CN101905555A - Flame-retardant porous polymer film and preparation method thereof - Google Patents
Flame-retardant porous polymer film and preparation method thereof Download PDFInfo
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- CN101905555A CN101905555A CN2010102208294A CN201010220829A CN101905555A CN 101905555 A CN101905555 A CN 101905555A CN 2010102208294 A CN2010102208294 A CN 2010102208294A CN 201010220829 A CN201010220829 A CN 201010220829A CN 101905555 A CN101905555 A CN 101905555A
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a preparation method for a flame-retardant porous polymer film. The method comprises the following steps of: a, dissolving the polymer with an organic solvent and adding a pore-forming agent into the dissolved polymer to obtain emulsion; b, coating the emulsion on a matrix and carrying out drying or extraction treatment on the matrix to obtain a porous polymer-based film; and c, plating an aluminum hydroxide film on the surface of the porous polymer-based film and heating the obtained product to decompose the aluminum hydroxide on the surface of the matrix into aluminum oxide to obtain the flame-retardant porous polymer film. The invention also provides the flame-retardant porous polymer film prepared by the method and a battery containing the same. The flame-retardant porous polymer film prepared by the method of the invention has uniformly dispersed aluminum oxide, so that the obtained flame-retardant porous polymer film has uniform flame retardance and the use safety of the battery is improved.
Description
Technical field
The present invention relates to flame retardant area, relate in particular to fire-retardant porous polymer film and preparation method thereof.
Background technology
Easily cause the inside battery burning when both positive and negative polarity of lithium ion battery is short-circuited, thereby the security that whole consumer is used impacts.In order to address this problem, between the both positive and negative polarity of battery, add flame-retardant layer usually, simultaneously in order not influence the migration of lithium ion between the both positive and negative polarity in the battery, the flame-retardant layer of use need have loose structure.Positive pole, negative pole or membrane surface at battery apply the porous polymer film with fire resistance, the internal-combustion phenomenon that can avoid battery to cause because of short circuit, the security performance of raising consumer.
Traditional fire-retardant porous polymer film prepares with phase inversion method usually, phase inversion method is with a kind of solvent polymer and pore creating material evenly to be disperseed, and the mode that re-uses another kind of solvent extraction or directly volatilization behind the system film to be dried is separated pore creating material from film.Concrete preparation method is: with PVDF (Vingon), PVDF-HFP (Vingon-hexafluoropropene), PAN polymer such as (polyacrylonitrile) as fire-retardant matrix, then fire-retardant matrix is added pore creating material after with organic solvent dissolution, then solution is applied as polymer film, again polymer film is carried out drying, utilize when dry that the rate of volatilization of different component is different to come pore-creating, perhaps use solvent to extract pore-creating dried polymer film.Adopt said method can prepare the apertured polymeric film that membrane pores is even, imbibition ability is strong, but film strength and fire resistance deficiency.In order to improve film strength and fire resistance, the preparation method of existing fire-retardant porous membrane is: add Al in the polymer solution that contains pore creating material
2O
3Powder is as reinforcing agent, solution stirred into coating film forming behind the suspension, but adopt the shortcoming of said method to be Al
2O
3Powder is easily reunited in solution, therefore, and Al
2O
3Powder is difficult to be scattered in the solution system uniformly, thereby makes Al
2O
3Skewness in film, thus, one side Al
2O
3Bulky grain after the reunion can stop up fenestra, influences the operate as normal of battery, does not have Al on the other hand around the part fenestra
2O
3Distribute, cause the local poor fire of film, have potential safety hazard in use for battery.
Summary of the invention
In order to solve above technical problem, the invention provides a kind of preparation method of fire-retardant porous polymer film, adopt Al in the thin polymer film that this method prepares
2O
3Be uniformly dispersed, fire resistance is even.
In view of this, the invention provides a kind of preparation method of fire-retardant porous polymer film, comprising:
The present invention also provides a kind of fire-retardant porous polymer film of preparing according to the method described above.
The present invention also provides a kind of battery, comprising:
The invention provides a kind of preparation method of fire-retardant porous polymer film, with respect to prior preparation method, the present invention uses phase inversion method to form porous polymer-based film at battery anode slice, negative plate or membrane surface earlier, use chemical method after the porous polymer-based film surface plates aluminum hydroxide film, to heat then, the aluminium hydroxide decomposes generates aluminium oxide, thereby obtain containing the porous polymer film of aluminium oxide reinforced flame retardant, therefore adopt method provided by the invention can avoid Al
2O
3Powder is reunited in the polymer thin film system, and because the aluminium hydroxide film is evenly to be plated on the porous polymer-based film surface, therefore the aluminium oxide that forms after the aluminium hydroxide decomposes also is to be dispersed in the porous polymer-based film surface, therefore, adopt method preparation provided by the invention can prepare the finely dispersed fire-retardant porous polymer film of aluminium oxide, and then make the fire-retardant porous polymer film that obtains have uniform anti-flammability, and then improved the security that battery uses.
The specific embodiment
In order to make those skilled in the art further understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, but should be appreciated that these describe just to further specifying the features and advantages of the present invention, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of preparation method of fire-retardant porous polymer film, comprising:
A, polymer is added pore creating material after with organic solvent dissolution, obtain emulsion;
B, the emulsion that step a is obtained are coated on and carry out drying behind the matrix or extraction is handled, and obtain porous polymer-based film;
C, heat behind porous polymer-based film that step b obtains surface plating aluminum hydroxide film, the aluminium hydroxide decomposes of matrix surface generates aluminium oxide, obtains fire-retardant porous polymer film.
Step a to b is that phase inversion method prepares porous polymer-based film, wherein polymer preferably adopts one or more in Kynoar (PVDF), Kynoar-hexafluoropropene (PVDF-HFP) and the polyacrylonitrile (PAN), because above-mentioned polymer not only has heat-resisting quantity, oxidative resistance preferably, also has stronger absorbent; Preferably above-mentioned polymer is added pore creating material with acetone or oxolane (THF) equal solvent dissolving back, to utilize when dry different component rate of volatilization difference to carry out pore-creating behind the solution coating filmform again, or film extracted pore-creating in extractant, according to the present invention, pore creating material is preferably selected water, ethanol or dibutyl phthalate for use, when using dibutyl phthalate as pore creating material, the preferred methyl alcohol that adopts is as extractant, and described matrix can be positive plate, negative plate or the barrier film of battery.Make porous polymer-based film through step a, b.
Step c is to use chemical method to form aluminum hydroxide film earlier on the porous polymer-based film that step b makes, the porous polymer-based film that the surface is contained aluminum hydroxide film heats again, aluminium hydroxide is decomposed to form aluminium oxide, prepare the fire-retardant porous polymer film that contains aluminium oxide thus, and aluminium oxide is to be dispersed in the film.Wherein the method that forms the aluminium hydroxide film on porous polymer-based film preferably adopts following four kinds of modes:
Mode one: will immerse alum solution again behind the described porous polymer-based film immersion sodium radio-phosphate,P-32 solution, following chemical reaction takes place in the porous polymer-based film surface:
Na
3PO
4+KAl(SO
4)
2·12H
2O＝Al(OH)
3↓+3Na
++K
++3H
++2(SO
4)
2-+(PO
4)
3-+9H
2O
The porous polymer-based film surface forms aluminum hydroxide film.
Mode two: will immerse sodium aluminate solution again behind the described porous polymer-based film immersion aluminum sulfate solution, following chemical reaction takes place in the porous polymer-based film surface:
Al
2(SO
4)
3+6NaAlO
2+12H
2O＝8Al(OH)
3↓+3Na
2SO
4
The porous polymer-based film surface forms aluminum hydroxide film.
Mode three: will immerse sodium carbonate liquor again behind the described porous polymer-based film immersion aluminum sulfate solution, on the porous polymer-based film surface following chemical reaction takes place like this:
Al
2(SO
4)
3+2Na
2CO
3+3H
2O＝2Al(OH)
3↓+3Na
2SO
4+3CO
2
The porous polymer-based film surface forms aluminum hydroxide film.
Mode four: will immerse again in the ammoniacal liquor behind the described porous polymer-based film immersion liquor alumini chloridi, on the porous polymer-based film surface following chemical reaction takes place like this:
AlCl
3+3NH
3·H
2O＝Al(OH)
3↓+3NH
4Cl
The porous polymer-based film surface forms aluminum hydroxide film.
Obtain being coated with on the porous polymer-based film aluminum hydroxide film according to above-mentioned steps, then this is coated with the porous polymer-based film heating of aluminum hydroxide film, the aluminium hydroxide decomposes forms aluminium oxide, obtain the homodisperse fire-retardant porous polymer film of aluminium oxide thus, heating-up temperature is preferably 120 ℃～150 ℃, more preferably 130 ℃～140 ℃, in order to remove impurity attached to fire-retardant porous polymer film surface, also preferably will fire-retardant porous polymer film with washed with de-ionized water after drying.
The present invention also provides a kind of battery, comprising: positive plate, negative plate, barrier film, electrolyte and shell, positive plate, negative plate or membrane surface apply the fire-retardant porous polymer film of preparing according to the method described above.Described fire-retardant porous polymer film has uniform fire resistance, so the safety coefficient that battery uses is higher.
In order further to understand the present invention, the preparation method of fire-retardant porous polymer film provided by the invention is described below in conjunction with embodiment.
Embodiment 1
1, gets 5gPVDF, 10gPVDF-HFP respectively and mix and be dissolved in the 80g tetrahydrofuran solution, add 5g ethanol, obtain emulsion after stirring.
2, the emulsion that step 1 is obtained carries out drying after being sprayed at the battery anode slice surface, obtains porous polymer-based film.
3, the porous polymer-based film that step 2 is obtained immerses the Na of 30wt%
3PO
4Dry behind the solution, dry behind the alum solution with dried porous polymer-based film immersion 30wt%, the porous polymer surface forms aluminum hydroxide film, again this film is heated to 135 ℃, obtains fire-retardant porous polymer film.
Embodiment 2
1, getting 5gPVDF, 10gPVDF-HFP is dissolved in 80g oxolane dissolving back and adds and obtain emulsion after the 5g dibutyl phthalate stirs.
2, the emulsion that step 1 is obtained carries out drying after being sprayed at PE nonwoven membrane surface, obtains polymer-based film.
3, the polymer-based film that step 2 is obtained extracts with methyl alcohol, obtains porous polymer-based film.
4, the porous polymer-based film that step 3 is obtained immerses the Al of 20wt%
2(SO
4)
3Dry behind the solution, with the NaAlO of dried porous polymer-based film immersion 50wt%
2Dry behind the solution, the porous polymer surface forms aluminum hydroxide film, again this film is heated to 135 ℃, obtains fire-retardant porous polymer film.
Comparative example 1
1, gets 5gPVDF, 10gPVDF-HFP respectively and mix and be dissolved in the 80g tetrahydrofuran solution, add 5g water, obtain emulsion after stirring.
2, the emulsion that step 1 is obtained adds 3g nanometer Al
2O
3Powder carries out high speed dispersion, obtains suspension.
3, the suspension that step 2 is obtained carries out drying after being sprayed at the battery anode slice surface, obtains porous polymer-based film.
The battery of getting 100 fire-retardant porous polymer films that contain embodiment 1 is numbered a1～a100 as test battery; The battery of getting 100 fire-retardant porous polymer films that contain embodiment 2 is numbered b1～b100 as test battery; The battery of getting 100 fire-retardant porous polymer films that contain comparative example 1 is numbered c1～c100 as test battery.Above-mentioned test battery is overcharged experiment, overcharge experiment condition and be: test battery is charged with 3 times of electric currents, when cell voltage is charged to 10V, stop charging,, be considered as not by experiment if battery is blasted in charging process; If battery is considered as by test finishing abnormal conditions do not take place yet to charging.Above-mentioned test battery overcharges the experimental result of experiment and lists in table 1:
Table 1 overcharges experimental result
By The above results as can be known, the fire-retardant porous polymer film fire resistance that adopts method provided by the invention to prepare is even, the battery security height.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined herein General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. the preparation method of a fire-retardant porous polymer film is characterized in that, comprising:
A, polymer is added pore creating material after with organic solvent dissolution, obtain emulsion;
B, described emulsion is coated on carries out drying behind the matrix or extraction is handled, obtain porous polymer-based film;
C, heat behind described porous polymer-based film surface plating aluminum hydroxide film, the aluminium hydroxide decomposes of matrix surface generates aluminium oxide, obtains fire-retardant porous polymer film.
2. method according to claim 1 is characterized in that, described polymer is one or more in Kynoar, Kynoar-hexafluoropropene and the polyacrylonitrile.
3. method according to claim 1 is characterized in that, described pore creating material is water, ethanol or dibutyl phthalate.
4. method according to claim 1 is characterized in that, is specially at described porous polymer-based film surface plating aluminum hydroxide film among the step c:
To immerse alum solution again behind the described porous polymer-based film immersion sodium radio-phosphate,P-32 solution.
5. method according to claim 1 is characterized in that, is specially at described porous polymer-based film surface plating aluminum hydroxide film among the step c:
To immerse sodium aluminate solution again behind the described porous polymer-based film immersion aluminum sulfate solution.
6. method according to claim 1 is characterized in that, is specially at described porous polymer-based film surface plating aluminum hydroxide film among the step c:
To immerse sodium carbonate liquor again behind the described porous polymer-based film immersion aluminum sulfate solution.
7. method according to claim 1 is characterized in that, is specially at described porous polymer-based film surface plating aluminum hydroxide film among the step c:
To immerse in the ammoniacal liquor again behind the described porous polymer-based film immersion liquor alumini chloridi.
8. method according to claim 1 is characterized in that, the temperature that described porous polymer-based film is heated is 120 ℃～150 ℃.
9. the fire-retardant porous polymer film of any method preparation of claim 1 to 8.
10. a battery is characterized in that, comprising: positive plate, negative plate, barrier film, electrolyte and shell is characterized in that described positive plate, negative plate or membrane surface apply fire-retardant porous polymer film as claimed in claim 9.
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| CN2010102208294A CN101905555A (en) | 2010-07-02 | 2010-07-02 | Flame-retardant porous polymer film and preparation method thereof |
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| CN2010102208294A CN101905555A (en) | 2010-07-02 | 2010-07-02 | Flame-retardant porous polymer film and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134329A (en) * | 2011-02-14 | 2011-07-27 | 中南大学 | Aluminum oxide modified polymer electrolyte thin film and preparation method thereof |
| CN103904270A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103904272A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103904275A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103972444A (en) * | 2013-01-28 | 2014-08-06 | 海洋王照明科技股份有限公司 | Electrochemical power supply separation membrane and preparation method thereof, electrochemical battery or capacitor |
| CN105552285A (en) * | 2015-12-30 | 2016-05-04 | 东莞漠泉新材料科技有限公司 | Ceramic coating diaphragm, preparation method thereof and application in lithium ion battery |
| CN107978780A (en) * | 2016-10-21 | 2018-05-01 | 中国科学院大连化学物理研究所 | The preparation and film and application of a kind of organic and inorganic Multi-layer composite proton exchange membrane |
| CN108123155A (en) * | 2016-11-28 | 2018-06-05 | 中国科学院金属研究所 | A kind of preparation method of non-fluorine porous composite film used for all-vanadium redox flow battery |
| CN108134108A (en) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | A kind of Kynoar-application of the hexafluoropropene diaphragm in flow battery |
| WO2019154275A1 (en) * | 2018-02-06 | 2019-08-15 | 比亚迪股份有限公司 | Polymer separator, preparation method therefor and use thereof, and lithium-ion battery and preparation method therefor |
| CN110380022A (en) * | 2019-06-26 | 2019-10-25 | 荆门市格林美新材料有限公司 | A kind of high voltage monocrystalline nickel-cobalt-manganternary ternary anode material and preparation method |
| CN111697188A (en) * | 2020-06-23 | 2020-09-22 | 南京理工大学 | Lithium-sulfur battery interlayer with flame retardant property and preparation method thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134329A (en) * | 2011-02-14 | 2011-07-27 | 中南大学 | Aluminum oxide modified polymer electrolyte thin film and preparation method thereof |
| CN103904270A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103904272A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103904275A (en) * | 2012-12-28 | 2014-07-02 | 海洋王照明科技股份有限公司 | Electrochemical power source diaphragm and preparation method thereof, and electrochemical cell or capacitor |
| CN103972444A (en) * | 2013-01-28 | 2014-08-06 | 海洋王照明科技股份有限公司 | Electrochemical power supply separation membrane and preparation method thereof, electrochemical battery or capacitor |
| CN105552285A (en) * | 2015-12-30 | 2016-05-04 | 东莞漠泉新材料科技有限公司 | Ceramic coating diaphragm, preparation method thereof and application in lithium ion battery |
| CN107978780A (en) * | 2016-10-21 | 2018-05-01 | 中国科学院大连化学物理研究所 | The preparation and film and application of a kind of organic and inorganic Multi-layer composite proton exchange membrane |
| CN107978780B (en) * | 2016-10-21 | 2020-10-16 | 中国科学院大连化学物理研究所 | Preparation of organic-inorganic multilayer composite proton exchange membrane, membrane and application |
| CN108123155A (en) * | 2016-11-28 | 2018-06-05 | 中国科学院金属研究所 | A kind of preparation method of non-fluorine porous composite film used for all-vanadium redox flow battery |
| CN108134108A (en) * | 2016-12-01 | 2018-06-08 | 中国科学院大连化学物理研究所 | A kind of Kynoar-application of the hexafluoropropene diaphragm in flow battery |
| WO2019154275A1 (en) * | 2018-02-06 | 2019-08-15 | 比亚迪股份有限公司 | Polymer separator, preparation method therefor and use thereof, and lithium-ion battery and preparation method therefor |
| US11824225B2 (en) | 2018-02-06 | 2023-11-21 | Byd Company Limited | Separator including substrate, hydrophilic blocking layer, and polar polymer bonding with nodal structure, and method of preparing the same |
| CN110380022A (en) * | 2019-06-26 | 2019-10-25 | 荆门市格林美新材料有限公司 | A kind of high voltage monocrystalline nickel-cobalt-manganternary ternary anode material and preparation method |
| CN110380022B (en) * | 2019-06-26 | 2022-06-10 | 荆门市格林美新材料有限公司 | High-voltage single-crystal nickel-cobalt-manganese ternary positive electrode material and preparation method thereof |
| CN111697188A (en) * | 2020-06-23 | 2020-09-22 | 南京理工大学 | Lithium-sulfur battery interlayer with flame retardant property and preparation method thereof |
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Application publication date: 20101208 |