CN105932226B - Drying method of battery pole piece - Google Patents
Drying method of battery pole piece Download PDFInfo
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- CN105932226B CN105932226B CN201610334686.7A CN201610334686A CN105932226B CN 105932226 B CN105932226 B CN 105932226B CN 201610334686 A CN201610334686 A CN 201610334686A CN 105932226 B CN105932226 B CN 105932226B
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
- B05D3/0263—After-treatment with IR heaters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
- B05D3/0406—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
- B05D3/0413—Heating with air
-
- 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)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The application relates to the field of lithium ion batteries, in particular to a drying method of a battery pole piece. At least comprises the following steps: coating slurry with N-methyl pyrrolidone as a solvent on the pole piece, and then drying at 50-81 ℃. The method is based on the saturated vapor pressure principle and the explosion limit theory, and realizes the low-temperature drying process by controlling and controlling the slurry and the coating process parameters, so that the production is in a 100% safety state, the efficiency of an NMP recovery system is improved, and the energy consumption of NMP recovery is greatly reduced.
Description
Technical field
This application involves field of lithium ion battery, specifically, are related to a kind of drying means of battery pole piece.
Background technology
Safety is the most important thing of production enterprise.In order to control the risk of explosion in coating drying process, ensure safety
Production, country and manufacturing enterprise all take many measures.
In cell production process, NMP gas concentrations are the important references amounts for ensureing safety in production or proposing production, for reality
When detection baking oven in NMP gas concentrations, Some Enterprises can install online NMP gas detection alarm devices.Online NMP gas detections
Device is the detection device based on principle of catalyst combustion.By the catalytic action of catalyst, in catalyst surface nothing occurs for NMP gases
Flame burns, and discharges heat, causes gas sensor resistance to increase, resistance amplification and NMP gas concentrations are directly proportional.NMP gas detections
The included circuit of device can measure resistance amplification, export corresponding concentration values.
In cell production process, need that NMP recovery systems are installed.NMP recovery systems by air inlet, heat sink, go out
Air port forms.Fresh air is constantly sent to baking oven by NMP recovery systems, and takes the gaseous mixture in baking oven away, to make NMP gas
Bulk concentration is less than lower explosion limit.The gaseous mixture taken away cools down by heat sink, and NMP therein reaches saturated concentration and is condensed back to
It receives.By cooling down, condensed gas is discharged through exhaust outlet.Since national standard GB50493-2009 is provided, air combustible gas concentration
It is not to be exceeded the 25% of its lower explosion limit.Although NMP recovery systems can effectively reduce NMP gas concentrations in baking oven, take out
NMP concentration is too low (≤25%) in the gaseous mixture walked, and causes the organic efficiency of NMP recovery systems relatively low.Currently, enterprise is in order to protect
Barrier safety in production needs the power for improving NMP recovery systems so that the production cost increases.
Although online NMP gas-monitorings alarm can monitor NMP gas concentrations in baking oven in real time.But due to NMP gas
Body being unevenly distributed in baking oven, NMP gas detection alarms are a kind of measurement methods of one-point measurement.In baking oven
Some regions, NMP concentration can exceed that lower explosion limit, and detector cannot effectively be found.Increase NMP detector numbers
Amount realizes multimetering, although NMP gas concentrations in baking oven can be obtained more fully, provides for safety in production judgement and more may be used
The data leaned on.But increasing NMP detectors causes cost to increase.Meanwhile online NMP detectors failure rate is high,
It is susceptible to measured deviation and influences recognition accuracy of the enterprise to risk.Therefore, there are still latent in lithium ion battery production
Security risk.
In view of the deficiencies in the prior art, special to propose the application.
Invention content
Present invention purpose is to propose a kind of drying means of battery pole piece.
In order to complete the purpose of the application, the technical solution used for：
This application involves a kind of drying means of battery pole piece, at least include the following steps：Coating solvent is on pole piece
The slurry of N-Methyl pyrrolidone, is then dried, and dry temperature is 50~81 DEG C.
Preferably, in the drying process, the gas concentration for controlling N-Methyl pyrrolidone in baking oven is N- crassitudes
The 50%~98% of ketone gas burst least concentration.
Preferably, the solid content in the slurry is 1~100%, preferably 30~100%.
Preferably, the width of the coating is 0.1~1000cm, preferably 30~100cm.
Preferably, the surface density of the coating is 1.0~5.0g/cm2, preferably 2.0~5.0g/cm2。
Preferably, the speed of the coating is 0.1~10m/min, preferably 0.1~2m/min.
Preferably, the mode of the drying includes at least one of heated-air drying or infra-red drying.
Preferably, the intake of the heated-air drying is 1000~16000m3/ hour, preferably 8000~10000m3/ small
When.
Preferably, the coating method includes continuous coating, interval coating.
Preferably, the battery pole piece is anode pole piece, contains positive electrode active materials, conductive addition in the anode pole piece
Agent and adhesive, wherein the positive electrode active materials are selected from cobalt acid lithium, lithium titanate, nickel cobalt aluminium, mangaic acid reason, nickel-cobalt-manganese ternary material
At least one of material, LiFePO4, the conductive additive are selected from SP, KS-6, acetylene black；The adhesive is selected from PVDF.
The application at least can reach following advantageous effect：
The application is based on saturated vapor pressure principle and explosion limit is theoretical, regulates and controls slurry and coating process parameter by control,
Low temperature drying technology is realized, to make production be in 100% safe condition, and improves NMP recovery system efficiency, significantly
Reduce NMP recycling energy consumptions.
With reference to specific embodiment, the application is expanded on further.It should be understood that these embodiments are merely to illustrate the application
Rather than limitation scope of the present application.
Specific implementation mode
Present application relates generally to a kind of drying means of pole piece.In the preparation process of lithium ion battery, including slurrying, painting
The processing procedures such as cloth, drying, roll-in, cutting, winding.A kind of innovative be used as N-Methyl pyrrolidone that propose of the application is starched
Expect the low temperature drying method of solvent.Wherein, drying refers to the process of the solvent volatilization in wet film in certain heating device.
N-Methyl pyrrolidone (NMP) is a kind of colourless transparent liquid.- 24.4 DEG C of fusing point, 204 DEG C of boiling point, 95 DEG C of flash-point,
Difficult volatilization, has good thermal stability and chemical stability under room temperature.It is answered extensively because of its good physical and chemical performance
For lithium ion battery industry.Currently, the slurry coating for making solvent with NMP all uses high temperature drying processes, drying temperature to be up to
100~140 DEG C, which is higher than the flash temperature (95 DEG C) of NMP.Under the conditions of existing high temperature drying processes, in slurry
NMP becomes gas, a large amount of to volatilize, and NMP gas concentrations in air is made constantly to increase.If concentration is more than lower explosion limit, just there is hair
The risk of raw explosion, massive losses are brought to enterprise.For this purpose, enterprise limits from the angle of safety in production and according to relevant regulations
Under 100~140 DEG C of drying temperature, in drying box the concentration of NMP air is not to be exceeded the 25% of its lower explosion limit.This
Although behave has ensured safety, but since the concentration of NMP air in drying box is relatively low, lead to the organic efficiency of NMP recovery systems
It is relatively low.
In the technical solution of the application, best do is calculated by explosion limit principle and saturated vapor pressure principle
Dry temperature.
In confined condition, at a certain temperature, it is in pressure possessed by the steam to balance each other with solid or liquid and claims
For vapour pressure.In confined condition, at a certain temperature, it is in pressure possessed by the steam to balance each other with solid or liquid and claims
For vapour pressure.Same substance has different vapour pressures at different temperatures, and increases with the raising of temperature.Work as gaseous pressure
Increasing, gas molecule can be converted into liquid, and when gaseous pressure reduces, fluid molecule in turn translates into gas.
Combustible (fuel gas, steam and dust) must be in certain concentration range uniformly with air (or oxygen)
Mixing forms premix gas, and meeting ignition source can just explode, this concentration range is known as explosion limit or the explosion ratio limit.
Explosion limit principle refers to that when combustable gas concentration is too high or too low in air, mixed gas will not explode, only
When flammable gas concentration is between a certain range, mixed gas is possible to explode.The minimum of the range is known as under exploding
It limits (LEL), maximum value is known as upper explosion limit (UEL).
According to the data (being checked in by data) of lower explosion limit, the saturated vapor pressure of NMP is calculated, calculation formula is：
y≈LEL×Patm
Wherein, PatmIndicate an atmospheric pressure.
The calculation formula of the corresponding temperature of the lower explosion limit of NMP is：
Y=3.89 × 10-8×x4-2.87×10-6×x3+1.61×10-4×x2-2.50×10-3×x+0.0264
Wherein, x is temperature, and y is saturated vapor pressure.
It is calculated by above-mentioned formula, the corresponding temperature of NMP lower explosion limit is 83.15 DEG C.
The application ensures that drying temperature is less than 83.15 DEG C, wherein in the drying process that drying temperature refers to, moisture membrane surface is surveyed
The temperature measured.In this application, in order to further guarantee safe production, dry maximum temperature is set in 81 DEG C.
Under the drying temperature, it is only necessary to which the gas concentration for controlling N-Methyl pyrrolidone in baking oven is N- crassitudes
The 50%~98% of ketone gas burst least concentration.Under the temperature condition of the application, when NMP partial pressures are high in baking oven
When set temperature corresponding saturated vapor pressure, NMP gases will condense, therefore the concentration of NMP gases does not exceed under explosion
Limit, thus will not explode.Simultaneously as NMP gas concentrations increase so that the amount that unit air takes away NMP increases, from
And the organic efficiency of NMP recovery systems is improved, achieve the purpose that reduce NMP cost recovery.
Under the conditions of room temperature is to 140 DEG C, the gas concentration of NMP gas burst lower limits is 1.3%, that is, controls NMP gases
The 50%~98% of a concentration of 1.3%.
Slurry in the application is prepared by pulping process, and pulping process refers to adding active material with conductive
The powder body materials such as agent, adhesive are uniformly distributed technical process in a solvent；Coating process refer to by slurry by coating machine with
Certain coating method is applied on collector base material, is the manufacturing process that slurry forms a film in collection liquid surface.Collector can be
Aluminium foil, copper foil.
In the application by way of rationally controlling slurry solid content, tape running speed, coating width, coated face density, and
Ensure that drying temperature is less than the corresponding temperature of NMP gas burst lower limits (83.15 DEG C).
As a kind of improvement of the application preparation method, the solid content in slurry is 1~100%, preferably 30~100%.
Solid content refers to the ratio of the quality and slurry gross mass of above-mentioned all powder body materials.Solid content is excessively high to cause slurry can not
It squeezes out；It is too low may cause it is dry insufficient.
As a kind of improvement of the application preparation method, the width of coating is 0.1~1000cm, preferably 30~100cm.It is wide
Degree is the effective width of coating.Coating width crosses conference and causes pole piece drying insufficient.
As a kind of improvement of the application preparation method, the surface density of coating is 1.0~5.0g/cm2, preferably 2.0~
5.0g/cm2.Surface density is the quality of unit area coating after drying, and excessively high pole piece drying is insufficient, too low, makes battery core energy
Density is too low.Face to face when consistent in density, the solid content the high more is conducive to drying.
As a kind of improvement of the application preparation method, the speed of coating is 0.1~10m/min, preferably 0.1~2m/
min.Tape running speed refers to the length that base material is passed by the unit interval.Excessive velocities are then dried insufficient.
As a kind of improvement of the application preparation method, dry mode include in heated-air drying or infra-red drying at least
It is a kind of.
As a kind of improvement of the application preparation method, the intake of heated-air drying is 1000~16000m3It is/hour, excellent
Select 8000~10000m3/ hour.Intake refers to the volume for the fresh air being supplemented into the unit interval in baking oven.
As a kind of improvement of the application preparation method, coating method includes continuous coating, interval coating.Institute in the application
The coating apparatus of use includes extrusion coated equipment, spraying equipment, transfer coated equipment, spin-coating equipment etc..
As a kind of improvement of the application preparation method, battery pole piece is anode pole piece, is lived containing anode in anode pole piece
Property material, conductive additive and adhesive, wherein positive electrode active materials be selected from cobalt acid lithium, lithium titanate, nickel cobalt aluminium, mangaic acid reason, nickel
At least one of cobalt-manganese ternary material, LiFePO4, conductive additive are selected from SP, KS-6, acetylene black；Adhesive is selected from
PVDF。
Production safety can not only be ensured using the technique of the application, and it is larger that NMP organic efficiencies can be made to obtain
It is promoted, NMP organic efficiencies can reach 75% or so.Wherein, NMP organic efficiencies refer in the set time recycling NMP mass with
The ratio between Theoretical Mass before recycling.The obtained NMP gas concentrations of recycling are the NMP gas by NMP recovery system air inlets position
Physical examination is surveyed alarm measurement and is obtained.NMP gas detection equipments use herein are based on principle of catalyst combustion.
Embodiment 1
Match anode sizing agent with positive active material, formula is as shown in table 1, and coating method is continuous using extrusion coated equipment
Coating.Coating and dry parameter and condition are as shown in table 2, wherein the gas concentration of LEL is 1.3%.Drying mode is two-sided
Heated-air drying；NMP gas concentrations are detected by NMP gas detection alarms in coating process, and calculate NMP organic efficiencies.Effect
Fruit data are as shown in table 4.
Table 1：Anode pole piece formula
Table 2：Coating and dry parameter
| Number | Drying temperature | Gas concentration | Solid content | Coated face density | Coating width | Tape running speed |
| 1-1 | 60℃ | 30%LEL | 70% | 30mg/cm2 | 60cm | 1m/min |
| 1-2 | 70℃ | 58%LEL | 50% | 20mg/cm2 | 60cm | 1m/min |
| 1-3 | 75℃ | 75%LEL | 50% | 25mg/cm2 | 30cm | 1m/min |
| 1-4 | 80℃ | 98%LEL | 60% | 26mg/cm2 | 60cm | 1m/min |
| 1-5 | 80℃ | 98%LEL | 70% | 26mg/cm2 | 60cm | 1m/min |
Comparative example
The slurry (as shown in table 1) being formulated using embodiment 1 is coated and is dried, and difference lies in drying condition such as tables 3
Shown, effect data is as shown in table 4.
Table 3：Coating and dry parameter
| Number | Drying temperature | Gas concentration | Solid content | Coated face density | Coating width | Tape running speed |
| D1-1 | 120℃ | 20%LEL | 70% | 30mg/cm2 | 60cm | 35m/min |
| D1-2 | 125℃ | 23%LEL | 50% | 20mg/cm2 | 60cm | 25m/min |
| D1-3 | 135℃ | 24%LEL | 50% | 25mg/cm2 | 30cm | 25m/min |
| D1-4 | 110℃ | 20%LEL | 60% | 26mg/cm2 | 60cm | 25m/min |
| D1-5 | 130℃ | 20%LEL | 70% | 26mg/cm2 | 60cm | 25m/min |
Note：In the comparative example, it is provided according to national standard GB50493-2009, combustable gas concentration is no more than 20 ± 5%LEL.
The reason is that when temperature is higher than 82 DEG C, local NMP gas concentrations may be more than lower explosion limit, and risk of explosion is very high.Therefore it is
Ensure safety in production, needs strictly to control the NMP gas concentrations under high temperature in baking oven, be allowed to be less than 25%.
Table 4：The efficacy parameter of experimental example and comparative example
| Number | NMP organic efficiencies | Intake |
| 1-1 | 70% | 9000 |
| 1-2 | 80% | 8000 |
| 1-3 | 80% | 8500 |
| 1-4 | 60% | 9000 |
| 1-5 | 75% | 9100 |
| D1-1 | 40% | 13000 |
| D1-2 | 50% | 15000 |
| D1-3 | 50% | 14400 |
| D1-4 | 45% | 16000 |
| D1-5 | 41% | 16050 |
Embodiment 2
Match anode sizing agent with positive active material, be formulated as shown in the 1-1 in embodiment 1, coating method is using extruding
Coating apparatus interval is coated with.Coating and dry parameter and condition are as shown in table 5, and drying mode is infra-red drying.Coating process
In NMP gas concentrations are detected by NMP gas detection alarms, effect data is as shown in table 6.
Table 5：Coating and dry parameter
| Number | Drying temperature | Gas concentration | Solid content | Coated face density | Coating width | Tape running speed |
| 2-1 | 60℃ | 30%LEL | 70% | 30mg/cm2 | 60cm | 2m/min |
| 2-2 | 70℃ | 55%LEL | 58% | 20mg/cm2 | 40cm | 4m/min |
| 2-3 | 75℃ | 75%LEL | 50% | 25mg/cm2 | 50cm | 6m/min |
| 2-4 | 80℃ | 98%LEL | 60% | 26mg/cm2 | 70cm | 8m/min |
| 2-5 | 80℃ | 96%LEL | 70% | 26mg/cm2 | 100cm | 10m/min |
| D2-1 | 120℃ | 22%LEL | 70% | 30mg/cm2 | 60cm | 50m/min |
| D2-2 | 125℃ | 23%LEL | 58% | 20mg/cm2 | 40cm | 50m/min |
| D2-3 | 135℃ | 24%LEL | 50% | 25mg/cm2 | 50cm | 45m/min |
| D2-4 | 110℃ | 22%LEL | 60% | 26mg/cm2 | 70cm | 45m/min |
| D2-5 | 130℃ | 25%LEL | 70% | 26mg/cm2 | 100cm | 45m/min |
Table 6：The efficacy parameter of experimental example and comparative example
| Number | NMP organic efficiencies | Intake |
| 2-1 | 70% | 9200 |
| 2-2 | 80% | 8100 |
| 2-3 | 80% | 8800 |
| 2-4 | 60% | 9300 |
| 2-5 | 75% | 9100 |
| D2-1 | 48% | 14000 |
| D2-2 | 55% | 15500 |
| D2-3 | 53% | 15400 |
| D2-4 | 50% | 16100 |
| D2-5 | 45% | 16250 |
It is not for limiting claim, any this field skill although the application is disclosed as above with preferred embodiment
Art personnel can make several possible variations and modification under the premise of not departing from the application design, therefore the application
Protection domain should be subject to the range that the application claim is defined.
Claims (10)
1. a kind of drying means of battery pole piece, which is characterized in that at least include the following steps：Coating solvent is N- on pole piece
The slurry of methyl pyrrolidone, is then dried, and dry temperature is 50~81 DEG C, in the drying process, controls in baking oven
The gas concentration of N-Methyl pyrrolidone is the 50%~98% of N-Methyl pyrrolidone gas burst least concentration.
2. drying means according to claim 1, which is characterized in that the solid content in the slurry is 30~70%.
3. drying means according to claim 1, which is characterized in that the width of the coating is 30~100cm.
4. drying means according to claim 1, which is characterized in that the surface density of the coating is 2.0~5.0g/cm2。
5. drying means according to claim 1, which is characterized in that the speed of the coating is 0.1~10m/min.
6. drying means according to claim 5, which is characterized in that the speed of the coating is 0.1~2m/min.
7. drying means according to claim 1, which is characterized in that the mode of the drying includes heated-air drying or infrared
It is at least one of dry.
8. drying means according to claim 7, which is characterized in that the intake of the heated-air drying be 8000~
10000m3/ hour.
9. drying means according to claim 1, which is characterized in that the coating method includes that continuous coating or interval apply
Cloth.
10. drying means according to claim 1, which is characterized in that the battery pole piece is anode pole piece, the anode
Contain positive electrode active materials, conductive additive and adhesive in pole piece, wherein the positive electrode active materials are selected from cobalt acid lithium, titanium
At least one of sour lithium, nickel cobalt aluminium, mangaic acid reason, nickel-cobalt-manganese ternary material, LiFePO4, the conductive additive are selected from KS-
6, acetylene black；The adhesive is selected from PVDF.
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| JP6845056B2 (en) * | 2017-03-21 | 2021-03-17 | 株式会社Ｓｃｒｅｅｎホールディングス | Coating device and coating method |
| CN109490467A (en) * | 2017-09-13 | 2019-03-19 | 河北银隆新能源有限公司 | The prior-warning device and method for early warning of NMP concentration over-standard in lithium titanate battery coating process |
| CN108682853B (en) * | 2018-04-24 | 2020-09-08 | 江西省金锂科技股份有限公司 | Preparation method of lithium iron phosphate and lithium iron phosphate cathode material prepared by same |
| CN108923090A (en) * | 2018-05-29 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of carbon-coated lithium iron manganese phosphate anode material is prepared from waste lithium iron phosphate battery recycling |
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| CN101262077A (en) * | 2008-04-29 | 2008-09-10 | 上海德朗能电池有限公司 | A high-capacity secure 26650 lithium ion battery and its making method |
| KR101475429B1 (en) * | 2012-05-15 | 2014-12-23 | 주식회사 엘지화학 | Flow Controller of Drying Oven with Automatic Air Charge for Manufacturing Secondary Battery |
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