CN107403914A - A kind of dry mixing process of artificial plumbago negative pole slurry - Google Patents
A kind of dry mixing process of artificial plumbago negative pole slurry Download PDFInfo
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The present invention relates to a kind of dry mixing process of artificial plumbago negative pole slurry, it is characterised in that the technique includes：(1) Delanium, conductive black, sodium carboxymethylcellulose (CMC) are added into agitator tank, dry-mixed 10~30min together；(2) deionized water is added, stirs 60~120min；(3) deionized water is added, stirs 60~120min；(4) SBR emulsion (SBR) is added, stirs 30~60min；(5) deaeration is inverted；(6) detection adjustment slurry parameter, slurry preparation is completed, the weight of deionized water in the step (2) is the 30%~60% of Delanium weight, and the weight of the deionized water in the step (3) is the 30%~70% of Delanium weight.Artificial plumbago negative pole slurry good dispersion made from the stirring technique of the present invention, uniformity are excellent.
Description
Technical field
The invention belongs to the dry-mixed work in lithium ion battery technology field, more particularly to a kind of artificial plumbago negative pole slurry
Skill.
Background technology
The conventional negative material of lithium ion battery includes Delanium, native graphite or carbonaceous mesophase spherules etc., wherein
Delanium has good cycle, good rate capability, specific capacity height, good conductivity, good to the selectivity of electrolyte, and price is just
The advantages that suitable, it is the most frequently used negative material of current lithium battery industry, but artificial plumbago negative pole slurry bad dispersibility, uniformity
Difference, the performance of lithium ion battery can be had a strong impact on.Prepared by traditional cathode size is all to use wet-mixing, i.e., first gluing (is matched somebody with somebody
Polymer Solution processed), then active material and conductive agent are sequentially added into mixing, it is eventually adding adhesive and disperses, this method prepares negative
Pole slurry, required time length, utilization rate of equipment and installations is low, and production capacity is relatively low, and slurry dispersiveness and uniformity are poor.In order to improve people
The dispersiveness and uniformity of graphite cathode slurry are made, dry mixing process turns into study hotspot, and so-called dry mixing process is：By active matter
The powder material such as matter and conductive agent is dry-mixed, then adds solvent mixing, because powder does not have toughness, stirring resistance when dry powder stirs
Power is smaller to be easier to stir, and dry powder is stirring evenly and then adding into solvent, and mixing is easily uniform, but current dry mixing process
Still cathode size dispersiveness and uniformity difference can not be solved the problems, such as.
Patent CN101127394A discloses a kind of lithium secondary battery anode and its manufacture method containing graphite, this method
Including：(1) the 50%~90% of binding agent and total solvent is placed in mixer and stirred；(2) by native graphite and artificial
Graphite is dry-mixed in de-airing mixer, then divides 2~3 batches to add binding agent glue prepared by 10%~80% step 1 and stir equal
It is even；(3) add SBR and stir；(4) add binding agent glue prepared by remaining step 1 and stir；(5) 1~3 is divided
Criticize and add remaining solvent and stir；(6) slurry vacuumizes, sieved, completing the preparation of slurry.Although the patent will be natural
Graphite and Delanium have carried out dry-mixed, but add the stirring of binding agent glue, whole material toughness increase, stir resistance liter
Height, the easy conglomeration of dry powder is difficult to be well mixed, and is unfavorable for the improvement of slurry dispersiveness and uniformity.
Patent CN106159266 A disclose a kind of cathode size preparation method for reducing lithium ion battery expansion, the party
Method comprises the following steps：(1) it is negative electrode active material and conductive agent is pre- dry-mixed；(2) sodium carboxymethylcellulose is dissolved in deionized water,
Obtain the CMC glues that concentration is 1.0-2.0%；(3) part CMC glues are added to negative electrode active material, conductive agent compound
In, high-speed stirred；(4) remaining CMC glues, high-speed stirred are added；(5) modified SBR binding agents, moderate-speed mixer are added, regulation is glued
Degree, homogenate, sieving.Although the patent is pre- dry-mixed by negative electrode active material and conductive agent, the stirring of binding agent glue is added, entirely
Material toughness increases, and stirring resistance rise, the easy conglomeration of dry powder is difficult to be well mixed, and is unfavorable for slurry dispersiveness and uniformity
Improvement.
Patent CN106654153 A disclose pulp of lithium ion battery and close paste-making method, and the conjunction paste-making method includes following step
Suddenly：Active material, binding agent and conductive agent is dry-mixed；Add 30-35wt% solvent mixing；Add 35-40wt% solvent
Mixing；Add the remaining solvent mixing.Although the patent improves slurry equality, but when adding solvent several times,
Slurry experienced the whipping process from high viscosity to low viscosity, in this process, the easy conglomeration of slurry, stick bucket in agitator tank
Bottom or bucket wall.
Patent CN104638229A discloses a kind of dry-mixed hard refining Preparation Method of power train in vehicle application lithium ion battery electrode sizing agent,
Addition agitator tank is dry-mixed together in proportion after electrode active material, conductive agent and binding agent are dried in the invention, then to stirring
A part of solvent is added in tank, is stirred, finally adds stirring solvent several times, above-mentioned technique improves the stability of slurry
With uniformity and stock utilization and operating efficiency, but when adding solvent several times, slurry experienced from high viscosity to low
The whipping process of viscosity, in this process, the easy conglomeration of slurry, stick in the bucket bottom of agitator tank or bucket wall.
Patent CN105489844A discloses a kind of preparation method of lithium ion power cell cathode slurry, and this method uses
Batch mixing order：(1) active material and conductive agent high-speed stirred are dry-mixed；(2) dispersant is added, with the black obtained by step (1)
Powder is dry-mixed；(3) solvent is added, leads to condensed water, high-speed stirred is disperseed after stirring at low speed；Frictioning, vacuumize, continue high-speed vacuum
Mixing；(4) binding agent, dispersion mixing are added.The invention production efficiency is high, improves the stability and uniformity of slurry, still
Disposable to add solvent, the quantity of solvent in agitator tank is excessive, and active material, conductive agent and dispersant can not be stirred into dough
Shape, into sposh shape, slurry is easily sticked to bucket bottom or the bucket wall of agitator tank, so as to cause slurry dispersiveness and uniformity to be deteriorated.
The content of the invention
In order to solve the problems, such as artificial plumbago negative pole slurry bad dispersibility, uniformity difference, the present invention proposes a kind of artificial stone
The dry mixing process of black cathode size.
The present invention adopts the technical scheme that to solve the above problems：
A kind of dry mixing process of artificial plumbago negative pole slurry, it is characterised in that the technique includes：
(1) Delanium, conductive black, sodium carboxymethylcellulose (CMC) are added into agitator tank together, mixing speed is set
For 5~30Hz, rate of dispersion is 50~300 revs/min, dry-mixed 10~30min；
(2) deionized water is added, setting mixing speed is 10~40Hz, and rate of dispersion is 100~600 revs/min, stirring
60~120min；
(3) deionized water is added, setting mixing speed is 10~40Hz, and rate of dispersion is 100~600 revs/min, stirring
60~120min；
(4) add SBR emulsion (SBR), settings mixing speed is 10~40Hz, rate of dispersion for 500~800 turns/
Minute, stir 30~60min；
(5) deaeration is inverted, setting mixing speed is 5~20Hz, stirs 10~50min；
(6) slurry viscosity, fineness and solid content are detected, adjusts slurry viscosity value, slurry preparation is completed；
The weight of deionized water in step (2) is the 30%~60% of Delanium weight.
Preferably, the weight of the deionized water in the step (2) is the 40%~50% of Delanium weight.
The weight of deionized water in step (3) is the 30%~70% of Delanium weight.
Slurry viscosity value is 2000~5000mPas in step (6), slurry fineness≤30um, solid content is 45~
55%.
A kind of lithium ion battery, the cathode size in lithium ion battery are prepared using above-mentioned technique.
The battery capacity tolerance of above-mentioned lithium ion battery is ± 2Ah, and internal resistance tolerance is ± 0.1m Ω.
The beneficial effects of the invention are as follows：Delanium, conductive black and CMC add dry-mixed in agitator tank together so that CMC
It is well mixed with Delanium, conductive black, CMC thickening peptizaiton can be given full play to；A certain amount of go is added after dry-mixed
Ionized water so that the dry powder in some corners such as the bucket wall of powder especially agitator tank and bucket bottom is kneaded into dough, is solved and is stirred
Mix the problem of dry powder in some corners such as bucket wall and the bucket bottom of tank is difficult to be stirred；Remaining deionized water disposably adds
Enter, be directly entered low viscosity stirring, avoid from high viscosity and conglomeration occur into low viscosity whipping process, be stained with the phenomenon of wall, this
Artificial plumbago negative pole slurry good dispersion is made in invention, and uniformity is excellent.
Embodiment
In order to solve the problems, such as artificial plumbago negative pole slurry bad dispersibility, uniformity difference, the present invention proposes a kind of artificial stone
The dry mixing process of black cathode size.The present invention is expanded on further with reference to specific embodiment.It should be appreciated that this specification
Described in specific embodiment merely to explain the present invention, be not intended to limit the present invention.
The main material used in comparative example and embodiment is lithium battery industry common used material.
Pass through the fluctuation range of this five parameters of the internal resistance of the viscosity of slurry, fineness, solid content, the capacity of battery and battery
To represent the dispersiveness of slurry and uniformity.
Viscosity in following comparative examples and embodiment uses viscosity meter.
Fineness in following comparative examples and embodiment is measured using Hegman grind gage.
The measurement of solid content in following comparative examples and embodiment：A certain amount of slurry is taken to claim its weight in wet base, then drying claims
Dry weight, the ratio between dry weight and weight in wet base are solid content.
Obtained battery carries out volume test, specific method of testing according to GB/T18287 in following comparative examples and embodiment
For：
Capacity is tested to obtain by battery testing cabinet.Under conditions of 20 DEG C ± 5 DEG C, charged with 1C, work as battery-end
When voltage reaches 3.65V, constant-voltage charge is changed to, stops charging until charging current is equal to 0.01C, 0.5~1h is shelved, 20.C
Under conditions of ± 5 DEG C, with 1C current discharges to 2.0V.
Internal resistance in following comparative examples and embodiment is tested and obtained using battery test system.
Embodiment 1
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 108kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 80min；(3) 220kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is
500 revs/min, stir 80min；(4) 23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min,
Stir 40min；(5) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(6) detect slurry viscosity value be 2000~
5000mPas, slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Embodiment 2
Except that, the addition of deionized water is 144kg in step (2) with embodiment 1.
Embodiment 3
Except that, the addition of deionized water is 180kg in step (2) with embodiment 1.
Embodiment 4
Except that, the addition of deionized water is 216kg in step (2) with embodiment 1.
Comparative example 1
Except that, the addition of deionized water is 90kg in step (2) with embodiment 1.
Comparative example 2
Except that, the addition of deionized water is 234kg in step (2) with embodiment 1.
Cathode size prepared by embodiment 1~4 and comparative example 1,2 was surveyed into a viscosity, fineness every 2 hours and contained admittedly
Amount, survey 10 times altogether, record fluctuation range, cathode size prepared by embodiment 1~4 and comparative example 1,2 is coated, roller
Negative plate is obtained after pressure, section, by negative plate and barrier film and positive pole winding, enters shell, fluid injection, sealing, lithium ion battery is made, each
Embodiment and comparative example respectively take 10 batteries, test its capacity and internal resistance, record fluctuation range.Table 1 is embodiment 1~4 and ratio
Compared with deionized water addition in step (2) in example 1,2, table 2 is deionized water addition in step (2) to slurry dispersiveness and one
The influence of cause property.
Deionized water addition in the step of table 1 (2)
Influence of the deionized water addition to slurry dispersiveness and uniformity in the step of table 2 (2)
As known from Table 2, when the addition of deionized water is the 30%~60% of Delanium weight in step (2), slurry
Viscosity, the fluctuation range of fineness and solid content it is small, slurry point small with battery capacity made of the slurry and internal resistance fluctuation range
Scattered property is good, and uniformity is good.From embodiment 1 to 4 as can be seen that when the addition of deionized water is 40~50% in step (2),
The addition that slurry dispersiveness and uniformity are better than deionized water in step (2) is 30~60%；From embodiment 2 and comparative example 1,
Comparative example 2 as can be seen that the deionized water added in step (2) is very few or the excessive dispersiveness for being all unfavorable for slurry with it is consistent
Property, because the deionized water added is very few, the amount of liquid in agitator tank is less, and dry powder can not be all kneaded into dough,
The dry powder in some corners such as bucket wall and the bucket bottom of agitator tank is caused to stir, the deionized water of addition is excessive, agitator tank
In amount of liquid it is too many, dry powder can not be kneaded into dough, and into sposh shape, slurry is easily sticked to bucket bottom or the bucket of agitator tank
Wall, so as to cause slurry dispersiveness and uniformity to be deteriorated.
Embodiment 5
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 162kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 80min；(3) 220kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is
500 revs/min, stir 80min；(4) 23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min,
Stir 40min；(5) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(6) detect slurry viscosity value be 2000~
5000mPas, slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Comparative example 3
(1) 360kg Delaniums, 6kg conductive blacks are added into agitator tank, setting mixing speed is 20Hz, rate of dispersion
For 200 revs/min, dry-mixed 25min；(2) 8kg CMC are added, setting mixing speed is 20Hz, and rate of dispersion is 200 revs/min
Clock, dry-mixed 25min；(3) 162kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, is stirred
Mix 80min；(4) 220kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, stirring
80min；(5) 23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min, stirs 40min；(6) it is anti-
Turn deaeration, setting mixing speed is 15Hz, stirs 30min；(7) detection slurry viscosity value is 2000~5000mPas, slurry
Fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Cathode size prepared by embodiment 5 and comparative example 3 was surveyed into a viscosity, fineness and solid content every 2 hours, altogether
Survey 10 times, record fluctuation range, cathode size prepared by embodiment 5 and comparative example 3 is coated, roll-in, must be born after section
Pole piece, by negative plate and barrier film and positive pole winding, enter shell, fluid injection, sealing, be made lithium ion battery, each embodiment and compare
Example respectively takes 10 batteries, tests its capacity and internal resistance, records fluctuation range.Table 3 is the addition of CMC in embodiment 5 and comparative example 3
Sequentially, influence of the addition sequence that table 3 is CMC to slurry dispersiveness and uniformity.
The CMC of table 3 addition sequence
| Embodiment 5 | Comparative example 3 | |
| CMC addition sequences | CMC and Delanium, conductive black add together | CMC adds in Delanium and the latter step of conductive black |
Influence of the CMC of table 4 addition sequence to slurry dispersiveness and uniformity
From table 4, it can be seen that CMC and Delanium, conductive black add agitator tank together when being stirred, slurry disperses
Property and uniformity are good.From embodiment 5 and comparative example 3 as can be seen that CMC is added and stirred in Delanium and the latter step of conductive black
When mixing tank and being stirred, slurry viscosity 3360~3428mPas of fluctuation range, fineness fluctuation range is 17~25um, solid content
Fluctuation range is 49.6~51.25%, and battery capacity fluctuation range be 48.8~51.7Ah, internal resistance fluctuation range for 0.44~
0.73m Ω, because CMC is a kind of additive with thickening and peptizaiton, CMC is after Delanium and conductive black
One step adds, it is impossible to is sufficiently well mixed with Delanium and conductive black, then when adding deionized water below, CMC
Thickening peptizaiton well cannot be played after dissolving expansion.
Embodiment 6
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 162kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 80min；(3) 210kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is
500 revs/min, stir 90min；(4) 23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min,
Stir 40min；(5) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(6) detect slurry viscosity value be 2000~
5000mPas, slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Comparative example 4 (is derived from patent CN104638229A)
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 162kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 80min；(3) 70kg deionized waters are added, setting mixing speed is 30Hz, rate of dispersion 500
Rev/min, stir 30min；(4) repeat step (3) is secondary；(5) 23kg SBR are added, setting mixing speed is 30Hz, is disperseed
Speed is 600 revs/min, stirs 40min；(6) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(7) detection slurry
Material viscosity number is 2000~5000mPas, and slurry fineness≤30um, solid content is 45~55%, and material, which is prepared, to be completed.
Comparative example 5 (is derived from patent CN106654153 A)
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 162kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 80min；(3) 105kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is
500 revs/min, stir 45min；(4) repeat step (3) is once；(5) 23kg SBR are added, setting mixing speed is 30Hz, point
It is 600 revs/min to dissipate speed, stirs 40min；(6) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(7) detect
Slurry viscosity value is 2000~5000mPas, and slurry fineness≤30um, solid content is 45~55%, and material, which is prepared, to be completed.
Comparative example 6 (is derived from patent CN105489844A)
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 372kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 170min；(3) 23kg SBR are added, settings mixing speed is 30Hz, rate of dispersion for 600 turns/
Minute, stir 40min；(4) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(5) detection slurry viscosity value is
2000~5000mPas, slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Cathode size prepared by embodiment 6 and comparative example 4~6 was surveyed into a viscosity, fineness and solid content every 2 hours,
Survey 10 times altogether, record fluctuation range, cathode size prepared by embodiment 6 and comparative example 4~6 is coated, roll-in, section
Negative plate is obtained afterwards, by negative plate and barrier film and positive pole winding, enters shell, fluid injection, sealing, lithium ion battery, each embodiment is made
10 batteries are respectively taken with comparative example, test its capacity and internal resistance, record fluctuation range.Table 5 is in embodiment 6 and comparative example 4~6
The feed postition of deionized water, table 6 are influence of the feed postition of deionized water to slurry dispersiveness and uniformity.
The feed postition of the deionized water of table 5
Influence of the feed postition of the deionized water of table 6 to slurry dispersiveness and uniformity
As can be seen from Table 6, a part of deionized water is first added after dry-mixed, when remaining deionized water disposably adds,
Slurry good dispersion, uniformity are good.From embodiment 6 and comparative example 4,5 as can be seen that first adding a part of deionization after dry-mixed
Water, remaining deionized water is in three times or during secondary addition, and slurry dispersiveness and uniformity are substantially deteriorated, because several times
When adding deionized water, slurry experienced the whipping process from high viscosity to low viscosity, and in this process, slurry is easily tied
Group, stick in the bucket bottom of agitator tank or bucket wall；From embodiment 6 and comparative example 6 as can be seen that disposable after dry-mixed add deionization
During water, slurry dispersiveness and uniformity are also substantially to be deteriorated, because, it is disposable after dry-mixed to add deionized water, agitator tank
In amount of liquid it is too many, dry powder can not be kneaded into dough, and into sposh shape, slurry is easily sticked to bucket bottom or the bucket of agitator tank
Wall, so as to cause slurry dispersiveness and uniformity to be deteriorated.
Embodiment 7
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums, 6kg conductive blacks, 8kg CMC being added into agitator tank, setting mixing speed is 20Hz,
Rate of dispersion is 200 revs/min, dry-mixed 25min；(2) 162kg deionized waters are added, setting mixing speed is 30Hz, disperses speed
Spend for 500 revs/min, stir 80min；(3) 215kg deionized waters are added, setting mixing speed is 30Hz, and rate of dispersion is
500 revs/min, stir 80min；(4) 23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min,
Stir 40min；(5) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(6) detect slurry viscosity value be 2000~
5000mPas, slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Comparative example 7 (is derived from patent CN101127394A)
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 8kg CMC and 300kg deionized water are first added into mixer, setting mixing speed is 20Hz, and rate of dispersion is
300 revs/min, stir 60min；(2) 360kg Delaniums and 6kg conductive blacks are placed in agitator tank, setting mixing speed is
20Hz, rate of dispersion are 250 revs/min, dry-mixed 60min；(3) the 15% of the CMC glues for preparing step (1) adds step
(2) in dry powder, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, stirs 60min, adds step (1) system
The 40% of standby CMC glues, setting mixing speed are 30Hz, and rate of dispersion is 500 revs/min, stirs 60min；(4) add
23kg SBR, setting mixing speed are 30Hz, and rate of dispersion is 600 revs/min, stirs 30min；(5) prepared by step (1)
The 45% of CMC glues is added in the slurry of step (4), and setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, stirring
60min；(6) 77kg deionized waters are added into de-airing mixer, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min
Clock, stir 90min；(7) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(8) it is 2000 to detect slurry viscosity value
~5000mPas, slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Comparative example 8 (embodiment 1 for selecting from patent CN106159266 A)
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) it is Delanium is pre- dry-mixed with conductive black Sp；(2) sodium carboxymethylcellulose is dissolved in deionized water, obtains dense
Spend the CMC glues for 1.0%；(3) the CMC glues that 10% is made in (2) are added in compound, sets rotation rotating speed
4000rpm, revolve round the sun rotating speed 64rpm, stirs 0.5h；(4) the CMC glues of residue 90% are added, set rotation rotating speed 4000rpm,
Revolve round the sun rotating speed 64rpm, stirs 3h；(5) modified SBR binding agents (modified SBR binding agents mass percent in cathode size is added
Content is 3%), to set rotation rotating speed 2000rpm, and revolve round the sun rotating speed 40rpm, stirs 0.3h；(6) viscosity, homogenate, sieving are adjusted.
Comparative example 9 (is derived from patent CN106159266 A)
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 360kg Delaniums and 6kg conductive blacks are placed in agitator tank, setting mixing speed is 20Hz, rate of dispersion
For 250 revs/min, dry-mixed 20min；(2) 8kg CMC and 377kg deionized water are first added into mixer, setting mixing speed is
20Hz, rate of dispersion are 300 revs/min, stir 60min；(3) the 10% of the CMC glues for preparing step (1) adds step
(2) in dry powder, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, stirs 30min；(4) by remaining CMC glue
Liquid is added in the slurry of step (3), and setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, stirs 270min；(5)
23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min, stirs 20min；(6) deaeration is inverted, if
It is 15Hz to put mixing speed, stirs 30min；(7) detection slurry viscosity value is 2000~5000mPas, slurry fineness≤
30um, solid content are 45~55%, and material, which is prepared, to be completed.
Comparative example 10
A kind of artificial plumbago negative pole slurry, it is made by technique stirred below, the technique includes：
(1) 8kg CMC and 377kg deionized water are first added into agitator tank, setting mixing speed is 20Hz, and rate of dispersion is
300 revs/min, stir 80min；(2) 6kg conductive blacks are added, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min
Clock, stir 80min；(3) 360kg Delaniums are added, setting mixing speed is 30Hz, and rate of dispersion is 500 revs/min, is stirred
Mix 150min；(4) 23kg SBR are added, setting mixing speed is 30Hz, and rate of dispersion is 600 revs/min, stirs 40min；
(5) deaeration is inverted, setting mixing speed is 15Hz, stirs 30min；(6) it is 2000~5000mPas to detect slurry viscosity value,
Slurry fineness≤30um, solid content are 45~55%, and material, which is prepared, to be completed.
Cathode size prepared by embodiment 7 and comparative example 7~10 was surveyed into a viscosity, fineness and solid content every 2 hours,
Survey 10 times altogether, record fluctuation range, cathode size prepared by embodiment 7 and comparative example 7~10 is coated, roll-in, cut
Negative plate is obtained after piece, by negative plate and barrier film and positive pole winding, enters shell, fluid injection, sealing, lithium ion battery is made, it is each to implement
Example and comparative example respectively take 10 batteries, test its capacity and internal resistance, record fluctuation range.Table 7 be embodiment 7 and comparative example 7~
Slurry agitation mode in 10, table 8 are the influence for going slurry agitation mode to slurry dispersiveness and uniformity.
The slurry agitation mode of table 7
Influence of the slurry agitation mode of table 8 to slurry dispersiveness and uniformity
As can be seen from Table 8, the slurry good dispersion prepared using the stirring technique of the present invention, uniformity are excellent.From reality
Example 7 and comparative example 7~9 are applied as can be seen that CMC glues are added in Delanium and conductive black when being dispersed with stirring, slurry point
It is also substantially to be deteriorated to dissipate property and uniformity, because, CMC glues are added in dry powder, whole material toughness increase, stirring resistance
Power raises, and the easy conglomeration of dry powder is difficult to be well mixed, so as to cause slurry dispersiveness and uniformity to be deteriorated；From embodiment 7 and ratio
Compared with example 10 as can be seen that the slurry viscosity prepared using common wet mixing agitating mode, fineness and solid content fluctuation range are big, with this
The capacity and internal resistance fluctuation range of battery prepared by slurry are big, and slurry dispersiveness and uniformity are excessively poor, because, it is common wet
Mixed technique is to sequentially add negative electrode active material and conductive agent in CMC glues to be dispersed with stirring, negative electrode active material and conductive agent
Can not fully it mix, the material toughness in whole mixing plant is big, and the easy conglomeration of material is difficult to be well mixed, and causes slurry point
Dissipate property and uniformity is poor.
Claims (6)
1. a kind of dry mixing process of artificial plumbago negative pole slurry, it is characterised in that the technique includes：
(1) Delanium, conductive black, sodium carboxymethylcellulose (CMC) are added into agitator tank together, it is 5 to set mixing speed
~30Hz, rate of dispersion are 50~300 revs/min, dry-mixed 10~30min；
(2) deionized water is added, setting mixing speed is 10~40Hz, and rate of dispersion is 100~600 revs/min, stirring 60~
120min；
(3) deionized water is added, setting mixing speed is 10~40Hz, and rate of dispersion is 100~600 revs/min, stirring 60~
120min；
(4) SBR emulsion (SBR) is added, setting mixing speed is 10~40Hz, and rate of dispersion is 500~800 revs/min
Clock, stir 30~60min；
(5) deaeration is inverted, setting mixing speed is 5~20Hz, stirs 10~50min；
(6) slurry viscosity, fineness and solid content are detected, adjusts slurry viscosity value, slurry preparation is completed；
The weight of deionized water in step (2) is the 30%~60% of Delanium weight.
2. the dry mixing process of a kind of artificial plumbago negative pole slurry according to claim 1, it is characterised in that in step (2)
Deionized water weight be Delanium weight 40%~50%.
3. the dry mixing process of a kind of artificial plumbago negative pole slurry according to claim 1, it is characterised in that in step (3)
Deionized water weight be Delanium weight 30%~70%.
4. the dry mixing process of a kind of artificial plumbago negative pole slurry according to claim 1, it is characterised in that in step (6)
Slurry viscosity value is 2000~5000mPas, and slurry fineness≤30um, solid content is 45~55%.
5. a kind of lithium ion battery, it is characterised in that the cathode size in lithium ion battery uses claim 1-4 any one
It is prepared by described technique.
6. lithium ion battery according to claim 5, its battery capacity tolerance is ± 2Ah, and internal resistance tolerance is ± 0.1m Ω.
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Denomination of invention: Dry mixing process of an artificial graphite cathode paste Effective date of registration: 20221024 Granted publication date: 20200818 Pledgee: Jiangxi Guangxin Rural Commercial Bank Co.,Ltd. Pledgor: JIANGXI ANC NEW ENERGY TECHNOLOGY Co.,Ltd. Registration number: Y2022980019421 |