CN109950505A - A kind of efficient lithium titanate battery slurry and preparation method thereof - Google Patents
A kind of efficient lithium titanate battery slurry and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of efficient lithium titanate battery slurry, is made of following raw material: 58-68 parts of lithium titanates, 3-8 parts of acetylene blacks, 3-5 parts of Ketjen blacks, 10-15 parts of active materials, 12-16 parts of modified epoxy glue, 20% dimethyl sulphoxide aqueous solution of 75-85 part；The invention also discloses a kind of preparation methods of efficient lithium titanate battery slurry；Raw material is used as by lithium titanate, acetylene black, active material and modified epoxy glue etc., prepare a kind of efficient lithium titanate battery slurry, using acetylene black and Ketjen black as conductive agent, acetylene black and Ketjen black exist with nano shape, with unique branched structure and excellent electric conductivity, different heating temperatures is first passed through during the preparation process to heat raw material, the processing can strengthen the characteristic of various raw materials itself, and moisture content contained by material can be eliminated, elimination prepares the error generated in lithium titanate battery slurry process, improves accuracy.
Description
Technical field
The invention belongs to technical field of lithium batteries, specially a kind of efficient lithium titanate battery slurry and preparation method thereof.
Background technique
With increasingly popularizing for electric car, the demand of lithium ion battery increasingly increases, the safety of current driving force battery,
The performances such as cycle life, quick charge needs are substantially improved.Commercialized lithium ion battery mostly uses greatly graphite cathode material, but
There are some drawbacks for graphite cathode material, such as while overcharging Li dendrite easy to form, cause battery short circuit, form security risk.
In addition graphite material platform is lower, Yi Yinqi electrolyte decomposition and the problem of be embedded in altogether, this can all be caused under cycle performance of battery
Drop and cannot big multiplying power fast charge etc..
Lithium titanate is not likely to produce Li dendrite to lithium current potential 1.55V or so, and security performance is more preferable；Lithium titanate is zero strain material
Material, has excellent cycle performance, and service life is longer than graphite cathode；The lithium ion diffusion coefficient of lithium titanate compares graphite cathode
It is order of magnitude greater so that fast charging and discharging may be implemented in battery.Therefore lithium titanate battery has huge as power battery
Commercial application prospect.But lithium titanate belongs to nanometer materials, large specific surface area, bad dispersibility, according to traditional slurry system
Preparation Method is difficult to prepare uniform slurry, leads to that pole coating effect is poor, particle is more, to influence the circulation of lithium titanate battery
Performance and high rate performance.
Chinese invention patent CN107681109A discloses a kind of lithium titanate battery slurry, including solute and solvent, wherein
The raw material of solute includes: lithium titanate 89-92%, conductive agent SP4%, conductive agent CNT1-2%, binder by weight percentage
PVDF3-5%.The invention also discloses the preparation methods of above-mentioned lithium titanate battery slurry.The present invention is by adjusting binder PVDF
Content and cooperate to obtain suitable formula with lithium titanate, conductive agent SP, conductive agent CNT with suitable proportion, and combine suitable
Suitable slurry-stirring process, which can be effectively improved, closes the excessive problem of slurry process medium viscosity, so that viscosity of the invention is by 6000-8000
It is reduced to 2000-4000, greatly improves coatability of the invention, promotes the high rate performance of battery；And operation of the present invention
Simply.Although but still Painting effect is still not excellent enough for the lithium titanate battery slurry viscosity reduction of invention preparation, metatitanic acid
The performance that lithium battery uses under high magnification is bad.
Summary of the invention
In order to overcome above-mentioned technical problem, the present invention provides a kind of efficient lithium titanate battery slurry and preparation method thereof；
It is used as raw material by lithium titanate, acetylene black, active material and modified epoxy glue etc., prepares a kind of efficient lithium titanate battery slurry
Material, exists using acetylene black and Ketjen black as conductive agent, acetylene black and Ketjen black with nano shape, has unique branch link
Structure and excellent electric conductivity first pass through different heating temperatures during the preparation process and heat to raw material, the processing
The characteristic of various raw materials itself can be strengthened, and moisture content contained by material can be eliminated, elimination prepares lithium titanate battery slurry
The error generated in the process improves accuracy；A kind of carboxyl end group polyethers, the object is made by polypropylene glycol and phthalic anhydride
Matter viscosity is lower and contains flexible molecule chain, and preliminary toughening can be carried out to epoxy resin, later by the way that fluorubber is added
By ball milling, the modes such as heating improve its performance, which had both possessed goes to be increased by carboxyl end group polyethers
The excellent toughness of tough acquisition has again through the increased excellent corrosion resistance of fluorubber.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of efficient lithium titanate battery slurry, is made of following raw material: 58-68 parts of lithium titanates, 3-8 parts of acetylene
It is black, 3-5 parts of Ketjen blacks, 10-15 parts of active materials, 12-16 parts of modified epoxy glue, 20% dimethyl sulfoxide water of 75-85 part
Solution；
The efficient lithium titanate battery slurry is made by the following method:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, at heating
The heating temperature of control lithium titanate and modified epoxy glue is 120 DEG C during reason, and pressure is -0.10MPa, and heating time is
20h, control acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, heating time 25h, heat treatment
After take out stand 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank
Vacuum degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is obtained after stirring 2h
Mixed liquor stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Entering active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/min, from
Speed of walking around is 300r/min, stirs to the viscosity of mixed slurry in 2000-2500mpas, obtains premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Further, the modified epoxy glue is made of following raw material: 8-15 parts of polypropylene glycols, 12-20
Part phthalic anhydride, 18-35 parts of bisphenol-As, 24-32 parts of epoxy chloroethanes, 18-30 parts of benzene, 5-13 10% sodium hydroxide of part are molten
Liquid, 3-5 parts of polyvinylpyrrolidones, 8-15 parts of fluorubber.
Further, the modified epoxy glue is made by the following method:
(1) bisphenol-A is added in dissolution kettle, epoxy chloroethanes and benzene is added, at the uniform velocity stir and be warming up to 75 DEG C, stirring
It is transferred in reaction kettle after 30min, 10% sodium hydroxide solution is added, is warming up to 45 DEG C, at the uniform velocity stirring 2h, filtering is stood, will
Benzole soln is pumped in reflux benzene kettle, is back to the benzene steamed and droplet does not occur, is stood cooling 45min, is transferred in de- benzene kettle,
It is decompressed to no distillate at 135 DEG C, takes out, dry obtained epoxy resin；
(2) polypropylene glycol is added in three-necked flask, is warming up to 110 DEG C of vacuum dehydration 2h, phthalic anhydride is added, risen
Temperature reacts 5h at this temperature and carboxyl end group polyethers is made, take out, mix in beaker with epoxy resin to 150 DEG C, 85 DEG C of heating
Until fusing, is stirring evenly and then adding into polyvinylpyrrolidone, taking-up standing 1h obtains mixture after reacting 3h；
(3) fluorubber is mixed with mixture, is poured into ball mill, high speed ball milling, ball are carried out with the revolving speed of 1600r/min
It is added after mill in the beaker equipped with 100mL dehydrated alcohol, ultrasonic 30min extracts the air in mixed liquor out, is transferred to vacuum
In drying box, vacuum degree -0.09MPa is controlled, temperature is 65 DEG C, and modified epoxy glue is made in dry 12h.
The present invention, using benzene as solvent, prepares asphalt mixtures modified by epoxy resin using bisphenol-A and epoxy chloroethanes as raw material under alkaline condition
Rouge, epoxy resin has excellent mechanical property, adhesive property and chemical stability, but epoxy resin brittleness is larger, resistance to punching
It is poor to hit performance, so need to be modified it, it is poly- that by polypropylene glycol and phthalic anhydride a kind of carboxyl end group is made in the present invention
Ether, the substance viscosity is lower and contains flexible molecule chain, and preliminary toughening, reaction process middle-end can be carried out to epoxy resin
Active end group in carboxyl polyethers is cured with epoxy resin to react, and makes flexible molecule chain in a manner of Covalent bonding together
Into in epoxy resin, so toughening effect can be reached but also obtain excellent mechanical property and thermal stability；Fluorubber
Branch is largely assembled, and random special construction is formed, and causes fluorubber resistance to low temperature poor, but fluorubber possess it is excellent resistance to
Corrosive nature and Weather resistant heat resistant performance, so the present invention passes through ball milling by the way that fluorubber is added, the modes such as heating prepare modification
Epoxide-resin glue had not only possessed and has gone the excellent toughness for carrying out toughening acquisition but also have to increase by fluorubber by carboxyl end group polyethers
Excellent corrosion resistance.
Further, the active material is any one in positive active material or negative electrode active material.
A kind of preparation method of efficient lithium titanate battery slurry, includes the following steps:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, at heating
The heating temperature of control lithium titanate and modified epoxy glue is 120 DEG C during reason, and pressure is -0.10MPa, and heating time is
20h, control acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, heating time 25h, heat treatment
After take out stand 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank
Vacuum degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is obtained after stirring 2h
Mixed liquor stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Entering active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/min, from
Speed of walking around is 300r/min, stirs to the viscosity of mixed slurry in 5000-8000mpas, obtains premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Beneficial effects of the present invention:
(1) present invention is used as raw material, preparation one by lithium titanate, acetylene black, active material and modified epoxy glue etc.
The efficient lithium titanate battery slurry of kind, is deposited using acetylene black and Ketjen black as conductive agent, acetylene black and Ketjen black with nano shape
There is unique branched structure and excellent electric conductivity, first passing through different heating temperatures during the preparation process to raw material
Heated, which can strengthen the characteristic of various raw materials itself, and can eliminate moisture content contained by material, eliminate
The error generated in lithium titanate battery slurry process is prepared, accuracy is improved；
(2) present invention prepares a kind of modified epoxy glue, passes through polypropylene glycol and phthalic acid in preparation process
A kind of carboxyl end group polyethers is made in acid anhydride, and the substance viscosity is lower and contains flexible molecule chain, can carry out to epoxy resin preliminary
Toughening, pass through ball milling by the way that fluorubber is added later, the modes such as heating improve its performance, which both gathered around
Have and goes the excellent toughness for carrying out toughening acquisition to have again and increase excellent corrosion resistance by fluorubber by carboxyl end group polyethers
Energy；
(3) the efficient lithium titanate battery slurry prepared of the present invention, viscosity between 2000-2500mpas so that
The lithium titanate battery slurry has excellent coating performance, has the lithium titanate battery of preparation under high magnification
Excellent using effect, and using modified epoxy glue as raw material, not only there is excellent bond effect, but also the titanium can be assigned
The good corrosion resistance of acid lithium battery slurry and excellent stability；Present invention process is simple, and the slurry of preparation is uniformly dispersed
Without bulky grain, the lithium titanate battery finally prepared has good cycle performance.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, all other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment 1
A kind of efficient lithium titanate battery slurry, is made of following raw material: 58 parts of lithium titanates, 3 parts of acetylene blacks, and 3 parts
Ketjen black, 10 parts of positive active materials, 12 parts of modified epoxy glue, 75 part of 20% dimethyl sulphoxide aqueous solution；
The efficient lithium titanate battery slurry is made by the following method:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, at heating
The heating temperature of control lithium titanate and modified epoxy glue is 120 DEG C during reason, and pressure is -0.10MPa, and heating time is
20h, control acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, heating time 25h, heat treatment
After take out stand 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank
Vacuum degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is obtained after stirring 2h
Mixed liquor stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Enter positive active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/
Min, rotation revolving speed are 300r/min, stir to the viscosity of mixed slurry in 2000-2500mpas, obtain premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry；
The modified epoxy glue is made by the following method:
(1) bisphenol-A is added in dissolution kettle, epoxy chloroethanes and benzene is added, at the uniform velocity stir and be warming up to 75 DEG C, stirring
It is transferred in reaction kettle after 30min, 10% sodium hydroxide solution is added, is warming up to 45 DEG C, at the uniform velocity stirring 2h, filtering is stood, will
Benzole soln is pumped in reflux benzene kettle, is back to the benzene steamed and droplet does not occur, is stood cooling 45min, is transferred in de- benzene kettle,
It is decompressed to no distillate at 135 DEG C, takes out, dry obtained epoxy resin；
(2) polypropylene glycol is added in three-necked flask, is warming up to 110 DEG C of vacuum dehydration 2h, phthalic anhydride is added, risen
Temperature reacts 5h at this temperature and carboxyl end group polyethers is made, take out, mix in beaker with epoxy resin to 150 DEG C, 85 DEG C of heating
Until fusing, is stirring evenly and then adding into polyvinylpyrrolidone, taking-up standing 1h obtains mixture after reacting 3h；
(3) fluorubber is mixed with mixture, is poured into ball mill, high speed ball milling, ball are carried out with the revolving speed of 1600r/min
It is added after mill in the beaker equipped with 100mL dehydrated alcohol, ultrasonic 30min extracts the air in mixed liquor out, is transferred to vacuum
In drying box, vacuum degree -0.09MPa is controlled, temperature is 65 DEG C, and modified epoxy glue is made in dry 12h.
Embodiment 2
A kind of efficient lithium titanate battery slurry, is made of following raw material: 60 parts of lithium titanates, 5 parts of acetylene blacks, and 3 parts
Ketjen black, 12 parts of positive active materials, 13 parts of modified epoxy glue, 18 part of 20% dimethyl sulphoxide aqueous solution；
The efficient lithium titanate battery slurry is made by the following method:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, at heating
The heating temperature of control lithium titanate and modified epoxy glue is 120 DEG C during reason, and pressure is -0.10MPa, and heating time is
20h, control acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, heating time 25h, heat treatment
After take out stand 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank
Vacuum degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is obtained after stirring 2h
Mixed liquor stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Enter positive active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/
Min, rotation revolving speed are 300r/min, stir to the viscosity of mixed slurry in 2000-2500mpas, obtain premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Embodiment 3
A kind of efficient lithium titanate battery slurry, is made of following raw material: 65 parts of lithium titanates, 7 parts of acetylene blacks, and 4 parts
Ketjen black, 13 parts of positive active materials, 14 parts of modified epoxy glue, 82 part of 20% dimethyl sulphoxide aqueous solution；
The efficient lithium titanate battery slurry is made by the following method:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, at heating
The heating temperature of control lithium titanate and modified epoxy glue is 120 DEG C during reason, and pressure is -0.10MPa, and heating time is
20h, control acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, heating time 25h, heat treatment
After take out stand 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank
Vacuum degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is obtained after stirring 2h
Mixed liquor stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Enter positive active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/
Min, rotation revolving speed are 300r/min, stir to the viscosity of mixed slurry in 2000-2500mpas, obtain premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Embodiment 4
A kind of efficient lithium titanate battery slurry, is made of following raw material: 68 parts of lithium titanates, 8 parts of acetylene blacks, and 5 parts
Ketjen black, 15 parts of positive active materials, 16 parts of modified epoxy glue, 85 part of 20% dimethyl sulphoxide aqueous solution；
The efficient lithium titanate battery slurry is made by the following method:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, at heating
The heating temperature of control lithium titanate and modified epoxy glue is 120 DEG C during reason, and pressure is -0.10MPa, and heating time is
20h, control acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, heating time 25h, heat treatment
After take out stand 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank
Vacuum degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is obtained after stirring 2h
Mixed liquor stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Enter positive active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/
Min, rotation revolving speed are 300r/min, stir to the viscosity of mixed slurry in 2000-2500mpas, obtain premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Comparative example 1
This comparative example replaces modified epoxy glue, the following institute of preparation method compared with Example 1, with Kynoar
Show:
Step S1, lithium titanate, acetylene black, Ketjen black and Kynoar are heated respectively, it is heat-treated
The heating temperature that lithium titanate and Kynoar are controlled in journey is 120 DEG C, and pressure is -0.10MPa, heating time 20h, control
Acetylene black, the heating temperature of Ketjen black are 160 DEG C, and pressure is -0.07MPa, and heating time 25h takes after heat treatment
2h is stood out, it is spare；
Step S2, Kynoar and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank vacuum
Degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is mixed after stirring 2h
Liquid stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, adds
Enter positive active material and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/
Min, rotation revolving speed are 300r/min, stir to the viscosity of mixed slurry in 2000-2500mpas, obtain premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Comparative example 2
This comparative example replaces acetylene black, Ketjen black compared with Example 1, with graphite fibre, and preparation method is as follows:
Step S1, lithium titanate, graphite fibre and Kynoar are heated respectively, is controlled in heat-treatment process
The heating temperature of lithium titanate and Kynoar processed is 120 DEG C, and pressure is -0.10MPa, heating time 20h, and control graphite is fine
The heating temperature of dimension is 160 DEG C, and pressure is -0.07MPa, heating time 25h, takes out after heat treatment and stands 2h, standby
With；
Step S2, Kynoar and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank vacuum
Degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is mixed after stirring 2h
Liquid stands 5h, spare；
Step S3, it by graphite fibre grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, positive-active is added
Substance and lithium titanate, control agitator tank vacuum degree are -0.08MPa, and control agitator tank revolution revolving speed is 45r/min, rotation revolving speed
For 300r/min, stirs to the viscosity of mixed slurry in 2000-2500mpas, obtain premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, control stirring
Tank revolves revolving speed as 20r/min, and rotation revolving speed is 500r/min, is taken out after stirring 30min, crosses 200 meshes, efficient metatitanic acid is made
Lithium battery slurry.
Comparative example 3
The present embodiment is a kind of lithium titanate battery slurry in market.
To the dispersion performance of the embodiment 1-4 and comparative example 1-3 efficient lithium titanate battery slurry prepared, high rate performance and follow
Ring performance is detected, as a result as shown in following table 1-3；
Dispersibility: slurry being respectively charged into 100mL graduated cylinder, is placed in 25 DEG C of temperature of insulating box, is placed for 24 hours afterwards to amount
Slurry carries out solid content test at cylinder surface layer 20mm, and test result is as follows shown in table 1；
Table 1
The fineness of embodiment 1-4 can be found out from table 1 at 27-32 μm, comparative example 1-3 fineness is at 33-57 μm；Embodiment 1-
4 viscosity preceding for 24 hours is at 2290-2489 (mpas), and the viscosity preceding for 24 hours of comparative example 1-3 is at 2673-5869 (mpas)；Implement
The viscosity rear for 24 hours of example 1-4 is at 2695-2858 (mpas), and the viscosity rear for 24 hours of comparative example 1-3 is at 3157-6769 (mpas)；
The solid content preceding for 24 hours of embodiment 1-4 is in 53.2-57.5%, and the solid content preceding for 24 hours of comparative example 1-3 is in 60.7-65.3%；Implement
The solid content rear for 24 hours of example 1-4 is in 53.1-56.3%, and the solid content rear for 24 hours of comparative example 1-3 is in 59.8-63.5%.
High rate performance:
1C constant-current discharge stands 10min, respectively using 3C/5C/8C/10C constant-current charge to 2.8V, as a result such as to 1.5V
Shown in the following table 2；
Table 2
| 3C | 5C | 8C | 10C | |
| Embodiment 1 | 98.5% | 97.6% | 95.3% | 94.3% |
| Embodiment 2 | 99.3% | 98.1% | 97.6% | 96.9% |
| Embodiment 3 | 99.7% | 99.2% | 98.5% | 98.0% |
| Embodiment 4 | 100% | 99.5% | 99.1% | 98.3% |
| Comparative example 1 | 96.5% | 94.6% | 93.9% | 93.1% |
| Comparative example 2 | 95.3% | 93.7% | 92.1% | 90.8% |
| Comparative example 3 | 94.7% | 91.5% | 89.7% | 87.5% |
The rate of charge of embodiment 1-4 is in 98.5-100% when 3C as can be seen from Table 2, and the charging of comparative example 1-3 is again
Rate is in 94.7-96.5%；The rate of charge of embodiment 1-4 exists in 97.6-99.5%, the rate of charge of comparative example 1-3 when 5C
91.5-94.6%；The rate of charge of embodiment 1-4 is in 95.3-99.1% when 8C, and the rate of charge of comparative example 1-3 is in 89.7-
93.9%；The rate of charge of embodiment 1-4 is in 94.3-98.3% when 10C, and the rate of charge of comparative example 1-3 is in 87.5%-
93.1%.
Cycle performance:
3C constant-current constant-voltage charging stands 10min by electric current 0.3C to 2.8V, and 3C constant-current discharge to 1.5V is stood
10min observes capacity retention ratio, as a result as shown in table 3 below；
Table 3
| 300 times | 600 times | 900 times | 1200 times | |
| Embodiment 1 | 98.7% | 97.6% | 96.8% | 95.3% |
| Embodiment 2 | 99.3% | 98.1% | 97.5% | 96.3% |
| Embodiment 3 | 99.5% | 98.8% | 97.8% | 97.1% |
| Embodiment 4 | 99.7% | 99.1% | 98.5% | 98.2% |
| Comparative example 1 | 94.3% | 93.5% | 92.1% | 91.5% |
| Comparative example 2 | 93.6% | 92.8% | 92.0% | 91.1% |
| Comparative example 3 | 91.2% | 90.2% | 89.5% | 87.3% |
The capacity retention ratio of 300 embodiment 1-4 is recycled as can be seen from Table 3 in 98.7-99.7%, comparative example 1-3
Capacity retention ratio in 91.2-94.3%；The capacity retention ratio of 600 embodiment 1-4 is recycled in 97.6-99.1%, comparative example
1-3 capacity retention ratio is in 90.2-93.5%；The capacity retention ratio of 900 embodiment 1-4 is recycled in 96.8-98.5%, comparative example
1-3 capacity retention ratio is in 89.5-92.1%；The capacity retention ratio of 1200 embodiment 1-4 is recycled in 95.3-98.2%, comparison
Example 1-3 capacity retention ratio is in 87.3-91.5%.So consolidated statement 1-3 is it can be seen that efficient lithium titanate battery prepared by the present invention
Slurry has lower viscosity, and lithium titanate battery is with good performance under high magnification, it may have good cycle performance.
In the description of this specification, the description of reference term " one embodiment ", " example ", " specific example " etc. means
Particular features, structures, materials, or characteristics described in conjunction with this embodiment or example are contained at least one implementation of the invention
In example or example.In the present specification, schematic expression of the above terms may not refer to the same embodiment or example.
Moreover, particular features, structures, materials, or characteristics described can be in any one or more of the embodiments or examples to close
Suitable mode combines.
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, and without departing from invention or surpasses
More range defined in the claims, is within the scope of protection of the invention.
Claims (5)
1. a kind of efficient lithium titanate battery slurry, which is characterized in that be made of following raw material: 58-68 parts of lithium titanates, 3-
8 parts of acetylene blacks, 3-5 parts of Ketjen blacks, 10-15 parts of active materials, 12-16 parts of modified epoxy glue, 20% dimethyl of 75-85 part
Sulfoxide aqueous solution；
The efficient lithium titanate battery slurry is made by the following method:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, it is heat-treated
The heating temperature that lithium titanate and modified epoxy glue are controlled in journey is 120 DEG C, and pressure is -0.10MPa, heating time 20h,
Control acetylene black, the heating temperature of Ketjen black is 160 DEG C, pressure is -0.07MPa, heating time 25h, and heat treatment terminates
It takes out afterwards and stands 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank vacuum
Degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is mixed after stirring 2h
Liquid stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, be added and live
Property substance and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/min, is walked around certainly
Speed is 300r/min, stirs to the viscosity of mixed slurry in 5000-8000mpas, obtains premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, and control agitator tank is public
Speed of walking around is 20r/min, and rotation revolving speed is 500r/min, takes out after stirring 30min, crosses 200 meshes, and efficient lithium titanate electricity is made
Pond slurry.
2. a kind of efficient lithium titanate battery slurry according to claim 1, which is characterized in that the modified epoxy glue
It is made of following raw material: 8-15 parts of polypropylene glycols, 12-20 parts of phthalic anhydrides, 18-35 parts of bisphenol-As, 24-32 parts
Epoxy chloroethanes, 18-30 parts of benzene, 10% sodium hydroxide solution of 5-13 part, 3-5 parts of polyvinylpyrrolidones, 8-15 parts of fluorubber.
3. a kind of efficient lithium titanate battery slurry according to claim 1, which is characterized in that the modified epoxy glue
It is made by the following method:
(1) bisphenol-A is added in dissolution kettle, epoxy chloroethanes and benzene is added, at the uniform velocity stir and be warming up to 75 DEG C, stirring 30min
After be transferred in reaction kettle, be added 10% sodium hydroxide solution, be warming up to 45 DEG C, at the uniform velocity stirring 2h, filtering, stand, benzene is molten
Liquid is pumped in reflux benzene kettle, is back to the benzene steamed and droplet does not occur, is stood cooling 45min, is transferred in de- benzene kettle,
It is decompressed to no distillate at 135 DEG C, takes out, dry obtained epoxy resin；
(2) polypropylene glycol is added in three-necked flask, is warming up to 110 DEG C of vacuum dehydration 2h, phthalic anhydride is added, is warming up to
150 DEG C, at this temperature react 5h be made carboxyl end group polyethers, take out, mixed in beaker with epoxy resin, 85 DEG C heating until
Fusing is stirring evenly and then adding into polyvinylpyrrolidone, and taking-up standing 1h obtains mixture after reacting 3h；
(3) fluorubber is mixed with mixture, is poured into ball mill, high speed ball milling, ball milling knot are carried out with the revolving speed of 1600r/min
It is added after beam in the beaker equipped with 100mL dehydrated alcohol, ultrasonic 30min extracts the air in mixed liquor out, is transferred to vacuum drying
In case, vacuum degree -0.09MPa is controlled, temperature is 65 DEG C, and modified epoxy glue is made in dry 12h.
4. a kind of efficient lithium titanate battery slurry according to claim 1, which is characterized in that the active material is anode
Any one in active material or negative electrode active material.
5. a kind of preparation method of efficient lithium titanate battery slurry, which comprises the steps of:
Step S1, lithium titanate, acetylene black, Ketjen black and modified epoxy glue are heated respectively, it is heat-treated
The heating temperature that lithium titanate and modified epoxy glue are controlled in journey is 120 DEG C, and pressure is -0.10MPa, heating time 20h,
Control acetylene black, the heating temperature of Ketjen black is 160 DEG C, pressure is -0.07MPa, heating time 25h, and heat treatment terminates
It takes out afterwards and stands 2h, it is spare；
Step S2, modified epoxy glue and 20% dimethyl sulphoxide aqueous solution are added in agitator tank, control agitator tank vacuum
Degree is -0.09MPa, and control agitator tank revolution revolving speed is 50r/min, and rotation revolving speed is 280r/min, is mixed after stirring 2h
Liquid stands 5h, spare；
Step S3, it by acetylene black, Ketjen black mixed grinding, sieves with 100 mesh sieve, is added in the mixed liquor of step S1 preparation, be added and live
Property substance and lithium titanate, control agitator tank vacuum degree is -0.08MPa, and control agitator tank revolution revolving speed is 45r/min, is walked around certainly
Speed is 300r/min, stirs to the viscosity of mixed slurry in 2000-2500mpas, obtains premix slurry；
Step S4, premix slurry is transferred in batch mixer and is stirred, control vacuum degree is -0.08MPa, and control agitator tank is public
Speed of walking around is 20r/min, and rotation revolving speed is 500r/min, takes out after stirring 30min, crosses 200 meshes, and efficient lithium titanate electricity is made
Pond slurry.
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