CN108183190A - The pore former minimizing technology of battery diaphragm and the preparation process of lithium ion secondary battery membrane - Google Patents
The pore former minimizing technology of battery diaphragm and the preparation process of lithium ion secondary battery membrane Download PDFInfo
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- CN108183190A CN108183190A CN201711430523.XA CN201711430523A CN108183190A CN 108183190 A CN108183190 A CN 108183190A CN 201711430523 A CN201711430523 A CN 201711430523A CN 108183190 A CN108183190 A CN 108183190A
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- pore former
- diaphragm
- extraction
- minimizing technology
- diaphragm substrate
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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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- 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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- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cell Separators (AREA)
- Secondary Cells (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of pore former minimizing technology of battery diaphragm and the preparation process of lithium ion secondary battery membrane, the step of pore former minimizing technology of battery diaphragm, includes：Diaphragm substrate is pre-processed by equipment, removes at least part pore former in diaphragm substrate in advance；Extraction processing is carried out to pretreated diaphragm substrate by ultrasonic extraction, pore former is extracted, and ensures that the pore former remnants rates of battery diaphragm being finally made are less than 1%.The present invention improves the rate of extraction of battery diaphragm, and especially suitable for the extraction compared with thick skirt substrate, solve the problems, such as that thicker substrate extraction is difficult in the case where not needing to increase battery producing line length, not needing to improve equipment precision and personnel's technical ability.
Description
Technical field
The present invention relates to a kind of pore former minimizing technology of battery diaphragm and the preparation processes of lithium ion secondary battery membrane.
Background technology
At present, lithium rechargeable battery is because its energy density is high, has extended cycle life, in consumer electronics, electric vehicle and storage
Energy field has been more and more widely used.As more and more diaphragm production lines are gone into operation, the competition between diaphragm enterprise is more next
It is fiercer.At present, most enterprises are to increase producing line quantity, to improve yield.There is no any technical innovation, and invest
Greatly, the period is long.Once not up to scheduled target, it will cause great loss.
In BOPP industries, the film produced is nonporous film, without will add in pore former in film and extract, therefore
The speed of production line can reach 500m/min, and breadth reaches 10m.
The production technology of diaphragm extracts afterwards first to stretch at present, and rate of extraction is difficult to be promoted, and restricts the big of producing line speed
Width is promoted.Difficulty is as follows：1. rate of extraction is accelerated, the length of producing line will be lengthened, increases equipment investment；2. rate of extraction adds
Soon, increase operational difficulty, to personnel's technical ability and equipment precision requirement higher.3. rate of extraction is accelerated, will take out of a large amount of
Solvent, cause the problem of appearance such as film surface piebald, striped.
The Dan Zhibosi of Japan exists《Processing and forming》11st phase page 762 described the technique for first extracting post-tensioning, still
The technique fails to realize industrialized production always, and mainly since current substrate is thicker (0.7-2mm), extraction is difficult, it is difficult to
Realize industrialized production.
Invention content
The technical problems to be solved by the invention are the defects of overcoming the prior art, provide a kind of pore former of battery diaphragm
Minimizing technology, it is improved in the case where not needing to increase battery producing line length, not needing to improve equipment precision and personnel's technical ability
The rate of extraction of battery diaphragm, and especially suitable for the extraction compared with thick skirt substrate, solve thicker substrate extraction difficulty
Problem.
In order to solve the above-mentioned technical problem, the technical scheme is that：A kind of pore former minimizing technology of battery diaphragm,
The step of it is applied in the preparation process of lithium ion secondary battery membrane, method includes：
Diaphragm substrate is pre-processed by equipment, removes at least part pore former in diaphragm substrate in advance；
Extraction processing is carried out to pretreated diaphragm substrate by ultrasonic extraction, pore former is extracted, and ensures
The pore former remnants rates for the battery diaphragm being finally made are less than 1%.
Further for the extraction efficiency for preferably improving diaphragm substrate, during ultrasonic extraction, ultrasonic frequency is
17KHz~28KHz, the time of ultrasonic extraction is more than 10min.
Further provide it is a kind of diaphragm substrate is pre-processed, so as to remove the part in diaphragm substrate into
The concrete structure of the equipment of hole agent, the equipment include scraping roller group equipment and at least one with what at least a pair scraped roller group
The vacuum adsorption equipment of vacuum suction roller, pretreatment include pre-processing diaphragm substrate by scraping roller group and inhaling by vacuum
Attached roller pre-processes diaphragm substrate.
Further, the extractant used during pore former and ultrasonic extraction is the organic solvent that dissolves each other.
Further, the thickness of diaphragm substrate is 0.7mm~2mm.
Further, the pore former is white oil.
Further for the preparation time for preferably reducing lithium ion secondary battery membrane, accelerate the extraction effect of diaphragm substrate
Rate, the preparation process of lithium ion secondary battery membrane include step：Biaxial tension process, pore former minimizing technology are located at two-way
Before stretching process.
The present invention also provides a kind of preparation process of lithium ion secondary battery membrane, the step of technique in contain：
(a) diaphragm substrate is formed after squeezing out and cooling down；
(b) using the pore former minimizing technology；
(c) then carry out biaxial tension；
(d) using the lithium ion secondary battery membrane that stable pore structure is formed with after heat treatment.
A kind of specific step (a) is further provided, step (a) is specially：By polyethylene and pore former as required
The mixing of each component mass percent after add in double screw extruder, fully melt, the melt after melting squeezes by twin-screw
The die head for going out machine squeezes out, and diaphragm substrate is formed on chill roll；Wherein, the mass percent of polyethylene is 15% -50%；
Remaining is pore former, amounts to 100%.
A kind of specific step (c) is further provided, step (c) is specially：To passing through at step (b) at 120 DEG C
Diaphragm substrate after reason carries out the stretching on horizontal and vertical；Wherein, stretching ratio during stretching is 4-9 times.
Can be non-volatile when squeezing out and melting and extraction be volatilized in heat treatment process further for pore former is allowed
Agent forms and stablizes pore structure, the highest melting temperature when boiling temperature of the pore former is squeezed out higher than step (a), ultrasound extraction
Maximum temperature when taking the boiling temperature of the extractant used in the process less than step (d) heat treatment.
After employing above-mentioned technical proposal, the present invention extracts biaxial tension and ultrasound in the technical process for preparing diaphragm
The process taken is exchanged, while diaphragm substrate is scraped by scraping roller group before ultrasonic extraction, can also be inhaled by vacuum
Attached roller adsorbs diaphragm substrate, can remove a part of pore former in diaphragm substrate in advance in this way, remove pore former
Ratio is probably 10% or so, and then diaphragm substrate can enter the extraction tank equipped with Vltrasonic device, by controlling the strong of ultrasonic wave
Degree and frequency, pore former is extracted, and ensures the pore former remnants rates of battery diaphragm being finally made less than 1%, so as to
It is effective to shorten extraction time and accelerate extraction rate, so as to reach the target of high speed production, the diaphragm substrate containing pore former
By scraping the pretreatment of roller group and vacuum suction roller, while it is subject to the ultrasonic wave of 17kHz-28kHz, when can be by the extraction of substrate
Between shortened from 90min to 10min, very effectively solve the problems, such as that thick substrate (0.7mm~2mm) extraction is difficult.
Description of the drawings
Fig. 1 is the structure diagram of the equipment component in the pore former minimizing technology of the battery diaphragm of the present invention.
Specific embodiment
In order that the present invention can be more clearly and readily understood, it is right below according to specific embodiment and with reference to attached drawing
The present invention is described in further detail.
Embodiment one
A kind of pore former minimizing technology of battery diaphragm, it is applied in the preparation process of lithium ion secondary battery membrane,
The step of method, includes：
Diaphragm substrate is pre-processed by equipment, removes at least part pore former in diaphragm substrate in advance；
In the present embodiment, pore former is white oil, and but not limited to this；White oil is at 40 DEG C, kinematic viscosity 45-55mm2/s；
Extraction processing is carried out to pretreated diaphragm substrate by ultrasonic extraction, pore former is extracted, and ensures
The pore former remnants rates for the battery diaphragm being finally made are less than 1%.
During ultrasonic extraction, ultrasonic frequency 17KHz, the time of ultrasonic extraction is 10min.
The equipment includes scraping roller group equipment and at least one vacuum suction roller 2 with what at least a pair scraped roller group 1
Vacuum adsorption equipment, pretreatment include pre-processing diaphragm substrate by scraping roller group 1 and by vacuum suction roller 2 to every
Film substrate is pre-processed, and after pretreatment, by weighing the weight change before and after diaphragm substrate, scrapes roller group 1 and vacuum is inhaled
The pore former rate of going of attached roller 2 is 10%；
The extractant used during pore former and ultrasonic extraction is the organic solvent that dissolves each other.
The thickness of diaphragm substrate in the present embodiment is 1mm.
The preparation process of lithium ion secondary battery membrane includes step：Biaxial tension process, pore former minimizing technology position
Before biaxial tension process.
A kind of preparation process of lithium ion secondary battery membrane, it is removed using the pore former of the battery diaphragm of the present embodiment
Contain in the step of method, preparation process：
(a) diaphragm substrate is formed after squeezing out and cooling down；
(b) using pore former minimizing technology；
(c) then carry out biaxial tension；
(d) using the lithium ion secondary battery membrane that stable pore structure is formed with after heat treatment.
Step (a) is specially：It is added in after polyethylene is mixed with each component mass percent of pore former as required double
It in screw extruder, is fully melted at 195 DEG C, the melt after melting squeezes out, and by the die head of double screw extruder 25
DEG C chill roll on formed 1mm thickness diaphragm substrate；Wherein, the mass percent of polyethylene is 30%, the molecular weight of polyethylene
It is 800,000, the molecular weight of the polyethylene can be in 300,000-350 ten thousand, preferably 300,000-250 ten thousand；Pore former is white oil, matter
It is 70% to measure percentage；In the present embodiment, the mass percent of polyethylene and pore former is respectively：30% and 70%, still
Without being limited thereto, the mass percent of polyethylene and pore former can also be respectively：15% and 85%；It can also be respectively 50% He
50%；The mass percent of polyethylene can select between 15%~50%.
Step (c) is specially：To being carried out on horizontal and vertical by step (b) treated diaphragm substrate at 120 DEG C
5 times stretching；Certainly, stretching ratio during stretching can select in 4-9 times, be not limited to 5 times of stretchings.
Highest melting temperature when the boiling temperature of the pore former is squeezed out higher than step (a) is adopted during ultrasonic extraction
The maximum temperature when boiling temperature of extractant is heat-treated less than step (d)；In the present embodiment, the boiling of the pore former
For point temperature higher than 210 DEG C, highest melting temperature during extrusion is 195 DEG C；Maximum temperature in step (d) during heat treatment is 130
℃。
The principle that the ultrasonic unit 4 of the present embodiment cleans, by energy converter, converts acoustic energy into mechanical energy, makes extraction
Cleaning solution in slot 3 generates vibration, generates a large amount of bubbles.When acoustic pressure or the sound intensity are under pressure arrival to a certain degree, gas
Bubble will expand rapidly, then be closed suddenly again.During this section, the moment that bubble is closed generates shock wave, makes bubble all
The pressure and bureau of temperature adjustment for generating 1012-1013pa are enclosed, immense pressure can destroy insoluble dirt caused by this ultrasonic cavitation
Object and make they break up in solution, therefore, using ultrasonic extraction diaphragm substrate, can effectively improve extraction efficiency, shorten
Extraction time.
Embodiment two
The present embodiment and embodiment one are essentially identical, unlike：During ultrasonic extraction, ultrasonic frequency is
28KHz, the time of ultrasonic extraction is 10min.
Embodiment three
The present embodiment and embodiment one are essentially identical, unlike：During ultrasonic extraction, ultrasonic frequency is
17KHz, the time of ultrasonic extraction is 15min.
Comparative example one
The present embodiment and embodiment one are essentially identical, unlike：The present embodiment does not use ultrasonic extraction, using conventional extraction
Mode is taken, in extraction process, the time of extraction is 10min.
Comparative example two
The present embodiment and embodiment one are essentially identical, unlike：During ultrasonic extraction, ultrasonic frequency is
120KHz, the time of ultrasonic extraction is 10min.
Comparative example three
The present embodiment and embodiment one are essentially identical, unlike：During ultrasonic extraction, ultrasonic frequency is
17KHz, the time of ultrasonic extraction is 5min.
The evaluation of above example and comparative example to effect of extracting generally uses pore former remnants rates and ventilative Gurley values
To characterize；
Pore former remnants rates are smaller, then effect of extracting is better；The Gurley values of film are lower, and the gas permeability for characterizing film is got over
It is good.
The acquisition method of pore former remnants rates is：Diaphragm substrates of the 10cm × 10cm through Overheating Treatment is cut, with electronics day
Its weight of flat weighing m1, after diaphragm substrate is extracted, taking-up, which is put in draught cupboard, dries, again its weight of weighing m2, then the diaphragm
The pore former remnants rates of substrate are：(m1-m2)/m1。
The acquisition method of ventilative value is：It is tested with Gurley, the diaphragm base that 100ml air is accumulated by 1 inch of circular section of φ
The piece required time.
General pore former remnants rates influence the ventilative value of film as follows
| Pore former remnants rates (%) | 3.4 | 2.1 | 0.8 | 0.4 |
| Ventilative value (s/100ml) | 485 | 367 | 216 | 204 |
When pore former remnants rates are less than 1%, the ventilative value ＜ 300s/100ml of microporous barrier, diaphragm substrate characteristics conjunction at this time
Lattice.
The pore former remnants rates and ventilative value such as following table of above example and comparative example acquisition：
| Embodiment one | Embodiment two | Embodiment three | Comparative example one | Comparative example two | Comparative example three | |
| Pore former remnants rates (%) | 0.79 | 0.87 | 0.18 | 0.41 | 1.81 | 1.58 |
| Ventilative value (s/100ml) | 236 | 243 | 221 | 227 | 437 | 412 |
It can be seen that by above example and comparative example and work as the diaphragm substrate for containing pore former by scraping roller group 1 and vacuum
After the pretreatment of adsorption roller 2, then by ultrasonic extraction, the extraction time of diaphragm substrate can be shortened, and solve thick substrate extraction
The problem of difficult, when the ultrasonic wave for being subject to 17kHz-28kHz, when the extraction time of diaphragm substrate shortens more than 10min, extraction
Excellent, this section are the Best Frequency Range and optimum extraction time of ultrasonic parameters.
Particular embodiments described above, pair present invention solves the technical problem that, technical solution and advantageous effect carry out
It is further described, it should be understood that the above is only a specific embodiment of the present invention, is not limited to this
Invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done should be included in this hair
Within bright protection domain.
Claims (10)
1. a kind of pore former minimizing technology of battery diaphragm, it is applied in the preparation process of lithium ion secondary battery membrane,
The step of being characterized in that method includes：
Diaphragm substrate is pre-processed by equipment, removes at least part pore former in diaphragm substrate in advance；
Extraction processing is carried out to pretreated diaphragm substrate by ultrasonic extraction, pore former is extracted, and is ensured final
The pore former remnants rates of manufactured battery diaphragm are less than 1%.
2. pore former minimizing technology according to claim 1, it is characterised in that：During ultrasonic extraction, ultrasonic wave frequency
Rate is 17KHz~28KHz, and the time of ultrasonic extraction is more than 10min.
3. pore former minimizing technology according to claim 1, it is characterised in that：The equipment includes that there is at least a pair to scrape
Roller group (1) scrapes roller group equipment and the vacuum adsorption equipment at least one vacuum suction roller (2), and pretreatment is included by scraping
Roller group (1) pre-processes diaphragm substrate and diaphragm substrate is pre-processed by vacuum suction roller (2).
4. pore former minimizing technology according to claim 1, it is characterised in that：It is used during pore former and ultrasonic extraction
Extractant be the organic solvent to dissolve each other.
5. pore former minimizing technology according to claim 1, it is characterised in that：The thickness of diaphragm substrate for 0.7mm~
2mm。
6. pore former minimizing technology according to claim 1, it is characterised in that：The preparation work of lithium ion secondary battery membrane
Skill includes step：Biaxial tension process, pore former minimizing technology are located at before biaxial tension process.
7. a kind of preparation process of lithium ion secondary battery membrane, it is characterised in that contain in the step of technique：
(a) diaphragm substrate is formed after squeezing out and cooling down；
(b) using such as pore former minimizing technology according to any one of claims 1 to 6；
(c) then carry out biaxial tension；
(d) using the lithium ion secondary battery membrane that stable pore structure is formed with after heat treatment.
8. preparation process according to claim 8, it is characterised in that：Step (a) is specially：Polyethylene and pore former are pressed
According to being added in double screw extruder after each component mass percent mixing of needs, fully melt, the melt after melting is by double
The die head of screw extruder squeezes out, and diaphragm substrate is formed on chill roll；Wherein, the mass percent of polyethylene for 15%-
50%；Remaining is pore former, amounts to 100%.
9. preparation process according to claim 8, it is characterised in that：Step (c) is specially：To by walking at 120 DEG C
Suddenly (b) treated diaphragm substrate carries out the stretching on horizontal and vertical；Wherein, stretching ratio during stretching is 4-9 times.
10. preparation process according to claim 8, it is characterised in that：The boiling temperature of the pore former is higher than step (a)
Highest melting temperature during extrusion, when the boiling temperature of extractant used during ultrasonic extraction is heat-treated less than step (d)
Maximum temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711430523.XA CN108183190B (en) | 2017-12-26 | 2017-12-26 | Pore-forming agent removing method of battery diaphragm and preparation process of lithium ion secondary battery diaphragm |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711430523.XA CN108183190B (en) | 2017-12-26 | 2017-12-26 | Pore-forming agent removing method of battery diaphragm and preparation process of lithium ion secondary battery diaphragm |
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| CN108183190B CN108183190B (en) | 2021-03-19 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111081948A (en) * | 2019-12-26 | 2020-04-28 | 江苏厚生新能源科技有限公司 | Preparation method of high linear velocity-large width polyethylene diaphragm |
| CN112439224A (en) * | 2020-09-29 | 2021-03-05 | 河北金力新能源科技股份有限公司 | Diaphragm extraction system |
| CN112864528A (en) * | 2021-04-26 | 2021-05-28 | 江苏厚生新能源科技有限公司 | Biaxial tension coating microporous diaphragm for lithium ion battery and preparation method thereof |
| CN113871791A (en) * | 2021-08-25 | 2021-12-31 | 江西省通瑞新能源科技发展有限公司 | High-pressure-resistance diaphragm for lithium ion battery and preparation method thereof |
| CN114851506A (en) * | 2022-07-07 | 2022-08-05 | 溧阳月泉电能源有限公司 | Manufacturing process of lithium battery polyolefin diaphragm |
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| US4252756A (en) * | 1979-06-27 | 1981-02-24 | General Motors Corporation | Process for manufacturing ultra-thin sintered PVC battery separators |
| CN106450112A (en) * | 2016-11-25 | 2017-02-22 | 上海恩捷新材料科技股份有限公司 | Battery isolating membrane preparation method |
| CN106531930A (en) * | 2016-10-28 | 2017-03-22 | 深圳瑞隆新能源科技有限公司 | Paraffin oil-containing wet diaphragm production process |
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| US4252756A (en) * | 1979-06-27 | 1981-02-24 | General Motors Corporation | Process for manufacturing ultra-thin sintered PVC battery separators |
| CN106531930A (en) * | 2016-10-28 | 2017-03-22 | 深圳瑞隆新能源科技有限公司 | Paraffin oil-containing wet diaphragm production process |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111081948A (en) * | 2019-12-26 | 2020-04-28 | 江苏厚生新能源科技有限公司 | Preparation method of high linear velocity-large width polyethylene diaphragm |
| CN112439224A (en) * | 2020-09-29 | 2021-03-05 | 河北金力新能源科技股份有限公司 | Diaphragm extraction system |
| CN112864528A (en) * | 2021-04-26 | 2021-05-28 | 江苏厚生新能源科技有限公司 | Biaxial tension coating microporous diaphragm for lithium ion battery and preparation method thereof |
| CN113871791A (en) * | 2021-08-25 | 2021-12-31 | 江西省通瑞新能源科技发展有限公司 | High-pressure-resistance diaphragm for lithium ion battery and preparation method thereof |
| CN114851506A (en) * | 2022-07-07 | 2022-08-05 | 溧阳月泉电能源有限公司 | Manufacturing process of lithium battery polyolefin diaphragm |
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Effective date of registration: 20211207 Address after: 611500 No. 420, Tianlai 1st Road, new energy and new material industry functional zone, Tianfu new area, Qionglai City, Chengdu City, Sichuan Province Patentee after: Sichuan zhuoqin New Material Technology Co.,Ltd. Address before: 213300 no.619, wharf West Street, Liyang City, Changzhou City, Jiangsu Province Patentee before: LIYANG TNS ELECTRO-ENERGY Co.,Ltd. |