acid grafted modified epoxy is added after 15 hours in stirring, is stirred for 4.5 hours obtaining binder so that being completely dissolved
Solution, polyacrylic acid grafted modified epoxy in compound binding agent system: Kynoar: N-Methyl pyrrolidone mass ratio
It is 5: 39: 56.
Embodiment 4
(1) acrylic monomers is mixed with initiator benzoyl peroxide in mass ratio 1: 11, then by mixing and asphalt mixtures modified by epoxy resin
Rouge 601, with n-butanol, using benzoyl peroxide as initiator, is warming up to 115 DEG C, connects according to the ratio mixing of mass ratio 1: 5
Branch copolymerization 5 hours, polyacrylic acid grafted modified epoxy is made in high speed centrifugation, drying.
(2) by molecular weight Mn=1 × 105Kynoar powder be dissolved in N-Methyl pyrrolidone solution, room temperature
Polyacrylic acid grafted modified epoxy is added after 16 hours in stirring, is stirred for 5 hours that it is molten to obtain binder so that being completely dissolved
Liquid, polyacrylic acid grafted modified epoxy in compound binding agent system: Kynoar: N-Methyl pyrrolidone mass ratio is
10∶30∶60。
Test case
Test specimens: using the positive electrode compound binding agent being prepared in embodiment 4, contained with active material LiCo2
Amount is 80%, and conductive agent conductive black content is the sequin that anode slice of lithium ion battery made from 10% is washed into diameter 1cm,
As anode, using metal lithium sheet as cathode, import polyethylene/polypropylene/three layers of polyethylene microporous barrier (celgard 2325)
For diaphragm, 1M LiPF6/ ethylene carbonate (EC)+dimethyl carbonate (DMC)+diethyl carbonate (DEC) (mass ratio 1: 1: 1)
Mixed solution be electrolyte, button cell 2032 is assembled into the glove box of argon hydrogen gaseous mixture,
Control sample: using traditional Kynoar as binder, by method pulping film-forming in test model at anode,
Assembled battery again.
Test condition: charge-discharge performance test is carried out to battery with Land battery performance detection device, positive fills
Discharge voltage range is 2.5V~4.25V, and charge-discharge magnification 0.5C, test temperature is 25 DEG C.With electrochemical workstation CHI600E
Equipment carries out cyclic voltammetry to battery, and voltage range is 2.5V~4.5V, sweep speed 0.5mV/s.
Test result: Fig. 1 is that the battery of compound binding agent and traditional Kynoar binder prepared by embodiment 4 follows
Ring performance test comparison diagram.As can be seen from the figure the battery of the compound binding agent assembling prepared using embodiment 4 is discharged for the first time
Specific capacity is 178.9mAh/g, and capacity is maintained at 161.5mAh/g after circulation 50 times, and capacity retention ratio reaches 90.27%, and adopts
It is 112.9mAh/g with capacity after the circulating battery that Kynoar is binder 50 times, capacity retention ratio is only 67.8%.
Fig. 2 is the circulating battery volt-ampere of compound binding agent prepared by embodiment 4 and traditional Kynoar binder
It can test comparison chart.The cell oxidation reduction potential difference of the compound binding agent prepared using embodiment 4 is only 0.3V, redox
Peak is obvious, and charge and discharge invertibity is better than traditional Kynoar as battery made from binder.
Fig. 3 A, 3B are the pole piece patterns that compound binding agent prepared by embodiment 4 prepares the positive circle of charge and discharge cycles 50 front and back
Figure.Positive electrode active materials are evenly distributed with conductive agent, and obvious Cluster Phenomenon does not occur before and after charge and discharge.
Fig. 4 A, 4B are the pole piece shapes that traditional Kynoar prepares the positive circle of charge and discharge cycles 50 front and back as binder
Looks figure.Positive electrode active materials and conductive agent dispersion are uneven, and cluster easily occurs after charge and discharge.
The foregoing examples are merely illustrative of the technical concept and features of the invention, its object is to allow the person skilled in the art to be
It cans understand the content of the present invention and implement it accordingly, it is not intended to limit the scope of the present invention.It is all smart according to the present invention
The equivalent transformation or modification that refreshing essence is done, should be covered by the protection scope of the present invention.
Claims (6)
1. a kind of anode material for lithium-ion batteries compound binding agent, is prepared by the component of following mass percent: poly-
Acrylic graft-modified epoxy resin is 1~10%；Molecular weight 6 × 105Kynoar be 30~48%, N- methylpyrrole
Alkanone is 51~62%, and the number-average molecular weight of the Kynoar is Mn=6 × 105, the epoxy resin is epoxy resin
601；
Wherein, the polyacrylic acid grafted modified epoxy is prepared via a method which to obtain: by benzoyl peroxide and third
Olefin(e) acid mixing, then the mixing and epoxy resin are mixed in n-butanol, heat up graft reaction, obtains polyacrylic acid grafted modification
Epoxy resin.
2. the method for preparing compound binding agent as described in claim 1, which is characterized in that it includes the following steps:
(1) first initiator benzoyl peroxide is mixed with acrylic monomers, obtains mixing A,
(2) above-mentioned mixing A is added in n-butanol, then epoxy resin is added in the n-butanol, be uniformly mixed, heating connects
Branch copolyreaction, is made polyacrylic acid grafted modified epoxy；
(3) Kynoar powder is dissolved in N-Methyl pyrrolidone solution, adds above-mentioned polyacrylic acid grafted change
Property epoxy resin, reaction compound binding agent is prepared.
3. preparation method according to claim 2, which is characterized in that in the step (1), benzoyl peroxide and propylene
Acid monomers are 1: 10~1: 20 mixing in mass ratio.
4. preparation method according to claim 2, which is characterized in that in the step (2), mixing A and asphalt mixtures modified by epoxy resin lipid
Amount is than being 1: 3~1: 6.
5. preparation method according to claim 2, which is characterized in that in the step (2), n-butanol is added in mixing A
In, then epoxy resin is added in the n-butanol, is uniformly mixed, is warming up to 100~120 DEG C, graft copolymerization 3~6 hours,
Polyacrylic acid grafted modified epoxy is made in high speed centrifugation, drying.
6. preparation method according to claim 2, which is characterized in that in the step (3), Kynoar powder is molten
Polyacrylic acid grafted modified epoxy tree is added in N-Methyl pyrrolidone solution in solution after being stirred at room temperature 12~18 hours
Rouge is stirred for 3~6 hours, so that being completely dissolved, compound binding agent is made.
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| US11374223B2 (en) * | 2017-06-30 | 2022-06-28 | Ppg Industries Ohio, Inc. | Slurry composition including binder containing reaction product of epoxy functional polymer and acid functional polymer for lithium ion electrical storage devices |
| CN107863535A (en) * | 2017-10-20 | 2018-03-30 | 合肥国轩高科动力能源有限公司 | Composite binder of silicon-based negative electrode of lithium ion battery and preparation method thereof |
| CN109755575A (en) * | 2017-11-03 | 2019-05-14 | 南京知博工业科技有限公司 | A kind of composition and preparation method thereof |
| CN111200132B (en) * | 2018-11-16 | 2021-05-18 | 宁德时代新能源科技股份有限公司 | Battery with a battery cell |
| CN113764668B (en) * | 2021-08-17 | 2023-06-20 | 广州市乐基智能科技有限公司 | Composite binder for solid-state lithium battery and preparation method and application method thereof |
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