CN108123086A - A kind of method and lithium ion battery separator for preparing lithium ion battery separator - Google Patents
A kind of method and lithium ion battery separator for preparing lithium ion battery separator Download PDFInfo
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- CN108123086A CN108123086A CN201711139443.9A CN201711139443A CN108123086A CN 108123086 A CN108123086 A CN 108123086A CN 201711139443 A CN201711139443 A CN 201711139443A CN 108123086 A CN108123086 A CN 108123086A
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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
- 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
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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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- General Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Cell Separators (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
High intensity low thickness lithium ion battery separator method is prepared the invention discloses a kind of, the quality parts ratio that this method includes the use of is 9:1 to 8:2 high molecular weight polypropylene raw material and ultra-high molecular weight polyethylene raw material is process through double screw extruder extrusion.The double screw extruder is divided into 9 areas, and takes and select reversely conveying screwing element into 6th area in 4th area and the screw thread combination of blended thread element is selected in 6th to 8 area so that the melt index of gained melt is between 1 1.5.The present invention also provides pass through high intensity low thickness lithium ion battery separator made from the above method.
Description
Technical field
The invention belongs to lithium ion battery separator fields, and in particular to it is a kind of prepare high intensity low thickness lithium ion battery every
The method of film and obtained lithium ion battery separator.
Background technology
One of the four big crucial main materials of membrane as lithium ion battery, play prevents positive and negative anodes contact short circuit in the battery
Insulating effect, at the same in charge and discharge process provide ion transmission channel effect.Its performance to the internal resistance of battery, capacity, follow
The characteristics such as ring performance and security performance all have a certain impact.With the continuous development of lithium ion battery product technology, lithium from
Sub- battery specific energy density is continuously improved, and lithium ion battery ion security performance progressively upgrades.
Existing polyalkene diaphragm production technology is divided into two major classes according to dry and wet.Dry method simple tension technique, most
Celanese companies of the U.S. are early seen in the patent US 3 of last century the late sixties application, 426,754, for producing individual layer
Polypropylene porous film.It is highly developed in the U.S., Japan, South Korea by the development of decades.Under Japanese Asahi Chemical Industry
Celgard companies, UBE companies of Japan use such technique productions individual layer PP and three layers of PP/PE/PP composite diaphragms.State at present
Inside and outside dry method list drawing process produces PP PP/PE/PP separator products, and thickness has evolved to for 40 μm of industrialization since most
21 μm of membrane of mainstream.
Wet method membrane can be made relatively thin, but process is complicated, generate a large amount of pollutions, be unfavorable for environmental protection.Meanwhile wet method
Membrane is using polyethylene as base material, and heat resisting temperature is low, and fusing-off temperature is low.Therefore, dry method membrane needs to carry out technology upgrading, needs
Accomplish more to be thinned, the membrane intensity in addition with lithium ion battery security being closely related is also required to greatly promote.But at present
The production of dry method membrane is drawn using single screw rod list, and raw material range of choice can only be the smaller polypropylene of molecular weight, so thin
The consequence of type is exactly that intensity drastically reduces, and although wet method membrane employs the polyethylene of super high molecular weight, and intensity can be than dry
The polypropylene diaphragm that method list is drawn is high, but processing technology is complicated, and pollution is big, does not meet environmental requirement.
Therefore, this field needs the method for new production high intensity low thickness polypropylene lithium ion battery separator.
The content of the invention
It is greatly reduced to solve the problems, such as to exist in the prior art intensity after the slimming of dry method membrane, the present invention provides
It is a kind of to produce the method for high intensity low thickness polypropylene lithium ion battery separator, and therefore provide a kind of high intensity low thickness lithium from
Sub- battery diaphragm.
In one aspect, the present invention provides a kind of method for producing high intensity low thickness polypropylene lithium ion battery separator,
This method comprises the following steps：
Batch mixing：Pp material and polyethylene raw material in high speed mixing smelting machine are kneaded and uniformly obtain mixed raw material,
It squeezes out：Gained mixed raw material and additive are kneaded melting extrusion into melt by double screw extruder,
Slab：By gained melt on sharp cooling roll by high speed traction form a film slab,
Annealing：Gained slab is toasted at a certain temperature to obtain semi-finished product film,
Cold drawing：Gained semi-finished product film is stretched under normal temperature condition to obtain cold drawing film,
Hot-drawn：Gained cold drawing film is subjected to hot-stretch under the conditions of certain temperature and obtains hot-stretch film,
Thermal finalization：For a period of time, winding obtains state after gained hot-stretch film is kept above-mentioned hot-drawn at a certain temperature
High intensity low thickness lithium ion battery separator finished product,
Wherein, the polypropylene be high molecular weight polypropylene, the polyethylene be ultra-high molecular weight polyethylene, the high-molecular-weight poly
Propylene feedstocks and the quality parts ratio of the ultra-high molecular weight polyethylene raw material are 9:1 to 8:2, which is divided into 9
Area, and take and select reversely conveying screwing element into 6th area in 4th area and the screw thread of blended thread element is selected in 6th to 8 area
Combination so that the melt index of gained melt is between 1-1.5.
Specifically, the melt index scope of the high molecular weight polypropylene is between 0.2-1, and molecular weight distribution is in 1.5-2.5
Between, weight average molecular weight is 4 × 105-6×105Between.
Specifically, the melt index scope of the ultra-high molecular weight polyethylene is between 0.05-0.02, and molecular weight distribution is in 1-
Between 2.5, weight average molecular weight is 6.5 × 105-7.5×105Between.
Specifically, the temperature range in 9 areas is respectively：1st area, room temperature, 2nd area and 3rd area, 150-200 DEG C, 4th area to 7th area,
200-260 DEG C, 8th to 9 area, 180-240 DEG C.
More specifically, the temperature range in 9 areas is respectively：1st area, room temperature, 2nd area and 3rd area, 175-185 DEG C, 4th area to 7
Area, 220-240 DEG C, 8th to 9 area, 200-220 DEG C.
Specifically, the mixing speed of the high speed mixing smelting machine is 750-850 revs/min, and the temperature of annealing is 20 DEG C -100 DEG C, is moved back
The time of fire is 10min-40min, and cold drawing temperature is 10 DEG C -30 DEG C, stretching ratio 100%-150%, and the hot-drawn temperature is
80 DEG C -140 DEG C, stretching ratio 150%-250%, heat setting temperature is 120 DEG C -170 DEG C, and heat-setting time is 2-5 minutes.
More specifically, the mixing speed of the high speed mixing smelting machine is 800 revs/min, the temperature of annealing is 30 DEG C -80 DEG C, annealing
Time for 20min-30min, cold drawing temperature is 15 DEG C -20 DEG C, stretching ratio 110%-140%, and the hot-drawn temperature is 100
DEG C -120 DEG C, stretching ratio 180%-240%, heat setting temperature is 140 DEG C -160 DEG C, and heat-setting time is 3-4 minutes.
Additive in extrusion step operates common additive for the extrusion of this field, such as levelling agent, plasticiser, refreshing
Lubrication prescription etc..
On the other hand, the present invention provide a kind of high intensity low thickness polypropylene lithium prepared according to the methods of the invention from
Sub- battery diaphragm.The membrane thicknesses are between 5-10 μm, and puncture strength is between 380-440g.Preferably, the film thickness is smaller
Thickness and with higher puncture strength.It is highly preferred that the film reaches the pierce depth of 440g with 5 μm of thickness.
The advantageous effects of the present invention
The present invention is 9 by using quality parts ratio:1 to 8:2 high molecular weight polypropylene raw material and super high molecular weight gathers
The mixture of ethylene raw, in particular by 8:2 high molecular weight polypropylene:Ultra-high molecular weight polyethylene ratio, that is, using can
The ultra-high molecular weight polyethylene of quantity is seen, so as to provide the material base for preparing high intensity low thickness polypropylene lithium ion battery separator
Plinth.Meanwhile by using being divided into the double screw extruder in 9 areas, and take and select reversely conveying screw thread into 6th area in 4th area
Element and the screw thread combination that blended thread element is selected in 6th to 8 area, so as to provide extruding macromolecular amount pp material and super
The Process ba- sis of the mixture of High molecular weight polyethylene raw material so that the melt index of gained melt is between 1-1.5, Ke Yishi
Existing obtained lithium ion battery separator has the higher-strength between relatively low thickness and 380-440g between 5-10 μm.
Specific embodiment
Clear, complete explanation is further made to the present invention with reference to specific embodiment.
The scientific terminology used herein has meaning well known in the art, unless otherwise defined.
Particularly, for forming the high molecular weight polypropylene of the method for the present invention (ultra-high molecular weight
Polypropylene) raw material has meaning well known in the art.In general, the melt index scope of the high molecular weight polypropylene exists
Between 0.2-1, molecular weight distribution is between 1.5-2.5, and weight average molecular weight is 4 × 105-6×105Between.
Particularly, for forming the ultra-high molecular weight polyethylene of the method for the present invention (ultra-high molecular
Weight polyethylene) raw material have meaning well known in the art.In general, the melt index of ultra-high molecular weight polyethylene
Scope is between 0.05-0.02, and molecular weight distribution is between 1-2.5, and weight average molecular weight is 6.5 × 105-7.5×105Between.
High molecular weight polypropylene and ultra-high molecular weight polyethylene are because of molecular weight height, it is more difficult to are machined.Common list
Screw extruder melting extrusion high molecular weight polypropylene is not easy uniformly with being kneaded during ultra-high molecular weight polyethylene, and melting extrusion is melted
The entanglement of body strand is very uneven or even gets to know in extrusion and melt fracture state occurs.Using the general of standard thread element
It is poor there is also plasticizing effect when logical double screw extruder melting extrusion high molecular weight polypropylene is with ultra-high molecular weight polyethylene, it melts
The problem of body is not easy to be molded.
The inventors discovered that it is selected by using the double screw extruder including 9 areas and taking in 4th area into 6th area instead
The screw thread combination of blended thread element is selected in 6th to 8 area to conveying screwing element so that the melt index of gained melt exists
Between 1-1.5, above-mentioned processing problems can be solved.
The screw thread used in the double screw extruder has following three kinds：
1. standard thread element：, when double screw extruder works, the effect of primarily serving is transport raw material and melt for it.Spiral shell
Line screw pitch is bigger, and conveying speed is faster, but simultaneously the time of Melt residence shorten, the time of melting mixing shortens.
2. reversely conveying screwing element：It plays the role of being when extending Melt residence when double screw extruder works
Between, while melt is kneaded, increase the melting effect between different material.Thread pitch is bigger, and the residence time is shorter again for melt,
Conveying speed is lower.
3. blended thread element：It plays the role of being to be kneaded difference by Strong shear when double screw extruder works
Raw material increases the admixture between different material.Thread pitch is smaller, and melting effect is better.
The length of one screw thread is 1D, and wherein D is screw diameter.In the present invention, all thread pitch are the same.It should
The draw ratio of double-screw extruder screw extruding zone is 35-41, and the length ratio in 9 areas is 6D:1D:4D:4D:6D:6D:4D:
6D:4D.Screwing element can arbitrarily replace combination between 9 areas, but in order to achieve the object of the present invention, it is desirable that it takes
4th area select reversely conveying screwing element into 6th area and the screw thread combination of blended thread element are selected in 6th to 8 area.
The temperature range in 9 areas is respectively：1st area, room temperature, 2nd area and 3rd area, 150-200 DEG C, 4th area to 7th area, 200-260
DEG C, 8th to 9 area, 180-240 DEG C.More specifically, the temperature range in 9 areas is respectively：1st area, room temperature, 2nd area and 3rd area, 175-
185 DEG C, 4th area to 7th area, 220-240 DEG C, 8th to 9 area, 200-220 DEG C.
It is combined by the above-mentioned screw thread of the present invention, and combines the temperature range in each area, be 9 for quality parts ratio:1 to 8:
2 high molecular weight polypropylene raw material and ultra-high molecular weight polyethylene raw material can make the melt index of melt of gained in 1-1.5
Between.If melt index is less than 1, melt cannot go up sharp cooling roll and can not form a film without viscosity；And if melt index is big
In 1.5, the membrane intensity finally produced of melt is less than requirement.
Embodiment
Below by way of non-limiting example, the present invention is further explained.
In these embodiments, in membrane thicknesses (5 μm and 10 μm), raw material (high molecular weight polypropylene raw material and superelevation point
Sub- weight northylen raw material and its ratio), extruder (single screw extrusion machine and double screw extruder), each area of double screw extruder
It is compared in terms of element, the index specifically compared is the melt index of melt and the puncture strength of obtained membrane.It is molten
Melt index and puncture strength to measure by method well known in the art.
Each embodiment extruding macromolecular amount pp material and super high molecular weight in the double screw extruder with 9 areas
Polyethylene raw material prepares membrane sample.Operating procedure is as follows：
Batch mixing：By high density poly propylene raw material and ultra high density polyethylene raw material with 800 revs/min in high speed mixing smelting machine
Mixing speed is kneaded uniformly, obtains mixed raw material；
It squeezes out：9 that gained mixed raw material and levelling agent, plasticiser, smooth agent addition agent are passed through into double screw extruder
Area is kneaded melting extrusion into melt,
Slab：By gained melt on sharp cooling roll by high speed traction form a film slab,
Annealing：Gained slab at 100 DEG C is toasted and obtains semi-finished product film,
Cold drawing：Gained semi-finished product film is stretched at 20 DEG C, stretching ratio 200% obtains cold drawing film,
Hot-drawn：Gained cold drawing film is subjected to hot-stretch at 100 DEG C, stretching ratio 200% obtains hot-stretch film,
Thermal finalization：Gained hot-stretch film is kept at 150 DEG C to state 3 minutes after above-mentioned hot-drawn, winding obtains membrane sample.
Wherein, 9 area's temperature ranges of extrusion step are respectively：1st area, room temperature, 2nd area and 3rd area, 180 DEG C, 4th area to 7th area,
230 DEG C, 8th to 9 area, 210 DEG C.
The testing program of each embodiment and the result is shown in the following table 1.
The testing program and result of 1 each embodiment of table
It discusses：
Embodiment 1-6 shows the situation of the membrane of 10 μ m thicks.
In embodiment 1, raw material not using ultra-high molecular weight polyethylene, and is squeezed out only with high molecular weight polypropylene
Machine is only with single screw extrusion machine, and not using double screw extruder, the melt index (MFR) of gained is 0.9, film forming
Difference, i.e. plasticizing effect are poor, it is impossible to be molded, therefore fail to measure puncture strength.
In example 2, raw material not using ultra-high molecular weight polyethylene, and is squeezed out only with high molecular weight polypropylene
Machine does not use single screw extrusion machine, but using double screw extruder, wherein whole region uses standard thread element, gained
MFR is 2.5, and film forming is preferable, and puncture strength reaches 320g.Embodiment 2 is compared with Example 1 as it can be seen that double screw extruder squeezes out
High molecular weight polypropylene could obtain preferable MFR and film forming.
In embodiment 3, for raw material simultaneously using high molecular weight polypropylene and ultra-high molecular weight polyethylene, the two ratio is 9
Than 1, extruder situation used is same as Example 2, and the melt MFR of gained is 0.8, and film forming is poor, i.e., plasticizing effect is poor, it is impossible to
Shaping, therefore fail to measure puncture strength.
In example 4, same as Example 3 using raw material condition, extruder used is also double screw extruder, but 4
Area and 6th area are using reversely conveying screwing element, and 7th area use blended thread element, and the melt MFR of gained is 1, and film forming is general,
Puncture strength is 380g.
In embodiment 5 and embodiment 6, the ratio of high molecular weight polypropylene and ultra-high molecular weight polyethylene is changed to by 9 to 1
8 to 2, that is, increase the amount of ultra-high molecular weight polyethylene, and blended thread element is used in embodiment 6 in 6th area and 8th area, MFR points
Not up to 1.2 and 1.4, film forming is respectively good extremely excellent, and puncture strength is respectively 400g and 420g.
By embodiment 1-6 as it can be seen that in the case where preparing the membrane of 10 μ m thicks, double screw extruder is squeezed better than single screw rod
Go out machine, while higher puncture strength can be obtained using high molecular weight polypropylene and ultra-high molecular weight polyethylene, wherein using
The ultra-high molecular weight polyethylene of higher proportion, and blended thread element is used in 6th area, 7th area and 8th area in double screw extruder
When, MFR, film forming and puncture strength are all more excellent.
Embodiment 7-11 shows the situation of the membrane of 5 μ m thicks.
Such as 7 finding of embodiment, even if using double screw extruder, and reversely conveying screw thread member is used in 4th area and 6th area
Part, MFR value also only have 0.9, and film forming is poor, i.e., plasticizing effect is poor, it is impossible to be molded, therefore fail to measure puncture strength.
If as described in Example 8 in 4 and 6 areas using reversely conveying screwing element, 7th area using blended thread element or
Person is divided as described in Example 9 in 4th area using reversely conveying screwing element in 6th area and 8th area using blended thread element, MFR
Not Wei 1 and 1.3, film forming is respectively general and good, and puncture strength is respectively 380g and 410g.As it can be seen that in 6th area and 8th area
Preferable MFR, film forming and puncture strength are obtained using blended thread element.
In embodiment 10 (comparative examples 4), raw material is simultaneously using high molecular weight polypropylene and superhigh molecular weight polyethylene
Alkene, the two ratio are 9 to 1, and 6th area and 8th area even in double screw extruder also use blended thread element, MFR 0.9,
Film forming is poor, i.e., plasticizing effect is poor, it is impossible to be molded, therefore fail to measure puncture strength.
In embodiment 11, for raw material simultaneously using high molecular weight polypropylene and ultra-high molecular weight polyethylene, the two ratio is 8
Than 2, and 6th area of double screw extruder and 8th area, also using blended thread element, MFR is up to 1.4, and film forming is excellent, and puncture strength reaches
440g。
By embodiment 1-11 as it can be seen that prepare thinner thickness and the higher lithium ion battery separator of intensity, raw material preferably make
With high molecular weight polypropylene and the mixture of ultra-high molecular weight polyethylene, the more preferably ratio of the two is 8 to 2, i.e., 4 to 1；
Extruder will use double screw extruder, and preferably in 4th area to 6th area using screwing element is reversely conveyed, more preferably
It is to use blended thread element in 6th area to 8th area.
The description of this invention above for illustration purposes only, is not meant to the model limiting the invention in any way
It encloses.Under the introduction of the spirit of the present invention, those skilled in the art can make under the premise without departing from the essence of the invention
Many modifications and equivalent program.These modifications and equivalent program as long as not conflicting with the prior art, each fall within right
In the scope of the present invention that claim is covered.
Claims (6)
1. a kind of prepare high intensity low thickness lithium ion battery separator method, the described method comprises the following steps：
Batch mixing：Pp material and polyethylene raw material in high speed mixing smelting machine are kneaded and uniformly obtain mixed raw material,
It squeezes out：Gained mixed raw material and additive are kneaded melting extrusion into melt by double screw extruder,
Slab：By gained melt on sharp cooling roll by high speed traction form a film slab,
Annealing：Gained slab is toasted at a certain temperature to obtain semi-finished product film,
Cold drawing：Gained semi-finished product film is stretched under normal temperature condition to obtain cold drawing film,
Hot-drawn：Gained cold drawing film is subjected to hot-stretch under the conditions of certain temperature and obtains hot-stretch film,
Thermal finalization：For a period of time, winding obtains high-strength state after gained hot-stretch film is kept above-mentioned hot-drawn at a certain temperature
Low thickness lithium ion battery separator finished product is spent,
It is characterized in that, the polypropylene be high molecular weight polypropylene, the polyethylene be ultra-high molecular weight polyethylene, the height
The quality parts ratio of molecular weight polypropylene raw material and the ultra-high molecular weight polyethylene raw material is 9:1 to 8:2, the twin-screw squeezes
Go out machine and be divided into 9 areas, and take and select reversely conveying screwing element into 6th area in 4th area and mixing spiral shell is selected in 6th to 8 area
The screw thread combination of texel part so that the melt index of gained melt is between 1-1.5.
2. according to the method described in claim 1, it is characterized in that, the melt index scope of the high molecular weight polypropylene exists
Between 0.2-1, molecular weight distribution is between 1.5-2.5, and weight average molecular weight is 4 × 105-6×105Between；The super high molecular weight
The melt index scope of polyethylene between 0.05-0.02, molecular weight distribution between 1-2.5, weight average molecular weight 6.5 ×
105-7.5×105Between.
3. according to the method described in claim 1, it is characterized in that, the temperature range in 9 areas is respectively：1st area, room temperature, 2
Area and 3rd area, 150-200 DEG C, 4th area to 7th area, 200-260 DEG C, 8th to 9 area, 180-240 DEG C.
4. method according to any one of claim 1-3, which is characterized in that the mixing speed of the high speed mixing smelting machine is
750-850 revs/min, the temperature of the annealing is 20 DEG C -100 DEG C, and time of annealing is 10min-40min, the cold drawing temperature
For 10 DEG C -30 DEG C, stretching ratio 100%-150%, the hot-drawn temperature is 80 DEG C -140 DEG C, stretching ratio 150%-
250%, the heat setting temperature is 120 DEG C -170 DEG C, and heat-setting time is 2-5 minutes.
5. a kind of high intensity low thickness lithium ion battery separator, which is characterized in that the membrane passes through according in claim 1-4
It is prepared by any one of them method.
6. high intensity low thickness lithium ion battery separator according to claim 5, which is characterized in that the membrane thicknesses exist
Between 5-10 μm, puncture strength is between 380-440g.
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| CN101914242A (en) * | 2010-08-17 | 2010-12-15 | 东华大学 | Ultrahigh molecular weight polypropylene/ultrahigh molecular weight polythene/epoxy resin composite membrane |
| CN102769115A (en) * | 2012-08-02 | 2012-11-07 | 常州大学 | Lithium ion battery membrane prepared by polypropylene mixture and preparing method thereof |
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