CN107611375A - A kind of preparation method of lithium ion battery anode glue size - Google Patents
A kind of preparation method of lithium ion battery anode glue size Download PDFInfo
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- CN107611375A CN107611375A CN201710718621.7A CN201710718621A CN107611375A CN 107611375 A CN107611375 A CN 107611375A CN 201710718621 A CN201710718621 A CN 201710718621A CN 107611375 A CN107611375 A CN 107611375A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention relates to the preparation method of lithium ion battery anode glue size, and it comprises the following steps：Binding agent, dispersant and solvent are added in mixer first and carry out disperseing to be made at a high speed, secondly, conductive agent is added into glue, after agitated machine stirs, heating water bath is carried out in dislocation temperature controlled ultrasonic ripple dispersion machine, pre-dispersed conductive rubber cement is made；Furthermore the ultrasonic wave divergent function of temperature controlled ultrasonic ripple dispersion machine is opened, high frequency ultrasound is carried out and disperses, scattered conductive rubber cement is made；Finally, conductive rubber cement and active material are added in mixer, carries out high-speed stirred and disperse, anode sizing agent is made.The preferable lithium ion battery anode glue size of dispersiveness can be prepared with reference to ultrasonic dispersion technique within the shorter time by also having by the preparation method by dispersant, improve stock quality simultaneously, production efficiency is improved, reduces organic solvent usage amount, production cost is reduced and reduces and pollute.
Description
Technical field
The present invention relates to secondary cell field, more specifically to a kind of preparation side of lithium ion battery anode glue size
Method.
Background technology
Lithium rechargeable battery has energy density height, environmental pollution is small, power density is big, service life is long, adapts to model
The advantages of to enclose that wide, self discharge coefficient is small etc. prominent, is one of battery being most widely used in the world now, and new energy hair
The important component of exhibition.
After lithium ion battery forms battery core by positive/negative plate and barrier film, load housing, be filled with what is obtained after electrolyte.Its
Middle positive plate is uniform coating after forming slurry in a solvent by positive active material and the scattered suspension of other a small amount of auxiliary materials
Obtained after being dried on to collector.The customary preparation methods of positive electrode current slurry are first to dissolve high polymer binder in a solvent
Glue is formed, then conductive agent is added in glue and uses mixer mechanical dispersion, last substep adds active material, carries out for a long time
Mechanical dispersion be made anode sizing agent；Or using it is another directly by active material, binding agent, conductive agent it is dry-mixed after step by step
Solvent is added, anode sizing agent is made after carrying out mechanical dispersion.Received because the conductive agent conductive black commonly used in anode sizing agent belongs to
The other particle of meter level, particle diameter is small, specific surface area is big, there is the characteristic for being easily agglomerated into bulky grain, and it is difficult uniform scattered to cause it
In active material surface, play a part of increasing electric conductivity.Conventional method does not add dispersant, only with the side of mechanical dispersion
Formula is disperseed, and not only the time is grown, and dispersion effect is poor, unstable product quality, to be reached viscosity needed for coating and be used
Quantity of solvent it is more, in batches use when defect it is obvious.
The content of the invention
The technical problem to be solved in the present invention is, there is provided one kind can solve the problem that jitter time long, dispersion effect difference and
The preparation method of the lithium ion battery anode glue size of unstable product quality.
The technical solution adopted for the present invention to solve the technical problems is：Construct a kind of system of lithium ion battery anode glue size
Preparation Method, comprise the following steps：
S1, binding agent, dispersant and solvent are added to the scattered obtained glue of progress high speed in mixer；
S2, conductive agent added to the glue, after the mixer stirs, be placed in temperature controlled ultrasonic ripple dispersion machine
Middle progress water bath with thermostatic control heating, is made pre-dispersed conductive rubber cement；
S3, the ultrasonic wave divergent function for opening the temperature controlled ultrasonic ripple dispersion machine, carry out high frequency ultrasound and disperse, be made and divide
The conductive rubber cement dissipated；
S4, the conductive rubber cement and active material added in mixer, carry out high-speed stirred and scattered, positive pole slurry is made
Material.
Preferably, the binding agent, the dispersant, the solvent, the conductive agent, the parts by weight of the active material
Number is respectively：The bonding agent 2.5~3, the dispersant 0.2~0.5, the solvent 56~62, the conductive agent 2~3, institute
State active material 94~95.
Preferably, in the S1 steps, the binding agent is Kynoar, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, carboxylic first
The one or more of base sodium cellulosate.
Preferably, in the S1 steps, the dispersant is polyvinylpyrrolidone, polyacrylic acid, polyacrylamide
One or more.
Preferably, in the S1 steps, the solvent is 1-METHYLPYRROLIDONE, deionized water.
Preferably, in the S2 steps, the conductive agent is conductive black, the one or more of electrically conductive graphite.
Preferably, in the S2 steps, the temperature of the heating water bath process is controlled to be constant at 25~60 DEG C.
Preferably, in the S3 steps, the ultrasonic wave high-frequency dispersion frequency control is 20kHz~80kHz, is disperseed
Time control is 10~30 minutes.
Preferably, in S4 steps, the active material is LiFePO4, cobalt acid lithium, LiMn2O4, one kind of ternary material
It is or a variety of.
Preferably, in the S1 steps, the speed of the high-speed stirred is 30rpm/min~60rpm/min；Described
In S2 steps, the mixing speed is 10rpm/min~30rpm/min；In the S4 steps, the speed of the high-speed stirred
For 30rpm/min~60rpm/min, the scattered speed of the high speed is 1000rpm/min~5000rpm/min.
Implement the preparation method of the lithium ion battery anode glue size of the present invention, have the advantages that：The present invention is first
Binding agent, dispersant and solvent are added in mixer and carry out disperseing to be made at a high speed, secondly, conductive agent is added into glue,
After agitated machine stirs, heating water bath is carried out in dislocation temperature controlled ultrasonic ripple dispersion machine, pre-dispersed conductive rubber cement is made；Again
Person, the ultrasonic wave divergent function of temperature controlled ultrasonic ripple dispersion machine is opened, carry out high frequency ultrasound and disperse, scattered conducting resinl is made
Slurry；Finally, conductive rubber cement and active material are added in mixer, carries out high-speed stirred and disperse, anode sizing agent is made.This hair
Bright preparation method is disperseed by using dispersant and with reference to ultrasonic dispersing machine, by the scattered conductive agent rapid dispersion of hardly possible
In solvent, under the stably dispersing effect of dispersant so that the solvent that active material uniformly disperses to need is less, and is made
Anode sizing agent can reach coating required for range of viscosities.It can be prepared by the preparation method within the shorter time
The preferable lithium ion battery anode glue size of dispersiveness, while stock quality is improved, production efficiency is improved, reduces organic solvent
Usage amount, reduce production cost and reduce and pollute.
Brief description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing：
Fig. 1 is the process chart of the preparation method of lithium ion battery anode glue size of the present invention.
Embodiment
In order to which technical characteristic, purpose and the effect of the present invention is more clearly understood, now compares accompanying drawing and describe in detail
The embodiment of the present invention.
As shown in figure 1, the preparation method comprises the following steps：
S1, binding agent, dispersant and solvent are added to the scattered obtained glue of progress high speed in mixer.
Specifically, the dispersant and weight that are 0.2~0.5 by bonding agent that parts by weight are 2.5~3, parts by weight
The solvent that number is 56~62 is put into the agitator of mixer, disperse at a high speed, is selected scattered speed as 1000rpm/
Min~5000rpm/min.Further, scattered speed is preferably 2000rpm/min~3000rpm/min.Jitter time is excellent
Elect 120min as.
Wherein, binding agent can strengthen bond effect, and it can be Kynoar, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, carboxylic
The one or more of sodium carboxymethylcellulose pyce；On the one hand the surface that the dispersant can be adsorbed in solid particle can make consolidating for cohesion
Body particle surface is easier to soak, and on the other hand, solid particles surface can be made to produce ionic charge, physical shielding, hydrogen bond, idol
Pole is acted on so as to prevent solid particle from condensing again, and it can be polyvinylpyrrolidone, polyacrylic acid, the one of polyacrylamide
Kind is a variety of；The solvent can play a part of dissolving, and it can be 1-METHYLPYRROLIDONE, deionized water；Further, glue
It is preferably Kynoar to tie agent；Dispersant is preferably polyvinylpyrrolidone；Solvent is preferably deionized water.The bonding agent,
The mode of the mixing of dispersant and solvent is not exposed to specific limitation, can be selected according to the actual requirements.
S2, conductive agent added to the glue, after the mixer stirs, be placed in temperature controlled ultrasonic ripple dispersion machine
Middle progress water bath with thermostatic control heating, is made pre-dispersed conductive rubber cement.
Specifically, the conductive agent that parts by weight are 2~3 is heated in glue, opens mixer and be stirred, preferably stir
It is 10rpm/min~30rpm/min to mix speed.Further, mixing speed is preferably 15rpm/min~20rpm/min；Stirring
Time is preferably 10min.Then the glue to stir is placed in temperature controlled ultrasonic ripple dispersion machine, opens heating water bath function,
Heating water bath is carried out, and controls water bath heating temperature to be constant at 25~60 DEG C.Further, the temperature of heated constant temperature is preferably 30
~40 DEG C.The speed that can accelerate wet with solvent conductive agent by heating water bath also has and drives bubble in glue away, and temperature is constant
It is then easily to cause solvent to volatilize because temperature is too high in 25~60 DEG C, temperature is too low to be unable to reach wetting effect.
Wherein, the conductive agent can be used for strengthening electric conductivity, and it can be one kind or more of conductive black, electrically conductive graphite
Kind；Further, conductive agent is preferably conductive black.
S3, the ultrasonic wave divergent function for opening the temperature controlled ultrasonic ripple dispersion machine, carry out high frequency ultrasound and disperse, be made and divide
The conductive rubber cement dissipated.
Specifically, the ultrasonic wave divergent function of the temperature controlled ultrasonic ripple dispersion machine is opened, selects the scattered frequency of ultrasonic wave；Should
Ultrasonic wave dispersion frequency can be 20kHz~80kHz；Jitter time can be 10~30 minutes.Further, the ultrasonic wavelength-division
Scattered frequency is preferably 40kHz~50kHz, and jitter time is preferably 15~20 minutes.Being disperseed by high-frequency ultrasonic wave can
Conductive agent is separated into the smaller particle of particle diameter, in order to soak the conductive agent, accelerates the conductive agent dissolution velocity.
S4, the conductive rubber cement and active material added in mixer, carry out high-speed stirred and scattered, positive pole slurry is made
Material.
Specifically, parts by weight are added in mixer again for 94~95 active material and conductive rubber cement, carried out high
Speed stirring and scattered, it be 30rpm/min~60rpm/min to select mixing speed, rate of dispersion for 1000rpm/min~
5000rpm/min.Further, the speed of stirring is preferably 40rpm/min~50rpm/min, and rate of dispersion is preferably
3000rpm/min~4000rpm/min.Stirring and jitter time are preferably 120min.
Wherein, active material can be LiFePO4, cobalt acid lithium, LiMn2O4, the one or more of ternary material；Further
Ground, the active material are preferably LiFePO4 and ternary material.
It will be illustrated below with specific embodiment.Following embodiments and comparative example are in Guangzhou good luck machinery production
Completed in 10L double planetary mixers.
Embodiment one：
Following every part of setting represents 50g；
3 parts of binding agents, 0.3 part of dispersant, 60 parts of solvents are taken, adds in mixer and is disperseed with 3000rpm/min under rotating speed
Scattered 120min forms glue；Take 2 parts of conductive blacks, add in glue, using being stirred in advance under 20rpm/min speeds of agitator
After 10min, mixed liquor is transferred in temperature controlled ultrasonic ripple dispersion machine, the ultrasound point under the conditions of 35 DEG C of temperature, ultrasonic frequency 40kHz
15min is dissipated, the conductive rubber cement formed after disperseing.Scattered conductive rubber cement is transferred in mixer, adds 95 parts of activity
Material LiFePO4, with 40rpm/min mixing speeds, 3000rpm/min rate of dispersions, positive pole is obtained after being dispersed with stirring 120min
Slurry.
Embodiment two：
Following every part of setting represents 50g；
3 parts of binding agents, 0.2 part of dispersant, 62 parts of solvents are taken, adds in mixer and is disperseed with 3000rpm/min under rotating speed
Scattered 120min forms glue；Take 2 parts of conductive blacks, add in glue, using being stirred in advance under 20rpm/min speeds of agitator
After 10min, mixed liquor is transferred in temperature controlled ultrasonic ripple dispersion machine, the ultrasound point under the conditions of 35 DEG C of temperature, ultrasonic frequency 40kHz
15min is dissipated, the conductive rubber cement formed after disperseing.Scattered conductive rubber cement is transferred in mixer, adds 95 parts of activity
Material LiFePO4, with 40rpm/min mixing speeds, 4000rpm/min rate of dispersions, positive pole is obtained after being dispersed with stirring 120min
Slurry.
Embodiment three：
Following every part of setting represents 50g；
3 parts of binding agents, 0.4 part of dispersant, 58 parts of solvents are taken, adds in mixer and is disperseed with 3000rpm/min under rotating speed
Scattered 120min forms glue；2 parts of conductive blacks, 1 part of electrically conductive graphite are taken, is added in glue, using 20rpm/min speeds of agitator
After lower pre- stirring 10min, mixed liquor is transferred in temperature controlled ultrasonic ripple dispersion machine, in 40 DEG C of temperature, ultrasonic frequency 50kHz conditions
Lower ultrasonic disperse 20min, the conductive rubber cement formed after disperseing.Scattered conductive rubber cement is transferred in mixer, adds 94
The active compound lithium iron phosphate of part, with 40rpm/min mixing speeds, 4000rpm/min rate of dispersions, after being dispersed with stirring 120min
Obtain anode sizing agent.
Example IV：
3 parts of binding agents, 0.5 part of dispersant, 56 parts of solvents are taken, adds in mixer and is disperseed with 3000rpm/min under rotating speed
Scattered 120min forms glue；2 parts of conductive blacks, 1 part of electrically conductive graphite are taken, is added in glue, using 20rpm/min speeds of agitator
After lower pre- stirring 10min, mixed liquor is transferred in temperature controlled ultrasonic ripple dispersion machine, in 40 DEG C of temperature, ultrasonic frequency 50kHz conditions
Lower ultrasonic disperse 20min, the conductive rubber cement formed after disperseing.By scattered conductive rubber cement into mixer, 94 parts are added
Active compound lithium iron phosphate, with 40rpm/min mixing speeds, 4000rpm/min rate of dispersions, obtained after being dispersed with stirring 120min
Anode sizing agent.
Comparative example one：
Following every part of setting represents 50g；
3 parts of binding agents, 100 parts of solvents are taken, adds in mixer and scattered 120min shapes under rotating speed is disperseed with 3000rpm/min
Into glue；2 parts of conductive blacks, 1 part of electrically conductive graphite are taken, adds in glue, rotating speed and 40rpm/min is disperseed with 4000rpm/min
120min is dispersed with stirring under mixing speed and forms conductive rubber cement.94 parts of active compound lithium iron phosphate is added, is stirred with 40rpm/min
Speed is mixed, 4000rpm/min rate of dispersions, anode sizing agent is obtained after being dispersed with stirring 120min.
The contrast of the technique and product quality of embodiment one, two, three, four and comparative example one is summarized as follows table.
| Group | Total incorporation time | Slurry fineness | Conducting resinl D50 | Slurry viscosity | Solvent usage amount |
| Embodiment one | 265min | 5~6um | 24.3um | 7600 | 3000g |
| Embodiment two | 265min | 6~7um | 25.0um | 8100 | 3100g |
| Embodiment three | 270min | 5~7um | 24.8um | 7500 | 2900g |
| Example IV | 270min | 5~6um | 24.6um | 6800 | 2800g |
| Comparative example one | 360min | 8~9um | 35.5um | 9200 | 5000g |
From the experimental results, the fineness for the slurry that embodiment is drawn and the fineness of conducting resinl are superior to comparative example, are mixed always
Time shortening 1.5h is closed, under conditions of slurry viscosity is lower, the usage amount of solvent is less, improves efficiency, reduces again molten
Agent dosage.
It should be understood that above example only expresses the preferred embodiment of the present invention, it describes more specific and detailed
Carefully, but the limitation to the scope of the claims of the present invention therefore can not be interpreted as；It should be pointed out that the common skill for this area
For art personnel, without departing from the inventive concept of the premise, independent assortment can be carried out to above-mentioned technical characterstic, can also done
Go out several modifications and improvements, these belong to protection scope of the present invention；Therefore, it is all to be done with scope of the invention as claimed
Equivalents and modification, the covering scope of the claims in the present invention all should be belonged to.
Claims (10)
1. a kind of preparation method of lithium ion battery anode glue size, it is characterised in that comprise the following steps：
S1, binding agent, dispersant and solvent are added to the scattered obtained glue of progress high speed in mixer；
S2, conductive agent added to the glue, after the mixer stirs, be placed in temperature controlled ultrasonic ripple dispersion machine
Row water bath with thermostatic control is heated, and pre-dispersed conductive rubber cement is made；
S3, the ultrasonic wave divergent function for opening the temperature controlled ultrasonic ripple dispersion machine, carry out high frequency ultrasound and disperse, be made scattered
Conductive rubber cement；
S4, the conductive rubber cement and active material added in mixer, carry out high-speed stirred and scattered, anode sizing agent is made.
2. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that the binding agent,
The dispersant, the solvent, the conductive agent, the parts by weight of the active material are respectively：The bonding agent 2.5~3,
The dispersant 0.2~0.5, the solvent 56~62, the conductive agent 2~3, the active material 94~95.
3. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in the S1 steps
In, the binding agent is Kynoar, polytetrafluoroethylene (PTFE), butadiene-styrene rubber, the one or more of sodium carboxymethylcellulose.
4. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in the S1 steps
In, the dispersant is polyvinylpyrrolidone, polyacrylic acid, the one or more of polyacrylamide.
5. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in the S1 steps
In, the solvent is 1-METHYLPYRROLIDONE, deionized water.
6. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in the S2 steps
In, the conductive agent is conductive black, the one or more of electrically conductive graphite.
7. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in the S2 steps
In, control the temperature of the heating water bath process to be constant at 25~60 DEG C.
8. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in the S3 steps
In, the ultrasonic wave high-frequency dispersion frequency control is 20kHz~80kHz, and jitter time control is 10~30 minutes.
9. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that in S4 steps,
The active material is LiFePO4, cobalt acid lithium, LiMn2O4, the one or more of ternary material.
10. the preparation method of lithium ion battery anode glue size according to claim 1, it is characterised in that walked in the S1
In rapid, the speed of the high-speed stirred is 30rpm/min~60rpm/min；In the S2 steps, the mixing speed is
10rpm/min~30rpm/min；In the S4 steps, the speed of the high-speed stirred is 30rpm/min~60rpm/min,
The scattered speed of the high speed is 1000rpm/min~5000rpm/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108923059A (en) * | 2018-05-18 | 2018-11-30 | 远东福斯特新能源有限公司 | Promote the method and its ternary lithium ion battery of ternary cycle performance of lithium ion battery |
| CN109786661A (en) * | 2019-01-14 | 2019-05-21 | 天能电池集团有限公司 | A kind of lithium battery pole slice and its preparation method and application of full-filling conductive agent |
| CN109904456A (en) * | 2019-03-11 | 2019-06-18 | 重庆市紫建电子有限公司 | A kind of preparation method of lithium ion battery oily cathode slurry |
| CN111477848A (en) * | 2020-04-13 | 2020-07-31 | 江苏中兴派能电池有限公司 | Electrode and battery prepared from cathode water system conductive slurry |
| CN111628175A (en) * | 2020-06-05 | 2020-09-04 | 淮北市吉耐新材料科技有限公司 | Conductive slurry based on carbon nano tube and preparation process thereof |
| CN112121660A (en) * | 2020-08-26 | 2020-12-25 | 风帆有限责任公司 | Method for preparing anode slurry of lithium ion battery |
| CN112234198A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery anode slurry and preparation method thereof |
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| CN114420930A (en) * | 2021-12-23 | 2022-04-29 | 山东精工电子科技有限公司 | Dispersing method of conductive agent in lithium ion battery slurry and lithium ion battery slurry |
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| CN112121660A (en) * | 2020-08-26 | 2020-12-25 | 风帆有限责任公司 | Method for preparing anode slurry of lithium ion battery |
| CN112234198A (en) * | 2020-09-15 | 2021-01-15 | 深圳市拓邦锂电池有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN113328097A (en) * | 2021-07-06 | 2021-08-31 | 深圳一特科技有限公司 | Improved conductive glue solution for lithium ion battery anode and preparation method and application thereof |
| CN114420930A (en) * | 2021-12-23 | 2022-04-29 | 山东精工电子科技有限公司 | Dispersing method of conductive agent in lithium ion battery slurry and lithium ion battery slurry |
| CN114447337A (en) * | 2022-02-11 | 2022-05-06 | 湖北亿纬动力有限公司 | Conductive adhesive of negative electrode slurry and preparation method and application thereof |
| CN114447337B (en) * | 2022-02-11 | 2023-09-01 | 湖北亿纬动力有限公司 | Conductive adhesive of negative electrode slurry, and preparation method and application thereof |
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Application publication date: 20180119 |