CN103400954A - Polyvinylidene fluoride micropore diaphragm - Google Patents
Polyvinylidene fluoride micropore diaphragm Download PDFInfo
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- CN103400954A CN103400954A CN2013103136422A CN201310313642A CN103400954A CN 103400954 A CN103400954 A CN 103400954A CN 2013103136422 A CN2013103136422 A CN 2013103136422A CN 201310313642 A CN201310313642 A CN 201310313642A CN 103400954 A CN103400954 A CN 103400954A
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- kynoar
- supercritical
- autoclave
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- pressure
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a polyvinylidene fluoride micropore diaphragm which is mainly applied to a lithium ion battery. The micropore diaphragm is prepared by a supercritical fluid phase separation method.
Description
Technical field
The present invention relates to a kind of Kynoar micro-pore septum, it is mainly used in lithium ion battery.
Background technology
Lithium ion battery is high with its energy density, have extended cycle life and the electrical property of the high excellence of voltage and obtained development rapidly.The electronic product fields such as mobile phone, portable computer, camera, video camera have been widely used at present.Lithium ion battery is divided into again liquid lithium ionic cell and solid lithium ion battery, solid lithium ion battery generally is called polymer Li-ion battery or plastic lithium-ion battery, its operation principle is identical with liquid lithium ionic cell, the electrolyte of different is polymer Li-ion battery is not free electrolyte, but gel electrolyte or solid electrolyte.Polymer dielectric not only has high ionic conductivity, long cycle life, minimum pollution level and good processing characteristics, the flexibility that has again simultaneously better fail safe, configuration design, it is used for replacing liquid electrolyte, can overcome the problem that the liquid electrolyte lithium ion battery exists at aspects such as capacity, security performances, for lithium ion battery provides advantage to all solid state, ultrathin development.Thereby this battery become the focus of the research and development of chemical power source in recent years, and extraordinary development prospect is arranged.
At present, polymer lithium ion battery electrolyte membrane properties quality directly affects optimization and the raising of polymer Li-ion battery performance., to the preparation of this class microporous polymer electrolyte barrier film, mainly contain at present the methods such as immersion precipitation is separated and thermic is separated.The disadvantage of immersion precipitation is the film that is difficult to obtain symmetrical configuration, and finger-like pore easily occurs, and this is unfavorable for contacting between barrier film and electrode.Studying in recent years more is thermally induced phase separation, its advantage is that pore-size distribution is narrow, symmetrical configuration, without finger-like pore, shortcoming is that easily to present between blind hole structure, hole connectivity poor, thereby be unfavorable for that ion passes through, and need to use a large amount of solvents in preparation process, easily cause the problems such as environmental pollution.
Summary of the invention
The objective of the invention is the deficiency for above-mentioned preparation method, a kind of Kynoar micro-pore septum is provided.
The technical solution used in the present invention is: a kind of Kynoar micro-pore septum, adopt the following methods preparation:
(1) Kynoar is placed on freeze-day with constant temperature 10～15h in drying box, to remove moisture content wherein, that dried Kynoar sealing is standby;
(2) with the accurate weighing Kynoar of electronic balance particle, and add the organic solvent that dissolves Kynoar, be made into mass concentration and be 25% casting solution;
(3) after Kynoar dissolves fully and stirs, sealing standing a period of time of black out, remove gas remaining in solution; Striking Kynoar solution film thickness is 200～300 μ m;
(4) setting bath temperature is 50～80 ℃, keeps constant after, open compressor and setting pressure, then opening high pressure gas cylinder and lasting several seconds, to blow away ducted air, then close gas cylinder;
The casting film dish that (5) will be loaded with casting solution is inserted in autoclave and is sealed rapidly;
(6) gas in gas cylinder is pressurized the pump pressure contracting, first sends into preheater and carries out preheating, then be pressed into autoclave, pressure setting is 20～30MPa, make the gas in autoclave be in supercriticality, become supercritical fluid, the dwell time is 50～80min;
(7) control valve of device for opening outlet, purge continuously to autoclave, finally system carried out slow pressure release, and the gas flow during pressure release is controlled at 0～0.3m3/h;
(8) last opening high pressure still, take out the barrier film sample of preparation.
Described supercritical fluid is selected from supercritical carbon dioxide, supercritical methane, overcritical ethane, supercritical propane, overcritical ethene, supercritical n pentane.
Described organic solvent is selected from methyl alcohol, ethanol, acetone, benzene, toluene, 1-METHYLPYRROLIDONE, DMF, oxolane, polyvinylpyrrolidone, dimethyl sulfoxide (DMSO), sulfolane.
The invention has the beneficial effects as follows: thisly with supercritical fluid, be separated and prepare membrane for polymer technique, utilize supercritical fluid can the swelling most polymers, can dissolve many micromolecular characteristics again, use the non-solvent of supercritical fluid as the casting film system, exchange by supercritical fluid and organic solvent makes supercritical fluid enter into polymer solution, and solution is separated, thereby obtain needed barrier film, this process is supercritical fluid and is separated and prepares membrane process.This preparation technology's advantage is: 1) supercritical fluid not only makes polymer solution be separated, also can play " drying " effect to formed microporous barrier (polymer-rich phase), thereby being separated in traditional L-S method united two into one with drying process thereafter; 2) because supercritical fluid can not produce vapour-liquid interface (without phase transformation) to the dry run of film, thereby avoided the structural collapse problem that very easily occurs in the film dry run; 3) organic solvent that dissolves each other with supercritical fluid can, by recycling after simple decompression separation operation, make whole film preparation process become the enclosed type technical process of a kind of " green "; 4) this technique has been introduced pressure as extra variable, also can regulate the phase process of system by the pressure that changes supercritical fluid, thus the morphosis of energy Effective Regulation film.
Embodiment
Below by specific embodiment, technical scheme of the present invention and the effect that reaches thereof are described further, but following instance does not form limitation of the invention.
A kind of Kynoar micro-pore septum, adopt the following methods preparation:
(1) Kynoar is placed on freeze-day with constant temperature 10～15h in drying box, to remove moisture content wherein, that dried Kynoar sealing is standby;
(2) with the accurate weighing Kynoar of electronic balance particle, and add the organic solvent that dissolves Kynoar, be made into mass concentration and be 25% casting solution;
(3) after Kynoar dissolves fully and stirs, sealing standing a period of time of black out, remove gas remaining in solution; Striking Kynoar solution film thickness is 200～300 μ m;
(4) setting bath temperature is 50～80 ℃, keeps constant after, open compressor and setting pressure, then opening high pressure gas cylinder and lasting several seconds, to blow away ducted air, then close gas cylinder;
The casting film dish that (5) will be loaded with casting solution is inserted in autoclave and is sealed rapidly;
(6) gas in gas cylinder is pressurized the pump pressure contracting, first sends into preheater and carries out preheating, then be pressed into autoclave, pressure setting is 20～30MPa, make the gas in autoclave be in supercriticality, become supercritical fluid, the dwell time is 50～80min;
(7) control valve of device for opening outlet, purge continuously to autoclave, finally system carried out slow pressure release, and the gas flow during pressure release is controlled at 0～0.3m
3/ h;
(8) last opening high pressure still, take out the barrier film sample of preparation.
(9) the micropore polymer diaphragm sample that takes out is dried, obtain final product.
Claims (3)
1. Kynoar micro-pore septum, it adopts the following methods preparation:
1) Kynoar is placed on freeze-day with constant temperature 10～15h in drying box, to remove moisture content wherein, that dried Kynoar sealing is standby;
2) with the accurate weighing Kynoar of electronic balance particle, and add the organic solvent that dissolves Kynoar, be made into mass concentration and be 25% casting solution;
3) after Kynoar dissolves fully and stirs, sealing standing a period of time of black out, remove gas remaining in solution; Striking Kynoar solution film thickness is 200～300 μ m;
4) setting bath temperature is 50～80 ℃, keeps constant after, open compressor and setting pressure, then opening high pressure gas cylinder and lasting several seconds, to blow away ducted air, then close gas cylinder;
The casting film dish that 5) will be loaded with casting solution is inserted in autoclave and is sealed rapidly;
6) gas in gas cylinder is pressurized the pump pressure contracting, first sends into preheater and carries out preheating, then be pressed into autoclave, pressure setting is 20～30MPa, make the gas in autoclave be in supercriticality, become supercritical fluid, the dwell time is 50～80min;
7) control valve of device for opening outlet, purge continuously to autoclave, finally system carried out slow pressure release, and the gas flow during pressure release is controlled at 0～0.3m
3/ h;
8) last opening high pressure still, take out the barrier film sample of preparation.
2. Kynoar micro-pore septum claimed in claim 1, is characterized in that, described supercritical fluid is selected from supercritical carbon dioxide, supercritical methane, overcritical ethane, supercritical propane, overcritical ethene, supercritical n pentane.
3. Kynoar micro-pore septum claimed in claim 1, it is characterized in that, described organic solvent is selected from methyl alcohol, ethanol, acetone, benzene, toluene, 1-METHYLPYRROLIDONE, DMF, oxolane, polyvinylpyrrolidone, dimethyl sulfoxide (DMSO), sulfolane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103136422A CN103400954A (en) | 2013-07-24 | 2013-07-24 | Polyvinylidene fluoride micropore diaphragm |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103136422A CN103400954A (en) | 2013-07-24 | 2013-07-24 | Polyvinylidene fluoride micropore diaphragm |
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| CN103400954A true CN103400954A (en) | 2013-11-20 |
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| CN2013103136422A Pending CN103400954A (en) | 2013-07-24 | 2013-07-24 | Polyvinylidene fluoride micropore diaphragm |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6558607B1 (en) * | 1999-09-30 | 2003-05-06 | University Of Massachusetts | Crystallization of constrained polymers |
| CN102070793A (en) * | 2010-12-22 | 2011-05-25 | 大连理工大学 | Process for preparing polymer lithium ion battery microporous membrane by supercritical fluid phase separation |
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2013
- 2013-07-24 CN CN2013103136422A patent/CN103400954A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6558607B1 (en) * | 1999-09-30 | 2003-05-06 | University Of Massachusetts | Crystallization of constrained polymers |
| CN102070793A (en) * | 2010-12-22 | 2011-05-25 | 大连理工大学 | Process for preparing polymer lithium ion battery microporous membrane by supercritical fluid phase separation |
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Application publication date: 20131120 |