CN109326760A - It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm - Google Patents
It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm Download PDFInfo
- Publication number
- CN109326760A CN109326760A CN201810909970.1A CN201810909970A CN109326760A CN 109326760 A CN109326760 A CN 109326760A CN 201810909970 A CN201810909970 A CN 201810909970A CN 109326760 A CN109326760 A CN 109326760A
- Authority
- CN
- China
- Prior art keywords
- antioxidant
- manufacturing
- paraffin oil
- polyethylene powder
- oil film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 13
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 34
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 34
- 239000004698 Polyethylene Substances 0.000 claims abstract description 23
- -1 polyethylene Polymers 0.000 claims abstract description 22
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920000573 polyethylene Polymers 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000005662 Paraffin oil Substances 0.000 claims abstract description 18
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 238000007493 shaping process Methods 0.000 claims abstract description 4
- 235000006708 antioxidants Nutrition 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000007499 fusion processing Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 claims description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 2
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 2
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 2
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 claims description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000012528 membrane Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000009740 moulding (composite fabrication) Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Cell Separators (AREA)
- Secondary Cells (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Abstract
The invention discloses a kind of for manufacturing the manufacturing method of lithium battery diaphragm, in specific proportions mixes the polyethylene powder fusing added with antioxidant and with paraffin oil, and squeezed out, be quickly cooled to as oil film with double screw extruder；Oil film passes through 5~10 grades of longitudinal stretchings, oil film after the stretching primary cross directional stretch within the scope of specific temperature, stretch rate be 2~10 times, by methylene chloride extraction by the inside paraffin oil extraction fall, extract metacneme within the scope of specific temperature after secondary horizontal drawing film forming, cooling and shaping.Carry out appropriate adjustment in the proportion of PE and paraffin oil, control temperature carries out longitudinal stretching and cross directional stretch in particular range, and it is more uniform thus to produce macroporosity membrane pore size, without through-hole, is suitble to the power battery use of big battery electric discharge.
Description
Technical field
The present invention relates to technical field of lithium batteries more particularly to a kind of for manufacturing the manufacturing method of lithium battery diaphragm.
Background technique
In the structure of lithium battery, diaphragm is crucial one of interior layer assembly.The performance of diaphragm determines the interface knot of battery
Structure, internal resistance etc. directly affect the characteristics such as capacity, circulation and the security performance of battery, and the diaphragm haveing excellent performance is to raising battery
Comprehensive performance play an important role.
Current driving force battery pursues heavy-current discharge, and this requires the porositys of the diaphragm of lithium battery to do more,
Common diaphragm porosity generally between 38 ± 5%, is insufficient for heavy-current discharge demand.Diaphragm is as positive and negative anodes simultaneously
Dielectric, it is necessary to have electronic isolation, and the diaphragm for improving porosity merely will appear through-hole, thus in battery production
Defect is caused in the process, is led to have conductive impurity folder to form electronic conduction point in through-holes, is influenced battery performance.
Summary of the invention
To overcome disadvantages mentioned above, the purpose of the present invention is to provide a kind of for manufacturing the manufacturing method of lithium battery diaphragm,
To improve diaphragm porosity, while the aperture for making diaphragm microcosmic is as uniform as possible, avoids the occurrence of the defect of through-hole class.
In order to reach the goals above, the technical solution adopted by the present invention is that: it is a kind of for manufacturing the manufacture of lithium battery diaphragm
Method, steps are as follows:
Step 1 squeezes into the polyethylene powder added with antioxidant in extruder, melts at a temperature of 200~300 DEG C,
And paraffin oil is squeezed into fusion process, the mixed proportion of polyethylene powder and paraffin oil is 1:1~1:5.5, between the two most
Excellent scheme are as follows: the proportion of polyethylene powder and paraffin oil is 25:75 or 26:74；
Liquid after the completion of step 2, polyethylene powder and paraffin oil mixing is squeezed out with double screw extruder, is squeezed out weight and is
200~1000 kilograms per hour, and the liquid after extrusion is rapidly cooled to 10~100 DEG C of temperature, forms oil film；
Step 3, oil film after cooling carry out 5~10 grades of longitudinal stretchings, every grade of draw ratio on 90~130 DEG C of draw roll
Example is 1.1~2.0 times, 5~10 grades of total 2~10 times of stretchings；
Oil film after the completion of step 4, longitudinal stretching carries out a cross directional stretch in 100~140 DEG C of drawing oven, draws
Stretching ratio is 2~10 times；
Step 5, primary oil film after stretching horizontally extract to fall the extraction of the inside paraffin oil via methylene chloride, in extraction tank
Temperature is at 18~30 DEG C；
Residual dichloromethane on oil film is dried again after step 6, extraction, then at diaphragm, secondary horizontal drawing after secondary horizontal drawing
Box temperature degree is 100~140 DEG C；
Step 7, by after secondary horizontal drawing diaphragm carry out cooling and shaping, 15~50 DEG C of cooling temperature.
Furthermore, it is understood that containing polyethylene particle, antioxidant a and antioxidant b, the antioxidant a in polyethylene powder, resisting
The quality of oxygen agent b accounts for the 0.1%~1% of total polyethylene powder quality respectively.Above-mentioned antioxidant a and antioxidant b is using as follows
The antioxidant trade mark in list.
Compared with prior art, the present invention carries out appropriate adjustment in the proportion in polyethylene powder and paraffin oil, control
Temperature carries out longitudinal stretching and cross directional stretch in particular range, and it is more uniform thus to produce macroporosity membrane pore size, does not have
There is defective hole, the power battery of suitable heavy-current discharge uses.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
Embodiment
One of the present embodiment is used to manufacture the manufacturing method of lithium battery diaphragm, manufactures under dustfree environment,
Steps are as follows:
Polyethylene particle, antioxidant a and antioxidant b are mixed into polyethylene powder by step 1, wherein antioxidant a and antioxygen
The quality of agent b accounts for the 0.1%~1% of total polyethylene powder quality respectively；Antioxidant a and antioxidant b is used as in following table
The antioxidant trade mark；
| Antioxidant 1010 | Antioxidant 1076 | Irgasfos 168 |
| Antioxidant 264 | Antioxidant 1098 | Antioxidant 2246 |
| Antioxidant 300,311 | Antioxidant B102 | Anti-oxidant DLTP, DSTP |
| Antioxidant B215, B225 | Antioxidant B900 |
Step 2 squeezes into polyethylene powder in extruder, melts at a temperature of 200~300 DEG C, and in fusion process
Squeeze into paraffin oil, the mixed proportion of polyethylene powder and paraffin oil is 1:1~1:5.5, between the two optimal scheme are as follows: poly- second
The proportion of alkene powder and paraffin oil is 25:75 or 26:74；
Step 3 squeezes out the liquid after the completion of mixing with double screw extruder, and squeezing out weight is 200~1000 kilograms every
Hour, and the liquid after extrusion is rapidly cooled to 10~100 DEG C of temperature, form oil film；
Step 4, oil film after cooling carry out 5~10 grades of longitudinal stretchings, every grade of draw ratio on 90~130 DEG C of draw roll
Example is 1.1~2.0 times, 5~10 grades of total 2~10 times of stretchings；Oil film after the completion of longitudinal stretching is dried in 100~140 DEG C of stretching
A cross directional stretch is carried out in case, stretch rate is 2~10 times；
Step 5, primary oil film after stretching horizontally extract to fall the extraction of the inside paraffin oil via methylene chloride, in extraction tank
Temperature is at 18~30 DEG C；
Residual dichloromethane on oil film is dried again after step 6, extraction, then at diaphragm, secondary horizontal drawing after secondary horizontal drawing
Box temperature degree is 100~140 DEG C；
Step 7, by after secondary horizontal drawing diaphragm carry out cooling and shaping, 15~50 DEG C of cooling temperature.
Lithium battery diaphragm carries out porosity test after completing, the environmental requirement of test is 25 ± 5 DEG C of temperature, humidity 30
~70%, there are two ways to test.
The first is tested using pressure water instrument, tests pressure setting range: 0-1400PS I, gradient pressurization.
This is sampled as 0.1m*0.1m square sample, area 10cm*10cm=100cm2, 20 μm of thickness, then V=
100*0.0002=0.02cm3, raw materials for production PE powder bulk density are as follows: 0.931g/cm3。
The calculation of use: P=[(M-m)/M) * 100% wherein, M=P0'*V, m are the quality of unit volume diaphragm,
kg/cm3；P0' is the bulk density of material, units/kg/cm3；V is volume, unit cm3。
Weigh sample diaphragm quality three times: m1=0.00981g, m2=0.00986g, m3=0.00979g take arithmetic flat
Mean value m=0.00982g；Calculate porosity P=(0.01862-0.00982)/0.01862*100%=47.26%.
The print that diaphragm is cut into for second 10*10cm, weighs accurate weight with assay balance (precision 0.0001g)
Amount is denoted as g, measures print thickness using calibrator (precision 0.00001mm), uniformly takes a little 9,9 points of measurement are made even
Mean value is denoted as print thickness and is denoted as h, and the density of diaphragm raw materials is denoted as ρ, then porosity is denoted as X, X value be can be used to down
Formula carries out approximate calculation:
The numerical value of X=[1-g/ (ρ * h)] * 100%X is recorded with %.
It is provided in the present embodiment that pressure water instrument is tested as a result, the lithium battery diaphragm hole manufactured using the present embodiment
Rate is big, membrane pore size is more uniform, without through-hole, it is made to meet the heavy-current discharge demand of power battery.
The technical concepts and features of embodiment of above only to illustrate the invention, its object is to allow be familiar with technique
People understands the contents of the present invention and is implemented, and it is not intended to limit the scope of the present invention, all spiritual according to the present invention
The equivalent change or modification that essence is done, should be covered by the scope of protection of the present invention.
Claims (4)
1. a kind of for manufacturing the manufacturing method of lithium battery diaphragm, it is characterised in that steps are as follows:
Step 1 squeezes into the polyethylene powder added with antioxidant in extruder, melts at a temperature of 200~300 DEG C, and
Squeeze into paraffin oil in fusion process, the mixed proportion of polyethylene powder and paraffin oil is 1:1~1:5.5；
Liquid after the completion of step 2, polyethylene powder and paraffin oil mixing is squeezed out with double screw extruder, and by the liquid after extrusion
Body is rapidly cooled to 10~100 DEG C of temperature, forms oil film；
Step 3, oil film after cooling carry out 5~10 grades of longitudinal stretchings on 90~130 DEG C of draw roll, and every grade of stretch ratio is
1.1~2.0 times, 5~10 grades of total 2~10 times of stretchings；
Oil film after the completion of step 4, longitudinal stretching carries out a cross directional stretch, draw ratio in 100~140 DEG C of drawing oven
Rate is 2~10 times；
Step 5, primary oil film after stretching horizontally extract to fall the extraction of the inside paraffin oil via methylene chloride, temperature in extraction tank
At 18~30 DEG C；
Residual dichloromethane on oil film is dried again after step 6, extraction, then at diaphragm, secondary horizontal drawing box temperature after secondary horizontal drawing
Degree is 100~140 DEG C；
Step 7, by after secondary horizontal drawing diaphragm carry out cooling and shaping, 15~50 DEG C of cooling temperature.
2. the manufacturing method according to claim 1, it is characterised in that: contain polyethylene particle, antioxygen in polyethylene powder
The quality of agent a and antioxidant b, the antioxidant a, antioxidant b account for the 0.1%~1% of total polyethylene powder quality respectively.
3. the manufacturing method according to claim 1, it is characterised in that: antioxidant can be used in the antioxidant a, antioxidant b
1010, antioxidant 1076, irgasfos 168, antioxidant 264, antioxidant 1098, antioxidant 2246, antioxidant 300, antioxidant
311, antioxidant B102, anti-oxidant DLTP, antioxidant DSTP, antioxidant B215, antioxidant B225, any in antioxidant B900
Two kinds.
4. the manufacturing method according to claim 1, it is characterised in that: the proportion of the polyethylene powder and paraffin oil is
25:75 or 26:74.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810909970.1A CN109326760A (en) | 2018-08-10 | 2018-08-10 | It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810909970.1A CN109326760A (en) | 2018-08-10 | 2018-08-10 | It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109326760A true CN109326760A (en) | 2019-02-12 |
Family
ID=65263443
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810909970.1A Pending CN109326760A (en) | 2018-08-10 | 2018-08-10 | It is a kind of for manufacturing the manufacturing method of lithium battery diaphragm |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109326760A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110286075A (en) * | 2019-06-12 | 2019-09-27 | 河北金力新能源科技股份有限公司 | A kind of test method of lithium ion battery separator closed pore temperature |
| CN112259904A (en) * | 2020-09-28 | 2021-01-22 | 河北金力新能源科技股份有限公司 | High-strength low-shrinkage lithium ion battery diaphragm and preparation method thereof |
| CN114274484A (en) * | 2021-11-11 | 2022-04-05 | 乐凯胶片股份有限公司 | Polyethylene microporous membrane, preparation method thereof and lithium ion battery |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110286075A (en) * | 2019-06-12 | 2019-09-27 | 河北金力新能源科技股份有限公司 | A kind of test method of lithium ion battery separator closed pore temperature |
| CN112259904A (en) * | 2020-09-28 | 2021-01-22 | 河北金力新能源科技股份有限公司 | High-strength low-shrinkage lithium ion battery diaphragm and preparation method thereof |
| CN114274484A (en) * | 2021-11-11 | 2022-04-05 | 乐凯胶片股份有限公司 | Polyethylene microporous membrane, preparation method thereof and lithium ion battery |
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Application publication date: 20190212 |
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