A kind of lithium ion cell positive dry mixing technique
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of lithium ion cell positive dry mixing technique.
Background technique
Lithium ion battery have many advantages, such as energy density it is high, it is environmental-friendly, have extended cycle life, in 3C number, energy storage, electronic
The fields such as tool, communications and transportation have a wide range of applications.Making technology has the quality of lithium ion battery great influence,
Mixing is the first step of entire making technology, there is important influence to the quality of subsequent technique and lithium ion battery.
Traditional method for mixing of anode material for lithium-ion batteries is material by wet type mixing, concrete mode are as follows: by solvent and binder
It is first mixed, glue is made, then be gradually added conductive agent, the powder body materials such as active material, there are conductive agents, activity for this method
The drawback of the powder body materials such as substance dispersion effect difference in low viscosity glue, while being influenced by binder dissolution characteristics, it is whole
A glue process needs 8-10 hours, takes a long time, mixing low efficiency.
Summary of the invention
It is an object of the invention to overcome deficiency in the prior art, a kind of lithium ion cell positive dry mixing work is provided
Skill solves the problem of existing method for mixing low efficiency bad dispersibility.
To achieve the goals above, the present invention is achieved by the following scheme:
A kind of lithium ion cell positive dry mixing technique, comprising the following steps:
(1) active material and powdered conductive agent are added into a mixing bowl, is stirred;
(2) binder is added into a mixing bowl, is stirred;
(3) solvent for accounting for solvent total weight 50~85% is added into a mixing bowl, is stirred;
(4) pulp-like conductive agent is added into a mixing bowl, is evacuated to -0.085~-0.1MPa, is stirred;
(5) remaining solvent is added, continues to be evacuated to -0.085~-0.1MPa, be stirred, obtain lithium ion battery
Anode sizing agent.
Preferably, in step (1), the condition being stirred includes that mixing speed is 20~25rpm, rate of dispersion
For 1500~1800rpm, being stirred the time is 10~20 minutes.
Preferably, in step (2), the condition being stirred includes that mixing speed is 25~30rpm, rate of dispersion
For 1500~1800rpm, being stirred the time is 10~20 minutes.
Preferably, in step (3), the condition being stirred includes that mixing speed is 25~30rpm, rate of dispersion
For 300~400rpm, being stirred the time is 30 minutes.
Preferably, in step (4), the condition being stirred includes that mixing speed is 33~38rpm, rate of dispersion
For 1500~1800rpm, being stirred the time is 120~180 minutes.
Preferably, in step (5), the condition being stirred includes that mixing speed is 20~25rpm, rate of dispersion
For 200~300rpm, being stirred the time is 30~60 minutes.
Compared with prior art, the present invention has following technical effect that
Lithium ion cell positive dry mixing technique provided by the invention, first step by step be added active material, conductive agent and
Binder carries out powder mixed at high speed, can make the sufficiently broken dispersion of conductive agent aggregate, dry powder high-speed stirred is realized microcosmic mixed
It closes, to form good conductive network;Adding appropriate solvent soaks granular material, stirs at low speed to form high viscosity slurry
Material;Pulp-like conductive agent is supplemented later and the shearing force formed by high speed dispersion is further crushed agglomerated particle, accelerates to dissolve
Binder and evenly dispersed material;Finally supplement residual solvent adjustment viscosity obtains lithium ion battery anode glue size.
The present invention is by the control to charging sequence and mixing procedure condition, so that granular material mixes well, improves
The stability and mixing efficiency of slurry.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is furture elucidated.
All raw materials in the present invention, are not particularly limited its source, buying on the market or according to this field skill
The preparation of conventional method known to art personnel.
All raw materials in the present invention, are not particularly limited its purity, and present invention preferably employs analyze pure or composite wood
The conventional purity that material field uses.
In order to solve existing method for mixing inefficiency, the technical issues of bad dispersibility, the present invention provides a kind of lithium from
Sub- anode dry mixing technique, comprising the following steps:
(1) active material and powdered conductive agent, low whipping speed 20 are added into a mixing bowl of planetary stirring machine
~25rpm, rate of dispersion are stirred 10~20 minutes under conditions of being 1500~1800rpm;
(2) binder is added into a mixing bowl, low whipping speed is 25~30rpm, and rate of dispersion is 1500~1800rpm
Under conditions of be stirred 10~20 minutes;
(3) solvent for accounting for solvent total weight 50~85% is added into a mixing bowl, low whipping speed is 25~30rpm, point
It dissipates under conditions of speed is 300~400rpm and is stirred 30 minutes;
(4) pulp-like conductive agent is added into a mixing bowl, is evacuated to -0.085~-0.1MPa, low whipping speed 33
~38rpm, rate of dispersion are stirred 120~180 minutes under conditions of being 1500~1800rpm;
(5) remaining solvent is added, continues to be evacuated to -0.085~-0.1MPa, low whipping speed is 20~25rpm,
Rate of dispersion is stirred 30~60 minutes under conditions of being 200~300rpm, obtains lithium ion battery anode glue size.
According to the present invention, the present invention does not do particular determination to the type of the active material and powdered conductive agent, can
Think it is well known to those skilled in the art, for example, the active material is LiMn2O4, ternary material, LiFePO4
One or more combinations;The powdered conductive agent is one or more combinations of KS-6, S-O, VGCF, Super P.
According to the present invention, in the present invention, the pulp-like conductive agent is carbon nanotube, one or two kinds of groups of graphene
It closes.
Heretofore described solvent selection prepares the common solvent of lithium ion battery anode glue size, example solvent as mentioned
For NMP;
Heretofore described binder selection prepares the common binder of lithium ion battery anode glue size, and example is as mentioned
Binder is PVDF.
Lithium ion cell positive dry mixing technique provided by the invention is made into one below by way of specific embodiment
The explanation of step.
Embodiment 1
A kind of lithium ion cell positive dry mixing technique, comprising the following steps:
(1) LiMn2O4, Super P and KS-6 powder are added in a mixing bowl of planetary stirring machine, mixing speed
20rpm, rate of dispersion 1650rpm open recirculated water, stir 10 minutes;
(2) PVDF, mixing speed 28rpm, rate of dispersion 1650rpm are added into a mixing bowl, opens recirculated water, stirring 20
Minute;
(3) NMP, mixing speed 30rpm, the rate of dispersion 400rpm for accounting for solvent total weight 68% are added into a mixing bowl,
Recirculated water is opened, is stirred 30 minutes;
(4) carbon nanotube conducting slurry is added into a mixing bowl, mixing speed 35rpm, rate of dispersion 1760rpm are opened
Recirculated water vacuumizes -0.085~-0.1MPa, stirs 165 minutes;
(5) residue NMP, mixing speed 20rpm, rate of dispersion 220rpm is added, opens recirculated water, vacuumizes -0.085
~-0.1MPa is stirred 45 minutes.
Embodiment 2
A kind of lithium ion cell positive dry mixing technique, comprising the following steps:
(1) LiMn2O4, ternary and Super P powder are added in a mixing bowl of planetary stirring machine, mixing speed
20rpm, rate of dispersion 1570rpm open recirculated water, stir 15 minutes;
(2) PVDF, mixing speed 25rpm, rate of dispersion 1600rpm are added into a mixing bowl, opens recirculated water, stirring 20
Minute;
(3) NMP, mixing speed 30rpm, the rate of dispersion 400rpm for accounting for solvent total weight 62% are added into a mixing bowl,
Recirculated water is opened, is stirred 30 minutes;
(4) carbon nanotube conducting slurry is added into a mixing bowl, is evacuated to -0.085~-0.1MPa, mixing speed
38rpm, rate of dispersion 1750rpm open recirculated water, stir 150 minutes;
(5) residue NMP, mixing speed 22rpm, rate of dispersion 200rpm is added, opens recirculated water, vacuumizes -0.085
~-0.1MPa is stirred 40 minutes.
Embodiment 3
A kind of lithium ion cell positive dry mixing technique, comprising the following steps:
(1) LiFePO4, ternary and Super P powder are added in a mixing bowl of planetary stirring machine, mixing speed
22rpm, rate of dispersion 1630rpm open recirculated water, stir 15 minutes;
(2) PVDF, mixing speed 30rpm, rate of dispersion 1680rpm are added into a mixing bowl, opens recirculated water, stirring 15
Minute;
(3) NMP, mixing speed 28rpm, the rate of dispersion 380rpm for accounting for solvent total weight 72% are added into a mixing bowl,
Recirculated water is opened, is stirred 30 minutes;
(4) carbon nanotube conducting slurry is added into a mixing bowl, is evacuated to -0.085~-0.1MPa, mixing speed
38rpm, rate of dispersion 1640rpm open recirculated water, stir 150 minutes;
(5) residue NMP is added, vacuumizes -0.085~-0.1MPa, mixing speed 22rpm, rate of dispersion 260rpm is opened
Recirculated water is opened, is stirred 50 minutes.
Comparative example 1
A kind of lithium ion cell positive mixing procedure, comprising the following steps:
(1) by LiMn2O4, ternary, Super P, PVDF and the NMP addition planetary stirring machine for accounting for solvent total weight 65%
A mixing bowl in, mixing speed 30rpm, rate of dispersion 400rpm, open recirculated water, stir 60 minutes;
(2) carbon nanotube conducting slurry is added into a mixing bowl, mixing speed 38rpm, rate of dispersion 1750rpm take out true
- 0.085~-0.1MPa of sky opens recirculated water, stirs 180 minutes;
(3) residue NMP, mixing speed 22rpm, rate of dispersion 200rpm is added, opens recirculated water, vacuumizes -0.085
~-0.1MPa is stirred 40 minutes.
Comparative example 2
A kind of lithium ion cell positive mixing procedure, comprising the following steps:
(1) LiMn2O4, ternary and PVDF are added in a mixing bowl of planetary stirring machine, mixing speed 30rpm, dispersion speed
400rpm is spent, recirculated water is opened, is stirred 50 minutes;
(2) by Super P, carbon nanotube conducting slurry and the NMP mixing speed 28rpm for accounting for solvent total weight 75%, divide
Speed 350rpm is dissipated, recirculated water is opened, is stirred 60 minutes;
(3) mixing speed 38rpm, rate of dispersion 1750rpm vacuumize -0.085~-0.1MPa, open recirculated water, stir
150 minutes;
(4) residue NMP, mixing speed 22rpm, rate of dispersion 250rpm is added, opens recirculated water, vacuumizes -0.085
~-0.1MPa is stirred 40 minutes.
Comparative example 3
A kind of lithium ion cell positive mixing procedure, comprising the following steps:
(1) by the addition a mixing bowl of PVDF and whole NMP planetary stirring machines, mixing speed 30rpm, rate of dispersion
1380rpm opens recirculated water, stirs 240 minutes;
(2) LiMn2O4, ternary, Super P are added in a mixing bowl, mixing speed 35rpm, rate of dispersion 1550rpm are opened
Recirculated water is opened, -0.085~-0.1MPa is vacuumized, is stirred 180 minutes;
(3) carbon nanotube conducting slurry is added into a mixing bowl, mixing speed 38rpm, rate of dispersion 1550rpm take out true
- 0.085~-0.1MPa of sky opens recirculated water, stirs 90 minutes;
(4) mixing speed 20rpm, rate of dispersion 250rpm open recirculated water, vacuumize -0.085--0.1MPa, stir
30 minutes.
The mixing time of embodiment 1-3, comparative example 1-3, slurry fineness, viscosity and viscosity change are tested, as a result
Such as table 1.
1 mixing time of table and size performance test result
As can be seen from Table 1, the size performance that 1-3 of the embodiment of the present invention is obtained is substantially better than comparative example 1-3.
The present invention is sufficiently effective by the shearing force that granular material high speed dispersion and highly viscous slurry, high dispersive speed are formed
Break up agglomerates, realize the microcosmic uniform mixing of particle, obtained slurry fineness is good, and viscosity stability is high, while it is time-consuming compared with
It is short.Comparative example 1-2 equally uses granular material and highly viscous slurry high speed dispersion, but thin in slurry because feeding sequence is different
Less than having in terms of degree and Stability of Slurry.Comparative example 3 uses conventional wet lay mixing, and glue viscosity low-shearing force is insufficient, dispersion
Effect is poor, therefore Stability of Slurry is bad, simultaneously because PVDF dissolution is slowly, time-consuming for entire ingredient.
Basic principles and main features and the features of the present invention of the invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement is both fallen in the range of claimed invention.The scope of protection of present invention is by appended claims
And its equivalent thereof.