CN103840113B - A kind of preparation method of the polyethylene separators for lithium battery - Google Patents
A kind of preparation method of the polyethylene separators for lithium battery Download PDFInfo
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- CN103840113B CN103840113B CN201410072974.0A CN201410072974A CN103840113B CN 103840113 B CN103840113 B CN 103840113B CN 201410072974 A CN201410072974 A CN 201410072974A CN 103840113 B CN103840113 B CN 103840113B
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- 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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Abstract
The present invention relates to the preparation method of a kind of polyethylene separators for lithium battery, this preparation method comprises the following steps successively: A, by be 20 by percentage by weight～the polyethylene of 40% and 60～80% film forming solvent form raw material mixing；B, raw materials melt step A mixed are extruded, are cooled into sheet material；C, the sheet material vertical and horizontal of step B are stretched and makes film；D, film step C prepared, by extractant, extract film forming solvent and form microporous barrier；E, microporous barrier thermal finalization step D-shaped become form barrier film；Wherein, the mean molecule quantity 5.0 × 10 of described polyethylene4～1.5 × 106, molecular weight is more than 106Polyethylene account for the 10～15% of polyethylene gross weight.It is an object of the invention to provide the preparation method of a kind of polyethylene separators for lithium battery, it has higher porosity and bigger aperture, more meets the requirement that high power lithium battery barrier film uses.
Description
Technical field
The present invention relates to the preparation method of a kind of polyethylene separators for lithium battery.
Background technology
Along with energy crisis and problem of environmental pollution become increasingly conspicuous, hybrid electric vehicle market shows flourish gesture
Head.Lithium ion battery in hybrid electric vehicle must have the performance characteristics that discharge current is relatively big, power is higher.It addition, some
The electronic product such as electric tool, model plane also requires that battery can high-multiplying power discharge.Traditional small-sized, low-power lithium ion battery is
The demand in market can not be fully met.
Following two scheme is mainly had: the first scheme is currently for the aperture and porosity improving lithium battery isolation membrane
Add inorganic matter as pore-foaming agent, such as alundum (Al2O3), titanium dioxide, barium sulfate etc., but inorganic material and polyethylene is mixed
Conjunction is very poor, is easily caused dispersion uneven, causes pore-size distribution the widest, and porosity is uneven, has influence on product physical property, as
Stretching and puncture etc., and good conforming product cannot be obtained；Another kind of scheme is by improving stretching in process
Multiplying power carrys out hole diameter enlargement, but stretching ratio increases, and can cause stretching uneven, and processing septation stress is relatively big, has influence on heat
Stability.
Summary of the invention
For the problems referred to above, it is an object of the invention to provide the preparation side of a kind of polyethylene separators for lithium battery
Method, it has higher porosity and bigger aperture, more meets the requirement that high power lithium battery barrier film uses.
For solving above-mentioned technical problem, the present invention adopts the following technical scheme that
A kind of preparation method of the polyethylene separators for lithium battery, this preparation method comprises the following steps successively:
A, by be 20 by percentage by weight～the polyethylene of 40% and 60～80% film forming solvent form raw material mixing；
B, raw materials melt step A mixed are extruded, are cooled into sheet material；
C, the sheet material vertical and horizontal of step B are stretched and makes film；
D, film step C prepared, by extractant, extract film forming solvent and form microporous barrier；
E, microporous barrier thermal finalization step D-shaped become form barrier film；
Wherein, the mean molecule quantity 5.0 × 10 of described polyethylene4～1.5 × 106, molecular weight is more than 106Polyethylene account for
The 10～15% of polyethylene gross weight.
Preferably, described film forming solvent is paraffin oil, solid paraffin, soybean oil, peanut oil, olive oil, phthalic acid
The mixture of one or more in ester, dioctyl phthalate, dibutyl phthalate and glyceride, described film forming is molten
The agent kinematic viscosity when 40 DEG C is 20 ~ 100cst.
Preferably, in described step A, first by polyethylene and the film forming solvent premix accounting for film forming solvent gross weight 60～80%
It is combined into a material, then remaining film forming solvent is mixed with described a material.
Mix it is highly preferred that remaining film forming solvent is injected in extruder with described a material.
Preferably, in described step C, sheet material is carried out repeatedly cross directional stretch after longitudinal stretching, repeatedly the drawing of longitudinal stretching
Stretch multiplying power to increase successively.
It is highly preferred that longitudinal stretching multiplying power and cross directional stretch multiplying power are all higher than four times, and total stretching ratio is 25～45 times,
Draft temperature is 90～125 DEG C, and preferably between 100～120 DEG C, draft temperature is less than 90 DEG C, then film may be caused to break
Splitting or stretch uneven, draft temperature is higher than 120 DEG C, and stretching is readily accomplished very much, but owing to molecular chain orientation is inadequate, then microporous barrier
Mechanical performance can be affected, and is likely to cause stretching and uneven thickness simultaneously.If longitudinal stretching multiplying power, cross directional stretch multiplying power
Less than 4 times, total stretching ratio is less than 25 times, then the mechanical performance of film is relatively low and the lack of homogeneity of vertical and horizontal.If it is total
Stretching ratio is higher than 45 times, then at drawing process it may happen that rupture, and the shrinkage factor of final microporous barrier can improve.
Preferably, in described step E, barrier film is placed on airtight baking oven before rolling by the barrier film after thermal finalization
In, in baking oven, blowing hot-air carries out longitudinally being heat-treated to eliminate the thermal stress of barrier film to described barrier film.
Preferably, in described step B, extrusion temperature is higher than paraffin oil and resin can be formed thermodynamic single phase temperature and
Less than heat decomposition temperature, extrusion temperature is 150～270 DEG C, preferably between 170～250 DEG C, cooldown rate more than 15 DEG C/
S, preferably higher than 80 DEG C/s, the mode of cooling is typically with roller cooling, and its cooling medium can be water or air, molten
Producing during body cooling and be separated, the size of cooldown rate is very big to the structure influence of final apertures, and the melt fracture to microporous barrier
The height of temperature has a direct impact, if cooldown rate is the least, then the separated speed between polypropylene and polyethylene is more than tree
Fat and the separated speed of film forming solvent, the compatibility poor between polypropylene and polyethylene, influence whether the melted of microporous barrier
Break temperature and physical property thereof.
Preferably, in described step D, extractant be dichloromethane, pentane, hexane, heptane, carbon tetrachloride, diethyl ether,
The mixture of one or more in dioxanes, methyl ethyl ketone, extraction generally use immersion, in conjunction with ultrasonic wave, sprinkling or
The modes such as vibrations, in microporous barrier, the weight content of film forming solvent is less than 1%, if film forming solvent content is more than 1%, then influences whether micro-
The physical property of pore membrane and air permeability, and then have influence on many performances of lithium ion battery；
Preferably, in described step E, carry out thermal finalization by stenter, with eliminate barrier film internal stress, reduce finally every
From film percent thermal shrinkage, stablize barrier film internal structure, the temperature of thermal finalization is 115～135 DEG C, and heat setting temperature is the lowest, produce
Internal stress cannot can fully be discharged, then have influence on the percent thermal shrinkage of product, heat setting temperature is the highest, then be likely to result in isolation
Fenestra closes, and causes air permeability to decline.
The present invention uses above scheme, has the advantage that the polyethylene by introducing more low weight percentage and height contain
The low viscosity film forming solvent of amount, is first pre-mixed polyethylene and part film forming solvent, and residue film forming solvent passes through extruder
The mode that is directly injected into is to realize the mixing of raw material, and the porosity distribution scope of the final polyethylene separators prepared is 40～55%,
Mean porosities is at least 45%, and pore size distribution range is 60～200nm, and average pore size is at least 100nm, and puncture strength is extremely
Being 0.25N/um less, ventilative value is less than 18s/100cc/ μm.
Detailed description of the invention
Below presently preferred embodiments of the present invention is described in detail so that advantages and features of the invention can be easier to by
Those skilled in the art understands, thus protection scope of the present invention is made apparent clear and definite defining.
Embodiment one
A kind of preparation method of the polyethylene separators for lithium battery, this preparation method comprises the following steps successively:
A, first the paraffin oil of the polyethylene of 20 weight portions and 48 weight portions is combined into a by blender premix and expects, then a is expected
Adding in extruder, the paraffin oil of remaining 32 weight portions is directly injected into from extruder, the mean molecule quantity of described polyethylene
5.0×104～1.5 × 106, molecular weight is more than 106Polyethylene account for the 15% of polyethylene gross weight；
B, raw material step A mixed are extruded by the die melt of extruder at 170 DEG C, are naturally cooled into sheet
Material；
C, the sheet material of step B is first carried out after five longitudinal stretchings cross directional stretch, always drawing of longitudinal stretching again by roller
Stretching multiplying power is 6.468, and the stretching ratio of five longitudinal stretchings is followed successively by 1.1,1.2,1.4,1.75,2, the stretching of cross directional stretch times
Rate is 6.468, and draft temperature is 110 DEG C；
D, film immersion dichloromethane step C prepared combine ultrasonic extraction and goes out paraffin oil formation microporous barrier, micro-
In pore membrane, the weight content of paraffin oil is less than 1%；
E, microporous barrier step D-shaped become carry out thermal finalization at 115～135 DEG C by stenter and form barrier film, heat
Its roller arranged by M type in airtight baking oven, before rolling, is drawn, blowing hot-air in baking oven by the barrier film after sizing
Barrier film carries out longitudinally being heat-treated to eliminate the thermal stress of barrier film.
The porosity distribution scope of the polyethylene separators for lithium battery prepared by the present embodiment is 45～55%, averagely
Porosity is 50%, and pore size distribution range is 80～200nm, and average pore size is 140nm, and puncture strength is 0.25N/um, ventilative
Value is less than 18s/100cc/ μm.Above-mentioned each physical property measures the most by the following method:
Porosity: according to GB/T21650.1-2008 standard, calculate porosity according to gravimetric method；
Taking the barrier film sample of 100mm × 100mm normal size acquisition actual weight of weighing and be designated as W, barrier film volume is
V, barrier film resin density is ρ, then porosimeter formula is as follows:
Porosity %=(1-W/V* ρ) * 100%；
Aperture: use mercury injection apparatus to test the average pore size of barrier film, pore-size distribution；
Puncture strength: according to GB/T23318-2009 standard, is sphere (radius of curvature R: 0.5mm), a diameter of with front end
Maximum loading when being needled into polyethylene separators of 1mm；
Ventilative value: according to JIS P8117 standard, utilize Gurley permeability apparatus to carry out air permeability mensuration.Test value
Being designated as Gurly1, T is film thickness, then the Gurly air permeability values of unit thickness is calculated as Gurly1/T
Embodiment two
A kind of preparation method of the polyethylene separators for lithium battery, this preparation method comprises the following steps successively:
A, first the polyethylene of 30 weight portions and the paraffin oil of 49 weight portions are premixed in an extruder it is combined into a material, then will be surplus
The paraffin oil of 21 remaining weight portions injects from extruder in a material and mixes further, the mean molecule quantity of described polyethylene
5.0×104～1.5 × 106, molecular weight is more than 106Polyethylene account for the 12% of polyethylene gross weight；
B, raw material step A mixed are extruded by the die melt of extruder at 210 DEG C, are naturally cooled into sheet
Material；
C, the sheet material of step B is first carried out after five longitudinal stretchings cross directional stretch, always drawing of longitudinal stretching again by roller
Stretching multiplying power is 5.25, and the stretching ratio of five longitudinal stretchings is followed successively by 1.05,1.15,1.35,1.65,1.95, cross directional stretch
Stretching ratio is 5.25, and draft temperature is 110 DEG C；
D, film immersion dichloromethane step C prepared combine ultrasonic extraction and goes out paraffin oil formation microporous barrier, micro-
In pore membrane, the weight content of paraffin oil is less than 1%；
E, microporous barrier step D-shaped become carry out thermal finalization at 115～135 DEG C by stenter and form barrier film, heat
Its roller arranged by M type in airtight baking oven, before rolling, is drawn, blowing hot-air in baking oven by the barrier film after sizing
Barrier film carries out longitudinally being heat-treated to eliminate the thermal stress of barrier film.
The porosity distribution scope of the polyethylene separators for lithium battery prepared by the present embodiment is 40～55%, averagely
Porosity is 45%, and pore size distribution range is 80～170nm, and average pore size is 120nm, and puncture strength is 0.30N/um, ventilative
Value is less than 15s/100cc/ μm.The method of testing of above-mentioned each physical property is with embodiment one.
Embodiment three
A kind of preparation method of the polyethylene separators for lithium battery, this preparation method comprises the following steps successively:
A, first the polyethylene of 40 weight portions and the paraffin oil of 48 weight portions are premixed in an extruder it is combined into a material, then will be surplus
The paraffin oil of 12 remaining weight portions injects from extruder in a material and mixes further, the mean molecule quantity of described polyethylene
5.0×104～1.5 × 106, molecular weight is more than 106Polyethylene account for the 15% of polyethylene gross weight；；
B, raw material step A mixed are extruded by the die melt of extruder, with roller with 80 DEG C/s's at 250 DEG C
Cooldown rate is cooled into sheet material, and cooling medium is water；
C, the sheet material of step B is the most first carried out after five longitudinal stretchings cross directional stretch, always drawing of longitudinal stretching again
Stretching multiplying power is 5.25, and the stretching ratio of five longitudinal stretchings is followed successively by 1.05,1.15,1.35,1.65,1.95, cross directional stretch
Stretching ratio is 5.25, and draft temperature is 120 DEG C；
D, film immersion dichloromethane step C prepared combine ultrasonic extraction and goes out paraffin oil formation microporous barrier, micro-
In pore membrane, the weight content of paraffin oil is less than 1%；
E, microporous barrier step D-shaped become carry out thermal finalization at 115～135 DEG C by stenter and form barrier film, heat
Its roller arranged by M type in airtight baking oven, before rolling, is drawn, blowing hot-air in baking oven by the barrier film after sizing
Barrier film carries out longitudinally being heat-treated to eliminate the thermal stress of barrier film.
The porosity distribution scope of the polyethylene separators for lithium battery prepared by the present embodiment is 40～55%, averagely
Porosity is 41%, and pore size distribution range is 60～150nm, and average pore size is 105nm, and puncture strength is 0.32N/um, ventilative
Value is less than 18s/100cc/ μm.The method of testing of above-mentioned each physical property is with embodiment one.
Above-described embodiment for technology design and the feature of the present invention are described, is only a kind of preferred embodiment, and its purpose exists
Will appreciate that present disclosure in person skilled in the art and implement according to this, the protection of the present invention can not be limited with this
Scope.All equivalent transformations made according to the Spirit Essence of the present invention or modification, all should contain protection scope of the present invention it
In.
Claims (8)
1. the preparation method of polyethylene separators for lithium battery, it is characterised in that this preparation method include successively with
Lower step:
A, by be 20 by percentage by weight～the polyethylene of 40% and 60～80% film forming solvent form raw material mixing；
B, raw materials melt step A mixed are extruded, are cooled into sheet material；
C, the sheet material vertical and horizontal of step B are stretched and makes film；
D, film step C prepared, by extractant, extract film forming solvent and form microporous barrier；
E, microporous barrier thermal finalization step D-shaped become form barrier film；
Wherein, the mean molecule quantity 5.0 × 10 of described polyethylene4～1.5 × 106, molecular weight is more than 106Polyethylene account for poly-second
The 10～15% of alkene gross weight；
In described step A, first polyethylene and the film forming solvent premix accounting for film forming solvent gross weight 60～80% are combined into a material, then
Remaining film forming solvent is injected in extruder and mix with described a material.
Preparation method the most according to claim 1, it is characterised in that: described film forming solvent is paraffin oil, solid paraffin, big
In soya-bean oil, peanut oil, olive oil, phthalic acid ester, dioctyl phthalate, dibutyl phthalate and glyceride
The mixture of one or more, the described film forming solvent kinematic viscosity when 40 DEG C is 20 ~ 100cst.
Preparation method the most according to claim 1, it is characterised in that: in described step C, carry out sheet material repeatedly longitudinally drawing
Stretching rear cross directional stretch, repeatedly the stretching ratio of longitudinal stretching increases successively.
Preparation method the most according to claim 3, it is characterised in that: longitudinal stretching multiplying power and cross directional stretch multiplying power are all higher than
Four times, and always stretching ratio is 25～45 times, draft temperature is 90～125 DEG C.
Preparation method the most according to claim 1, it is characterised in that: in described step E, barrier film before rolling by described
Barrier film is placed in airtight baking oven, and in baking oven, described barrier film is carried out longitudinally being heat-treated to eliminate barrier film by blowing hot-air
Thermal stress.
Preparation method the most according to claim 1, it is characterised in that: in described step B, extrusion temperature is 150～270
DEG C, cooldown rate is more than 15 DEG C/s.
Preparation method the most according to claim 1, it is characterised in that: in described step D, extractant be dichloromethane,
The mixture of one or more in pentane, hexane, heptane, carbon tetrachloride, diethyl ether, dioxanes, methyl ethyl ketone, micropore
In film, the percentage by weight of film forming solvent is less than 1%.
Preparation method the most according to claim 1, it is characterised in that: in described step E, carry out heat by stenter fixed
Type, the temperature of thermal finalization is 115～135 DEG C.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104201321A (en) * | 2014-09-16 | 2014-12-10 | 中国科学院化学研究所 | Large-power lithium ion battery diaphragm |
| CN105552280B (en) * | 2016-03-07 | 2018-09-11 | 上海恩捷新材料科技股份有限公司 | A kind of preparation method of lithium ion battery separator |
| CN109285981A (en) * | 2017-07-20 | 2019-01-29 | 上海凯矜新材料科技有限公司 | Lithium battery diaphragm and preparation method thereof |
| CN109326760A (en) * | 2018-08-10 | 2019-02-12 | 泰州衡川新能源材料科技有限公司 | It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm |
| CN111477814A (en) * | 2019-01-30 | 2020-07-31 | 泰州衡川新能源材料科技有限公司 | Wet diaphragm and preparation process thereof |
| CN112290165A (en) * | 2020-11-05 | 2021-01-29 | 青岛蓝科途膜材料有限公司 | Lithium ion battery diaphragm, preparation method and lithium ion battery |
| CN113967365A (en) * | 2021-09-29 | 2022-01-25 | 内蒙古中锂新材料有限公司 | Extraction decontamination method and device for lithium battery diaphragm |
| CN114784462A (en) * | 2022-04-14 | 2022-07-22 | 中材锂膜(常德)有限公司 | Isolation film, isolation film preparation method and isolation film preparation device |
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| CN102774009A (en) * | 2012-08-07 | 2012-11-14 | 重庆纽米新材料科技有限责任公司 | Method for preparing polyolefin micro-porous film |
| CN103522550A (en) * | 2013-10-27 | 2014-01-22 | 中国乐凯集团有限公司 | Polyolefin microporous film preparation method for lithium ion battery and microporous film |
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| KR101174986B1 (en) * | 2007-10-12 | 2012-08-17 | 토레이 밧데리 세퍼레이터 필름 고도 가이샤 | Microporous membranes and methods for making and using such membranes |
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| CN102774009A (en) * | 2012-08-07 | 2012-11-14 | 重庆纽米新材料科技有限责任公司 | Method for preparing polyolefin micro-porous film |
| CN103522550A (en) * | 2013-10-27 | 2014-01-22 | 中国乐凯集团有限公司 | Polyolefin microporous film preparation method for lithium ion battery and microporous film |
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