CN108987715A - A kind of lithium ion battery anode slurry and preparation method thereof - Google Patents
A kind of lithium ion battery anode slurry and preparation method thereof Download PDFInfo
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- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The present invention provides a kind of lithium ion battery anode slurry and preparation method thereof, 50-60 parts of expanded graphite, manganese dioxide -40-50 parts of mangano-manganic oxide composite material, 0.5-2 parts of conductive black, 1.5-3 parts of polyalcohol, 2.2-2.5 parts of butadiene-styrene rubber, 4-5.5 parts of carboxymethyl cellulose and 110-130 parts of deionized water.Compared with prior art, the present invention controls the selection of raw material, amount ratio, charging sequence and mixing time, speed in preparation process etc., it prevents from reuniting, condense and agglomerating, be conducive to improve first discharge specific capacity, can achieve 902mAh/g, 1000 90% or more circulation conservation rates.
Description
Technical field
The invention belongs to battery material fields, and in particular to a kind of lithium ion battery anode slurry and preparation method thereof.
Background technique
In recent years, lithium ion battery is extensive on portable device and power battery with its superior chemical property
Using.Lithium ion battery is a kind of rechargeable battery, it relies primarily on lithium ion, and movement carrys out work between a positive electrode and a negative electrode.It is filling
In discharge process, Li+Insertion and deintercalation back and forth between two electrodes: when charging, Li+From positive deintercalation, it is embedded in by electrolyte
Cathode, cathode are in lithium-rich state；It is then opposite when electric discharge.
The cathode of lithium ion battery is by carbon element or non-carbon material, adhesive and additive mixing system
Copper foil two sides are uniformly applied at paste adhesive, through drying, are rolled.
Cyclical stability and the specific capacity etc. for improving negative electrode of lithium ion battery are that main field of lithium ion battery is important at present
One of research topic.
Summary of the invention
The purpose of the present invention is to provide a kind of lithium ion battery anode slurries, utilize expanded graphite ,-four oxygen of manganese dioxide
Change three manganese composite materials, improve the electric conductivity and cyclicity of Electrode Negative slurry, CMC, butadiene-styrene rubber and polyalcohol conduct is added
Binder prevents negative electrode slurry from reuniting, and agglomeration improves cathode stability and safety.
Another object of the present invention is to provide a kind of preparation methods of lithium ion battery anode slurry, control adding for raw material
Enter sequence, mixing speed, improves caking property, prevent negative electrode slurry from reuniting.
Specific technical solution of the present invention is as follows:
A kind of lithium ion battery anode slurry, including following raw material:
The polyalcohol is selected from glycerol or ethylene glycol.
The manganese dioxide-mangano-manganic oxide composite material preparation method, comprising the following steps:
A, after mixing liquor potassic permanganate and manganese sulfate solution, polyalcohol is added under ultrasound condition, mixes, must mix molten
Liquid；
B, CTAB and ammonium hydroxide is added in the mixed system prepared to step A, after mixing, sealing, heating reaction；Reaction terminates
Afterwards, wash, it is dry, be cooled to room temperature to get.
Further, the molar ratio of potassium permanganate and manganese sulfate is 1:10-12 in step A mixed solution.
The volume ratio of the mixed solution and polyalcohol of liquor potassic permanganate and manganese sulfate solution is 9-13:0.8- in step A
1.5。
Polyalcohol described in step A is selected from ethylene glycol or glycerine.
Preferably, in step A be added polyalcohol after ultrasonic disperse 20-30min.
After CTAB and ammonium hydroxide is added in step B, potassium permanganate concentration is 0.001-0.05mol/L, permanganic acid in system
The molar ratio of ammonia is 1:2-3:4-7 in potassium, CTAB and ammonium hydroxide.
Heating reaction described in step B, which refers to, reacts 8-18h under the conditions of 150-165 DEG C.
Prepared manganese dioxide-mangano-manganic oxide composite material, it is of uniform size, it is the nanorod structure of nano-scale,
Nanorod diameter 5-80nm, length 50-1000nm.
A kind of preparation method of lithium ion battery anode slurry provided by the invention, comprising the following steps:
1) 90-100 parts of deionized water are added in planetary mixer, carboxymethyl cellulose 4- is added under agitation
4.5 parts, continue to be kept stirring, obtains mixture A；
2) 0.5-2 parts of conductive black sievings are added in step 1) the mixture A, in revolution speed 20rpm-
It is stirred under the conditions of 60rpm, rate of dispersion 1000-1600rpm；
3) expanded graphite 50-60 parts and manganese dioxide-mangano-manganic oxide composite material are added into system obtained by step 2)
It 40-50 parts, is stirred under the conditions of revolution speed 20rpm-60rpm, rate of dispersion 1300-1600rpm, obtains mixture B；
4) it will be mixed under 1.5-3 parts of remaining deionized water of formula ratio, 2.2-2.5 parts of butadiene-styrene rubber and polyalcohol stirring conditions
It is even, obtain mixture C；
5) mixture C is added in mixture B, in revolution speed 20rpm-50rpm, rate of dispersion 1000-1500rpm
Under the conditions of stir, then carry out vacuumizing stirring, stir 15-40min to get battery cathode slurry.
Refer to the condition of revolution speed 40-60rpm, rate of dispersion 700-1200rpm under stirring condition described in step 1)
Under.
Continue to stir the condition referred in revolution speed 40-60rpm, rate of dispersion 700-1200rpm described in step 1)
Under be kept stirring 40-60min.
Sieving described in step 2) referred to 300-400 mesh.Mixing time 1-2h described in step 2).
Mixing time described in step 3) is 2-3h.
Mixing speed described in step 4) is stirred 50-110min under the conditions of being 2000-3000rpm.
Described in step 5) under the conditions of revolution speed 20rpm-50rpm, rate of dispersion 1000-1500rpm mixing time
For 3-4h.
It is 30-40rpm that stirring revolution speed is vacuumized in step 5).
Manganese dioxide provided by the invention-mangano-manganic oxide composite material preparation method, during the preparation process ultrasonic item
Polyalcohol is added under part, is sufficiently mixed polyalcohol with manganese source, polyalcohol hydroxyl is abundant, has good hydrophily, then
CTAB cetyl trimethylammonium bromide and ammonium hydroxide is added, ammonium hydroxide provides alkaline environment, is conducive to manganese ion hydrolysis oxidation, into
And redox reaction occurs.CTAB has the cation of macoradical, and suction-operated is strong, and group large space steric hindrance is big, compels
Grow manganese dioxide-mangano-manganic oxide can only in specific region, meanwhile, CTAB is common with polyalcohol as surfactant
Effect drops low-surface-energy, product is finally made to be grown to nano bar-shape structure.Moreover, polyalcohol is added under ultrasound condition, mixing is more
Sufficiently, more evenly, so reaction is more evenly thorough, product size is nanoscale for dispersion.The rodlike knot of nanoscale produced by the invention
Structure can prevent dusting or reunion in charge and discharge process, moreover, nano-scale is conducive to improve specific capacity, club shaped structure increases electricity
The electronic conductivity of pole, therefore capacity attenuation is slow, has excellent cycle performance.
In preparation process of the present invention, control CMC, conductive black, expanded graphite and manganese dioxide-mangano-manganic oxide composite wood
Expect amount ratio, be conducive to active material and be uniformly dispersed, improves charge-discharge performance.In preparation process, first by deionized water and
CMC mixing is added conductive black in sieving, after being sufficiently stirred, is conducive to the surface that CM is adsorbed on conductive black, makes it sufficiently
The partial size for the conductive black that dispersion, sieving control are added keeps its electric conductivity more excellent persistently.The expanded graphite added and two
Manganese oxide-mangano-manganic oxide composite material, expanded graphite have lubricity, are uniformly dispersed, moreover, CMC can also be adsorbed on expansion stone
The surface of ink, thus caused by steric hindrance repulsion keep its fully dispersed, be conducive to disperse, not reunite, it is conductive more evenly, follow
Ring is more preferable.In addition, manganese dioxide-mangano-manganic oxide composite gauge of preparation is small, by being stirred, can be dispersed in
In expanded graphite gap, be conducive to improve and balance electric conductivity vertically and horizontally；Active material is uniformly dispersed, favorably
In conductive uniform, raising cycle performance.Remaining deionized water, butadiene-styrene rubber and polyalcohol are added together, due to polyalcohol
Polyhydroxy, which exists, is adsorbed on styrene-butadiene surface, is conducive to butadiene-styrene rubber and is dispersed in water, more stable in system, improves bonding
Property.Since CMC has been adequately mixed dispersion, the butadiene-styrene rubber being added at this time is sufficiently mixed upper for conductive black, expanded graphite etc.
It states in dispersion, avoids reuniting, the main caking property for improving negative electrode slurry prevents from falling off, lose powder.Moreover, be added
Polyalcohol and butadiene-styrene rubber are conducive to improve caking property, moreover it is possible to prevent gel, reunite, the problem of agglomeration, be conducive to improve battery
Cycle performance, moreover it is possible to improve the safety of battery.Moreover, the mixing speed and mixing time of each step are controlled in the present invention,
Be conducive to control being uniformly dispersed for raw material, do not destroy adhesive property.
Compared with prior art, the present invention controls the selection of raw material, amount ratio, charging sequence and stirring in preparation process
Time, speed etc. prevent from reuniting, condense and agglomerating, are conducive to improve first discharge specific capacity, can achieve 902mAh/g,
1000 90% or more circulation conservation rates.
Specific embodiment
Embodiment 1
A kind of lithium ion battery anode slurry, including following raw material:
The manganese dioxide-mangano-manganic oxide composite material preparation method, comprising the following steps:
A, after mixing liquor potassic permanganate and manganese sulfate solution that molar ratio is 1:10, the third three are added under ultrasound condition
Alcohol, ultrasonic disperse 20min mix, obtain mixed solution；The mixed solution and polyalcohol of liquor potassic permanganate and manganese sulfate solution
Volume ratio is 10:1；
B, CTAB and ammonium hydroxide is added in the mixed system prepared to step A, after mixing, potassium permanganate concentration is in system
0.005mol/L, the molar ratio of ammonia is 1:2:4.5 in potassium permanganate, CTAB and ammonium hydroxide, sealing, and heating is anti-under the conditions of 155 DEG C
Answer 16h；After reaction, wash, it is dry, be cooled to room temperature to get.Prepared manganese dioxide-mangano-manganic oxide composite wood
Material, it is of uniform size, it is the nanorod structure of nano-scale, nanorod diameter 5-80nm, length 50-1000nm.
A kind of preparation method of above-mentioned lithium ion battery anode slurry, comprising the following steps:
1) 90 parts of deionized water are added in planetary mixer, in revolution speed 60rpm, rate of dispersion 1000rpm
Under stirring condition be added 4.5 parts of carboxymethyl cellulose, revolution speed 60rpm, rate of dispersion 1000rpm stirring condition under after
It is continuous to be kept stirring 55min, obtain mixture A；
2) 0.8 part of 400 mesh of mistake of conductive black is added in step 1) the mixture A, in revolution speed 60rpm,
1.5h is stirred under the conditions of rate of dispersion 1600rpm；
3) 53 parts of expanded graphite and manganese dioxide-mangano-manganic oxide composite material 46 are added into system obtained by step 2)
Part, 2.5h is stirred under the conditions of revolution speed 40rpm, rate of dispersion 1600rpm, obtains mixture B；
4) the remaining deionized water of formula ratio, 2.2 parts of butadiene-styrene rubber and 1.8 parts of ethylene glycol are stirred under the conditions of 2500rpm
It mixes and is mixed under mixing 90min stirring condition, obtain mixture C；
5) mixture C is added in mixture B, is stirred under the conditions of revolution speed 40rpm, rate of dispersion 1300rpm
Then 3h carries out vacuumizing stirring, revolving speed 40rpm stirs 30min to get battery cathode slurry.
Embodiment 2
A kind of lithium ion battery anode slurry, including following raw material:
The manganese dioxide-mangano-manganic oxide composite material preparation method, comprising the following steps:
A, after mixing liquor potassic permanganate and manganese sulfate solution that molar ratio is 1:11, the third three are added under ultrasound condition
Alcohol, ultrasonic disperse 30min mix, obtain mixed solution；The mixed solution and polyalcohol of liquor potassic permanganate and manganese sulfate solution
Volume ratio is 12:1；
B, CTAB and ammonium hydroxide is added in the mixed system prepared to step A, after mixing, potassium permanganate concentration is in system
0.01mol/L, sealing, heating react 18h under the conditions of 160 DEG C；After reaction, wash, it is dry, be cooled to room temperature to get.
Prepared manganese dioxide-mangano-manganic oxide composite material, it is of uniform size, it is the nanorod structure of nano-scale, nanometer rods are straight
Diameter 5-80nm, length 50-1000nm.
A kind of preparation method of above-mentioned lithium ion battery anode slurry, comprising the following steps:
1) 100 parts of deionized water are added in planetary mixer, in revolution speed 60rpm, rate of dispersion 1000rpm
Under stirring condition be added 5 parts of carboxymethyl cellulose, revolution speed 60rpm, rate of dispersion 1000rpm stirring condition under continue
It is kept stirring 50min, obtains mixture A；
2) 1.3 parts of 400 meshes of mistake of conductive black are added in step 1) the mixture A, in revolution speed 60rpm,
1.5h is stirred under the conditions of rate of dispersion 1500rpm；
3) 58.5 parts of expanded graphite and manganese dioxide-mangano-manganic oxide composite material 47 are added into system obtained by step 2)
Part, 3h is stirred under the conditions of revolution speed 60rpm, rate of dispersion 1600rpm, obtains mixture B；
4) the remaining deionized water of formula ratio, 2.3 parts of butadiene-styrene rubber and 2.1 parts of glycerol are stirred under the conditions of 2800rpm
It is mixed under mixing 90min stirring condition, obtains mixture C；
5) mixture C is added in mixture B, is stirred under the conditions of revolution speed 60rpm, rate of dispersion 1500rpm
Then 3h carries out vacuumizing stirring, revolving speed 40rpm stirs 35min to get battery cathode slurry.
Embodiment 3
A kind of lithium ion battery anode slurry, including following raw material:
The manganese dioxide-mangano-manganic oxide composite material preparation method, with embodiment 1.
A kind of preparation method of above-mentioned lithium ion battery anode slurry, comprising the following steps:
1) 100 parts of solvents of deionized water are added in planetary mixer, in revolution speed 60rpm, rate of dispersion
5.5 parts of carboxymethyl cellulose are added under the stirring condition of 1200rpm, is stirred in revolution speed 60rpm, rate of dispersion 1200rpm
Continue to be kept stirring 60min under the conditions of mixing, obtains mixture A；
2) 1.6 parts of 400 meshes of mistake of conductive black are added in step 1) the mixture A, in revolution speed 60rpm,
2h is stirred under the conditions of rate of dispersion 1600rpm；
3) 58 parts of expanded graphite and manganese dioxide-mangano-manganic oxide composite material 50 are added into system obtained by step 2)
Part, 3h is stirred under the conditions of revolution speed 60rpm, rate of dispersion 1600rpm, obtains mixture B；
4) the remaining deionized water of formula ratio, 2.5 parts of butadiene-styrene rubber and 2.5 parts of glycerol are stirred under the conditions of 3000rpm
It is mixed under mixing 100min stirring condition, obtains mixture C；
5) mixture C is added in mixture B, is stirred under the conditions of revolution speed 60rpm, rate of dispersion 1500rpm
Then 4h carries out vacuumizing stirring, revolving speed 30rpm stirs 40min to get battery cathode slurry.
Comparative example 1
The formula of battery cathode slurry is commercially available graphite cathode piece.
Comparative example 2
The formula of battery cathode slurry is same as Example 2, comparative example 2 the preparation method comprises the following steps:
By all raw materials in being mixed in planetary mixer, in the stirring bar of revolution speed 50rpm, rate of dispersion 1500rpm
6h is stirred under part.
Comparative example 3
The formula of battery cathode slurry is same as Example 3, comparative example 3 the preparation method comprises the following steps:
By all raw materials in being mixed in planetary mixer, in the stirring bar of revolution speed 40rpm, rate of dispersion 1600rpm
8h is stirred under part.
Caking property detection:
The embodiment 1-3 and comparative example 1-3 negative electrode slurry prepared is respectively coated in metal collector, control coating is thick
Degree is 50-60 μm, is then dried, tabletting, punching is up to negative electrode tab.Existed using same procedure and experiment condition metal blade
The negative electrode tab of embodiment 1-3 and comparative example 1-3 preparation is drawn 100 times, and the negative electrode tab coating shedding area of embodiment 1-3 preparation is less than
0.5%.And the negative electrode tab coating shedding of comparative example 1 falls off serious 33% or so.Comparative example 1-2 falls off area on 15% left side
It is right.
Negative electrode tab the same terms prepared by embodiment 1-3 and comparative example 1-3 negative electrode slurry are struck into piece detection, embodiment 1-3
Negative electrode tab do not lose powder, and the negative electrode tab of comparative example 1-3 has picking phenomenon.Charge and discharge cycles 500 times, embodiment 1-3's is negative
Pole piece does not lose powder, and 1 negative electrode tab of comparative example largely loses powder, and embodiment 2-3 has a small amount of picking.
Charge and discharge electro-detection:
The negative electrode tab that the negative electrode slurry of embodiment 1-3 and comparative example 1-3 are prepared in the same manner respectively with ion lithium
Battery anode slice is assembled into battery, is tested, and carries out charge and discharge cycles with the current density of 100mAh/g, tests capacity of negative plates
And cycle life, embodiment 1 is under 50mA/g charge and discharge speed, first discharge specific capacity 902mAh/g, 500 circulation conservation rates
90%.Embodiment 2 is under 50mA/g charge and discharge speed, first discharge specific capacity 849mAh/g, 500 circulation conservation rates 92%.
Embodiment 3 is under 50mA/g charge and discharge speed, first discharge specific capacity 824mAh/g, 500 circulation conservation rates 90%.Comparative example
1 under 50mA/g charge and discharge speed, first discharge specific capacity 321mAh/g, 500 circulation conservation rates 38%.Comparative example 2 exists
Under 50mA/g charge and discharge speed, first discharge specific capacity 520mAh/g, 500 circulation conservation rates 67%.Comparative example 3 is in 50mA/
Under g charge and discharge speed, first discharge specific capacity 469mAh/g, 500 circulation conservation rates 63%.
Claims (10)
1. a kind of lithium ion battery anode slurry, which is characterized in that the lithium ion battery anode slurry includes following parts by weight
Raw material:
2. lithium ion battery anode slurry according to claim 1, which is characterized in that the polyalcohol is selected from glycerol or second
Glycol.
3. lithium ion battery anode slurry according to claim 1, which is characterized in that the oxidation of manganese dioxide-four three
The preparation method of manganese composite material, comprising the following steps:
A, after mixing liquor potassic permanganate and manganese sulfate solution, polyalcohol is added under ultrasound condition, mixes, obtains mixed solution；
B, CTAB and ammonium hydroxide is added in the mixed system prepared to step A, after mixing, sealing, heating reaction；After reaction,
Washing, it is dry, be cooled to room temperature to get.
4. lithium ion battery anode slurry according to claim 3, which is characterized in that permanganic acid in step A mixed solution
The molar ratio of potassium and manganese sulfate is 1:10-12；The mixed solution and polyalcohol of liquor potassic permanganate and manganese sulfate solution in step A
Volume ratio be 9-13:0.8-1.5.
5. lithium ion battery anode slurry according to claim 3, which is characterized in that CTAB and ammonium hydroxide are added in step B
Afterwards, potassium permanganate concentration is 0.001-0.05mol/L in system, and the molar ratio of ammonia is 1:2- in potassium permanganate, CTAB and ammonium hydroxide
3:4-7。
6. lithium ion battery anode slurry according to claim 3, which is characterized in that heating, which is reacted, described in step B is
Finger reacts 8-18h under the conditions of 150-165 DEG C.
7. a kind of preparation method of lithium ion battery anode slurry described in any one of claims 1-6, which is characterized in that described
Preparation method the following steps are included:
1) 90-100 parts of solvents of deionized water are added in planetary mixer, carboxymethyl cellulose 4- is added under agitation
4.5 parts, continue to be kept stirring, obtains mixture A；
2) 0.5-2 parts of conductive black sievings are added in step 1) the mixture A, in revolution speed 20rpm-60rpm, are divided
It is stirred under the conditions of scattered speed 1000-1600rpm；
3) expanded graphite 50-60 parts and manganese dioxide-mangano-manganic oxide composite material 50-60 is added into system obtained by step 2)
Part, it is stirred under the conditions of revolution speed 20rpm-60rpm, rate of dispersion 1300-1600rpm, obtains mixture B；
4) it will be mixed under 1.5-3 parts of remaining deionized water of formula ratio, 2.2-2.5 parts of butadiene-styrene rubber and polyalcohol stirring conditions,
Obtain mixture C；
5) mixture C is added in mixture B, in revolution speed 20rpm-50rpm, rate of dispersion 1000-1500rpm condition
Then lower stirring carries out vacuumizing stirring, stir 15-40min to get battery cathode slurry.
8. the preparation method of lithium ion battery anode slurry according to claim 7, which is characterized in that described in step 1)
Under conditions of referring to revolution speed 40-60rpm, rate of dispersion 700-1200rpm under stirring condition.
9. the preparation method of lithium ion battery anode slurry according to claim 7, which is characterized in that described in step 2)
Sieving referred to 300-400 mesh；Mixing time 1-2h described in step 2).
10. the preparation method of lithium ion battery anode slurry according to claim 7, which is characterized in that institute in step 5)
Stating the mixing time under the conditions of revolution speed 20rpm-50rpm, rate of dispersion 1000-1500rpm is 3-4h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112151756A (en) * | 2020-09-14 | 2020-12-29 | 江苏塔菲尔新能源科技股份有限公司 | Negative plate and battery |
| CN113466278A (en) * | 2021-06-29 | 2021-10-01 | 合肥国轩高科动力能源有限公司 | Method for detecting distribution uniformity of SBR (styrene butadiene rubber) binder of graphite cathode of lithium battery in pole piece |
| CN115594223A (en) * | 2022-10-25 | 2023-01-13 | 广东邦普循环科技有限公司（Cn） | Modified lithium ion sieve, manganese dioxide adsorbent, preparation method and application of manganese dioxide adsorbent, and method for extracting lithium from salt lake |
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| CN115594223A (en) * | 2022-10-25 | 2023-01-13 | 广东邦普循环科技有限公司（Cn） | Modified lithium ion sieve, manganese dioxide adsorbent, preparation method and application of manganese dioxide adsorbent, and method for extracting lithium from salt lake |
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