CN106025268A - Water-based lithium battery cathode slurry and preparation method thereof - Google Patents
Water-based lithium battery cathode slurry and preparation method thereof Download PDFInfo
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- CN106025268A CN106025268A CN201610552948.7A CN201610552948A CN106025268A CN 106025268 A CN106025268 A CN 106025268A CN 201610552948 A CN201610552948 A CN 201610552948A CN 106025268 A CN106025268 A CN 106025268A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/621—Binders
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a method for preparing water-based lithium battery cathode slurry. The method comprises the following steps: selecting a lithium manganate or lithium nickel manganese cobalt material as a cathode active material, a mixture of SP and KS-6 as a conductive agent, SBR or LA133 as a water-based adhesive and deionized water as a solvent. The slurry is excellent in stability, good in processing performance and high in pole piece bonding strength, and the production cost, the pollution to environment and damage to human health are greatly reduced.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to the preparation side of a kind of lithium battery water system anode sizing agent
Method.
Background technology
Lithium ion battery has high voltage, high-energy, have extended cycle life and the advantage such as memory-less effect, is considered green high
Energy battery is first-selected, extensively applies in 3C product, at new-energy automobile (including pure electronic, hybrid power etc.), electrical salf-walking
The fields such as car and other electric walk instead instrument are the most progressively applied popularization.The quality of performance of lithium ion battery will directly affect electricity
Electrical automobile and the application of energy storage industry and fast development.
Positive electrode is one of key factor determining performance of lithium ion battery, but the many employings of positive electrode current slurry are with NMP
(N-Methyl pyrrolidone) is the oil system system of organic solvent, and this solvent usage amount is big, reclaims difficulty, and use cost is high, to ecology
Environmental pollution is big, and healthy to production operation workman also has an impact.Therefore, the water system positive pole slurry of a kind of excellent performance is developed
Material has very important practical significance.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of lithium battery aqueous positive-pole slurry, the method can effectively solve oil
It is the deficiency existing for anode sizing agent and problem.
The technical scheme is that
The present invention comprises the following steps:
A adds deionized water in de-airing mixer, adds binding agent, described deionized water and the mass ratio of described binding agent
It is 1～5:1, after described de-airing mixer is with revolution mode stirring at low speed 10min, carries out vacuum moderate-speed mixer in rotation mode
Glue is obtained after 30min；
B adds conductive agent in described glue, and the mass ratio of described glue and described conductive agent is 10～15:1, and described vacuum is stirred
Machine of mixing is with mode stirring at low speed 10min that revolves round the sun, it is ensured that the pressed powder of described conductive agent is all infiltrated, described de-airing mixer
High-speed stirred 1-2h after vacuum moderate-speed mixer 30min is carried out in rotation mode；
C adds the positive active material of total amount 50% in described glue, and described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 1h after empty moderate-speed mixer 30min；
Adding remaining described positive active material in glue described in D, described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 2h after empty moderate-speed mixer 30min；
E carries out slurry viscosity test to described glue, controls the viscosity number of described glue by adding described deionized water
Between 3000-6000cp, described de-airing mixer, with moderate-speed mixer 30min, makes viscosity number reach requirement；
F discharging of sieving described glue obtains slurry.
A kind of preparation method of lithium battery water system anode sizing agent, it is characterised in that: comprise the following steps:
A adds deionized water in de-airing mixer, adds thickening agent, described deionized water and the mass ratio of described thickening agent
It is 40～110:1, after described de-airing mixer is with revolution mode stirring at low speed 10min, carries out vacuum middling speed in rotation mode and stir
Mix high-speed stirred 2h after 30min；
B adds conductive agent in described glue, and the mass ratio of described glue and described conductive agent is 10～25:1, and described vacuum is stirred
Machine of mixing is with mode stirring at low speed 10min that revolves round the sun, it is ensured that the pressed powder of described conductive agent is all infiltrated, described de-airing mixer
High-speed stirred 1-2h after vacuum moderate-speed mixer 30min is carried out in rotation mode；
C adds the positive active material of total amount 50% in described glue, and described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 1h after empty moderate-speed mixer 30min；
Adding remaining described positive active material in glue described in d, described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 2h after empty moderate-speed mixer 30min；
E carries out slurry viscosity test to described glue, controls the viscosity number of described glue by adding described deionized water
Between 3000-6000cp, described de-airing mixer, with moderate-speed mixer 30min, makes viscosity number reach requirement；
F adds SBR binding agent, discharging of sieving after stirring at low speed 30min in described glue.
Specifically, described positive active material is LiMn2O4 or nickle cobalt lithium manganate, and the quality of described positive active material contains
Amount ratio is 85～95%；
Specifically, described binding agent is LA133 or SBR, and thickening agent is CMC, and quality is 2%～8% than content, and LA133's is main
Composition is acrylic-multipolymer, solid content 15%, and SBR is mainly composed of butadiene-styrene rubber, solid content 40%, CMC solid content
It is 91%.
Specifically, described conductive agent is the mixture of SP and KS-6, and described SP and described KS-6 mass are respectively 1 than content
～5:1.
Specifically, the solid content of described slurry is 45%～65%；
Specifically, reaction temperature is less than 45 DEG C when stirring for described glue, and during stirring, glue temperature can rise, and stirring is conducive to
Glue temperature dispels the heat.
Specifically, the vacuum of described de-airing mixer is more than-0.095MPa.
Specifically, the speed of described stirring at low speed is revolution 10～15Hz, rotation 0rpm；The speed of moderate-speed mixer is revolution
20～30Hz, rotation 1000～2000rpm；The speed of high-speed stirred is revolution 40～50Hz, rotation 3000～4000rpm.
The present invention use deionized water as the solvent of anode sizing agent, and aqueous binders, greatly reduce lithium battery
Production cost, reduces the pollution to operator and environment, and size performance is stable, excellent.
Detailed description of the invention
Below by detailed description of the invention, the present invention will be further described in detail.
Embodiment 1
The concrete process for preparation of the present embodiment water system anode sizing agent is as follows:
A adds 1600g deionized water in de-airing mixer, is subsequently adding 36g thickening agent CMC, with 10Hz stirring of revolving round the sun
10min, then scraper, with the 20Hz that revolves round the sun, rotation 1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation
3500rpm stirs 2h；
B adds conductive agent, 98gSP and 33gKS-6, and to revolve round the sun, 10Hz stirs 10min, then scraper, with the 20Hz that revolves round the sun, rotation
1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation 3500rpm stirs 2h；.
C adds 1500g lithium manganate cathode active substance, and to revolve round the sun, 10Hz stirs 10min, then scraper, with the 20Hz that revolves round the sun, rotation
1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation 3500rpm stirs 1h；
D adds 1500g lithium manganate cathode active substance, and to revolve round the sun, 10Hz stirs 10min, then scraper, with the 20Hz that revolves round the sun, from
Turn 1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation 3500rpm stirs 2h；
E adds 770g deionized water, with the 25Hz that revolves round the sun, rotation 1500rpm vacuum stirring 30min；
F adds 245g binding agent SBR, and with the 15Hz that revolves round the sun, rotation 500rpm vacuum stirring 30min, then 100 mesh sieves crossed by slurry,
Discharging.
Embodiment 2
The concrete process for preparation of the present embodiment water system anode sizing agent is as follows:
A adds 835g deionized water in de-airing mixer, is subsequently adding 645g binding agent LA133N, with 10Hz stirring of revolving round the sun
10min, then with the 20Hz that revolves round the sun, rotation 1000rpm vacuum stirring 30min；
B adds conductive agent, 97gSP and 32gKS-6, and to revolve round the sun, 10Hz stirs 10min, then scraper, with the 20Hz that revolves round the sun, rotation
1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation 3500rpm stirs 2h；
C adds 1500g lithium manganate cathode active substance, and to revolve round the sun, 10Hz stirs 10min, then scraper, with the 20Hz that revolves round the sun, rotation
1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation 3500rpm stirs 1h；
D adds 1500g lithium manganate cathode active substance, and to revolve round the sun, 10Hz stirs 10min, then scraper, with the 20Hz that revolves round the sun, from
Turn 1000rpm vacuum stirring 30min；The most again with the 40Hz that revolves round the sun, rotation 3500rpm stirs 2h；
E adds 770g deionized water, with the 25Hz that revolves round the sun, rotation 1500rpm vacuum stirring 30min；
F slurry crosses 100 mesh sieves, discharging.
Comparative example 1
The addition of binding agent LA133 in embodiment 2 is become 870g, and remaining step is same as in Example 2.
Comparative example 2
The addition of binding agent LA133 in embodiment 2 is become 1100g, and remaining step is same as in Example 2.
Comparative example 3
Changing positive active material in embodiment 2 into nickle cobalt lithium manganate, remaining step is same as in Example 2.
Anode sizing agent prepared by above example and comparative example is coated, roll-in, test its pole piece performance and slurry
Performance.
Table 1 embodiment and comparative example slurry and pole piece the performance test results
Using LA133 higher as the slurry solid content of binding agent as can be seen from Table 1, stability is more preferable, the bonding of pole piece
Power is the most higher；And the increase of LA133 addition is not obviously improved the performance of slurry and the cohesive force of pole piece, and slurry viscosity is relatively
Height, is unfavorable for following process, therefore uses the addition of LA133 in embodiment 2 the most suitable；The stability of LiMn2O4 slurry is better than
Nickle cobalt lithium manganate slurry.
Embodiment of above is only the illustrative embodiments that the present invention is described, but it is not restricted to description
Listed utilization, for those skilled in the art, is easily achieved other amendment and improvement with in embodiment, because of
This is under the general concept limited without departing substantially from claim and equivalency range, and these amendments and improvement are also considered as the guarantor of the present invention
Protect scope.
Claims (9)
1. the preparation method of a lithium battery water system anode sizing agent, it is characterised in that: comprise the following steps:
A adds deionized water in de-airing mixer, adds binding agent, described deionized water and the mass ratio of described binding agent
It is 1～5:1, after described de-airing mixer is with revolution mode stirring at low speed 10min, carries out vacuum moderate-speed mixer in rotation mode
Glue is obtained after 30min；
B adds conductive agent in described glue, and the mass ratio of described glue and described conductive agent is 10～15:1, and described vacuum is stirred
Machine of mixing is with mode stirring at low speed 10min that revolves round the sun, it is ensured that the pressed powder of described conductive agent is all infiltrated, described de-airing mixer
High-speed stirred 1-2h after vacuum moderate-speed mixer 30min is carried out in rotation mode；
C adds the positive active material of total amount 50% in described glue, and described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 1h after empty moderate-speed mixer 30min；
Adding remaining described positive active material in glue described in D, described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 2h after empty moderate-speed mixer 30min；
E carries out slurry viscosity test to described glue, controls the viscosity number of described glue by adding described deionized water
Between 3000-6000cp, described de-airing mixer, with moderate-speed mixer 30min, makes viscosity number reach requirement；
F discharging of sieving described glue obtains slurry.
2. the preparation method of a lithium battery water system anode sizing agent, it is characterised in that: comprise the following steps:
A adds deionized water in de-airing mixer, adds thickening agent, described deionized water and the mass ratio of described thickening agent
It is 40～110:1, after described de-airing mixer is with revolution mode stirring at low speed 10min, carries out vacuum middling speed in rotation mode and stir
Mix high-speed stirred 2h after 30min；
B adds conductive agent in described glue, and the mass ratio of described glue and described conductive agent is 10～25:1, and described vacuum is stirred
Machine of mixing is with mode stirring at low speed 10min that revolves round the sun, it is ensured that the pressed powder of described conductive agent is all infiltrated, described de-airing mixer
High-speed stirred 1-2h after vacuum moderate-speed mixer 30min is carried out in rotation mode；
C adds the positive active material of total amount 50% in described glue, and described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 1h after empty moderate-speed mixer 30min；
Adding remaining described positive active material in glue described in d, described de-airing mixer is with the mode stirring at low speed that revolves round the sun
10min, it is ensured that the pressed powder of described positive active material is all infiltrated, described de-airing mixer is carried out very in rotation mode
High-speed stirred 2h after empty moderate-speed mixer 30min；
E carries out slurry viscosity test to described glue, controls the viscosity number of described glue by adding described deionized water
Between 3000-6000cp, described de-airing mixer, with moderate-speed mixer 30min, makes viscosity number reach requirement；
F adds SBR binding agent, discharging of sieving after stirring at low speed 30min in described glue.
3. the preparation method of lithium battery anode slurry as claimed in claim 1, it is characterised in that: described positive active material is manganese
Acid lithium or nickle cobalt lithium manganate, the mass content ratio of described positive active material is 85～95%.
4. the preparation method of as claimed in claim 1 lithium battery anode slurry, it is characterised in that: described binding agent be LA133 or
SBR, thickening agent is CMC, and quality is 2%～8% than content, and LA133 is mainly composed of acrylic-multipolymer, solid content
15%, SBR are mainly composed of butadiene-styrene rubber, solid content 40%, and CMC solid content is 91%.
5. the preparation method of lithium battery anode slurry as claimed in claim 1, it is characterised in that: described conductive agent is SP and KS-6
Mixture, described SP and described KS-6 mass are respectively 1～5:1 than content.
6. the preparation method of lithium battery anode slurry as claimed in claim 1, it is characterised in that: the solid content of described slurry is
45%～65%.
7. the preparation method of lithium battery anode slurry as claimed in claim 1, it is characterised in that: the reaction when stirring of described glue
Temperature is less than 45 DEG C.
8. the preparation method of lithium battery anode slurry as claimed in claim 1, it is characterised in that: the vacuum of described de-airing mixer
Degree is more than-0.095MPa.
9. the preparation method of lithium battery anode slurry as claimed in claim 1, it is characterised in that: the speed of described stirring at low speed is
Revolution 10～15Hz, rotation 0rpm；The speed of moderate-speed mixer is revolution 20～30Hz, rotation 1000～2000rpm；High-speed stirred
Speed for revolution 40～50Hz, rotation 3000～4000rpm.
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| CN201610552948.7A CN106025268A (en) | 2016-07-14 | 2016-07-14 | Water-based lithium battery cathode slurry and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106684381A (en) * | 2017-01-13 | 2017-05-17 | 天津中聚新能源科技有限公司 | Aqueous positive paste and preparation method thereof |
| CN107154488A (en) * | 2017-05-22 | 2017-09-12 | 惠州亿纬锂能股份有限公司 | A kind of anode sizing agent, its preparation method and the purposes in lithium ferrous disulfide battery |
| CN107834062A (en) * | 2017-11-20 | 2018-03-23 | 中山市电赢科技有限公司 | A kind of anode constituents of rate battery |
| CN108615889A (en) * | 2018-05-11 | 2018-10-02 | 合肥国轩高科动力能源有限公司 | A kind of single conjunction paste-making method of graphite particle again of lithium ion battery |
| CN108619927A (en) * | 2017-03-19 | 2018-10-09 | 深圳格林德能源有限公司 | A kind of new type lithium ion battery anode sizing agent stirring technique |
| CN109768253A (en) * | 2019-01-11 | 2019-05-17 | 合肥国轩高科动力能源有限公司 | A kind of proportioning process of lithium ion battery negative material |
| CN111029559A (en) * | 2019-12-16 | 2020-04-17 | 银隆新能源股份有限公司 | Lithium titanate battery and preparation method thereof |
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| CN103311504A (en) * | 2013-06-13 | 2013-09-18 | 高平唐一新能源科技有限公司 | Preparation method of lithium-ion battery paste |
| CN103618063A (en) * | 2013-09-26 | 2014-03-05 | 奇瑞汽车股份有限公司 | Lithium ion power battery positive electrode slurry and slurry mixing method |
| CN105206797A (en) * | 2015-09-10 | 2015-12-30 | 中天储能科技有限公司 | Lithium ion battery water-based positive electrode slurry dosing technology |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106684381A (en) * | 2017-01-13 | 2017-05-17 | 天津中聚新能源科技有限公司 | Aqueous positive paste and preparation method thereof |
| CN108619927A (en) * | 2017-03-19 | 2018-10-09 | 深圳格林德能源有限公司 | A kind of new type lithium ion battery anode sizing agent stirring technique |
| CN107154488A (en) * | 2017-05-22 | 2017-09-12 | 惠州亿纬锂能股份有限公司 | A kind of anode sizing agent, its preparation method and the purposes in lithium ferrous disulfide battery |
| CN107154488B (en) * | 2017-05-22 | 2020-03-17 | 惠州亿纬锂能股份有限公司 | Positive electrode slurry, preparation method thereof and application of positive electrode slurry in lithium-ferrous disulfide battery |
| CN107834062A (en) * | 2017-11-20 | 2018-03-23 | 中山市电赢科技有限公司 | A kind of anode constituents of rate battery |
| CN108615889A (en) * | 2018-05-11 | 2018-10-02 | 合肥国轩高科动力能源有限公司 | A kind of single conjunction paste-making method of graphite particle again of lithium ion battery |
| CN109768253A (en) * | 2019-01-11 | 2019-05-17 | 合肥国轩高科动力能源有限公司 | A kind of proportioning process of lithium ion battery negative material |
| CN111029559A (en) * | 2019-12-16 | 2020-04-17 | 银隆新能源股份有限公司 | Lithium titanate battery and preparation method thereof |
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Application publication date: 20161012 |