CN105206776A - Preparation method of modified sodium polyacrylate doped aluminum oxide diaphragm for lithium battery - Google Patents
Preparation method of modified sodium polyacrylate doped aluminum oxide diaphragm for lithium battery Download PDFInfo
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- CN105206776A CN105206776A CN201510676321.8A CN201510676321A CN105206776A CN 105206776 A CN105206776 A CN 105206776A CN 201510676321 A CN201510676321 A CN 201510676321A CN 105206776 A CN105206776 A CN 105206776A
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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
- 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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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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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Abstract
The invention discloses a preparation method of a modified sodium polyacrylate doped aluminum oxide diaphragm for a lithium battery, and belongs to the field of lithium battery diaphragm preparation. The preparation method comprises the following steps: sufficiently dissolving sodium polyacrylate in water to obtain a solution; adding diethylene triamine polyethylene glycol into the solution to obtain a mixture; adding sodium peroxide into the mixture for an exothermic reaction, so that micropores are formed in the surface of the mixture; adding aluminum oxide and magnesium oxide under the condition of stirring, so that aluminum oxide and magnesium oxide can are uniformly doped; carrying out extrusion and pelletization, inflation, reeling, irradiation, flushing and drying to obtain the diaphragm. The preparation method has the benefits that the service life of the diaphragm is prolonged by 50-60%; when in use, the diaphragm can better protect a lithium battery which is subjected to an internal short circuit, can provide sufficient safety for a lithium battery which is overcharged, is relatively high in mechanical property and thermal stability, and high in safety, thermal shrinkage, affinity for an electrolyte, hydrophility, and electrolyte solution impregnation property.
Description
Technical field
The present invention relates to a kind of preparation method of lithium battery modified polyacrylate sodium doped aluminium barrier film, belong to lithium battery diaphragm preparation field.
Background technology
Lithium ion battery has the characteristic of high-energy-density, long circulation life, memory-less effect, and have again safety, reliable and can the advantage such as fast charging and discharging, lithium ion battery forms primarily of positive and negative electrode material, electrolyte and barrier film.Between lithium ion cell positive and negative pole, have a membrane material, be commonly referred to barrier film, it is the important component part of lithium ion battery.The Main Function of barrier film is isolation positive and negative electrode and the electronics in battery can not be passed freely through, and ion can be allowed freely to pass through between both positive and negative polarity.Lithium battery diaphragm is in the structure of lithium battery, and barrier film is one of interior layer assembly of key.For lithium battery series, because electrolyte is organic solvent system, thus need the diaphragm material of organic solvent-resistant.Because polyethene microporous membrane has the retention of higher porosity, lower resistance, preferably tearing toughness, good antiacid alkali ability, good elasticity and aprotic solvent, therefore Study on Li-ion batteries initial stage of development is just adopted and is used it as its diaphragm material.At present, lithium ion battery separator material mainly still adopts polyethene microporous membrane.But adopt high density polyethylene (HDPE) as lithium battery diaphragm raw material, the melt temperature of barrier film is lower, and when temperature rises to its softening temperature and melt temperature, thermal contraction and fusing will occur barrier film.For improving the heat-shrinkable of barrier film and promoting thermal safety energy, what adopt at present is at the heat-resisting group of film surface grafting, interpolation refractory coating, thin-film material cross-linked modification method, causes its production cost to increase.Barrier film hydrophilicity is poor, cause the electrolyte wetting property of barrier film poor thus, polyethylene shows rudimentary property and hydrophobicity due to its molecular structure property of polyethylene, poor to electrolytical compatibility, improve diaphragm electrolyte wettability, be conducive to the ionic conductivity and the charge-discharge performance that promote lithium ion battery.
Summary of the invention
Technical problem to be solved by this invention: for high density polyethylene (HDPE) as lithium battery diaphragm raw material, the melt temperature of barrier film is lower, when temperature rises to its softening temperature and melt temperature, thermal contraction and fusing will be there is in barrier film, and show rudimentary property and hydrophobicity due to its molecular structure property of polyethylene, poor to electrolytical compatibility, cause the easy short circuit of battery, poor safety performance, barrier film hydrophilicity is poor, the drawback of electrolyte wetting property difference, provide a kind of preparation method of lithium battery modified polyacrylate sodium doped aluminium barrier film, the present invention gets Sodium Polyacrylate and water fully dissolves, add sodium peroxide reaction and generate NaOH releasing heat, accelerate dissolution, absorb moisture, mixture moisture content is reduced, there is bubble to emerge simultaneously, uniform micropore is formed on its surface, then in whipping process, aluminium oxide is added, magnesium oxide, Uniform Doped wherein obtains.Preparation method of the present invention is simple, and products obtained therefrom security performance is high, and thermal contraction performance is good, better to electrolytical compatibility, barrier film hydrophilicity and electrolyte wetting property good, be worthy to be popularized and use.
For solving the problems of the technologies described above, the present invention adopts technical scheme as described below to be:
(1) take 3 ~ 5g Sodium Polyacrylate powder, be placed in rectangular vessel, add the water of 300 ~ 500mL in container, control temperature is 75 ~ 85 DEG C, and rotating speed is 700 ~ 900r/min, and mix and blend 30 ~ 50min makes it fully dissolve;
(2) after it fully dissolves, to add weight fraction be wherein 0.1 ~ 0.5% diethylenetriamines crosslinking agent and weight fraction is 0.2 ~ 0.4% polyethylene glycol dispersant, and be warming up to 90 ~ 110 DEG C, control rotating speed is 1000 ~ 1500r/min, magnetic agitation 40 ~ 50min, obtains mixture;
(3) improving rotating speed is 1600 ~ 2000r/min, adds 1 ~ 2g sodium peroxide powder while stirring in said mixture, and added rear stopping and having stirred, constant temperature keeps 30 ~ 40min, makes mixture surface form uniform micropore;
(4) keep after 30 ~ 40min until constant temperature, add 2 ~ 3g aluminium oxide and 1 ~ 3g magnesium oxide respectively in mixture, and 100 ~ 120mL ethanol solution is added in mixture, 1000 ~ 1200r/min rotating speed lower magnetic force stir 40 ~ 60min, to be mixed complete after, pour in thermal response still, set temperature is 160 ~ 180 DEG C, reaction 12 ~ 14h, makes its Uniform Doped wherein, obtains colloid mixture;
(5) colloid mixture of above-mentioned gained is put into double screw extruder and carry out extruding pelletization, obtain the polyacrylic resin particle after blending and modifying, modified polyacrylic resin particle is added in hopper, again from die head die orifice out, through vane cooling, inflation, batching by surely steeping frame collapser carry-over pinch rolls, obtaining Sodium Polyacrylate film;
(6) the Sodium Polyacrylate film of above-mentioned preparation is placed in irradiation bottle, after vacuumizing, then passes into argon gas to it, the above-mentioned airtight irradiation bottle being full of argon gas is placed in room, gamma-ray irradiation source and carries out irradiation, exposure time is 20 ~ 30min;
(7) to be irradiated complete after, take out and put into deionized water and carry out flushing 3 ~ 5 times, after removing surperficial homopolymers, dry 3 ~ 5h, namely obtains a kind of lithium battery modified polyacrylate sodium doped aluminium barrier film under vacuo.
Application process of the present invention: the lithium battery diaphragm prepared is placed between positive pole and negative pole; extend original 50 ~ 60% in useful life of barrier film; better protection can be provided when internal short-circuit after using; sufficient fail safe can be provided when overcharging; there are good mechanical property and thermal stability; barrier film security performance is high, and thermal contraction performance is good, good to electrolyte compatibility.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the lithium battery diaphragm security performance for preparing of the method is high, and thermal contraction performance is good, better to electrolytical compatibility, barrier film hydrophilicity and electrolyte wetting property good;
(2) preparation method of the present invention is simple, can provide better protection after using when internal short-circuit, can provide sufficient fail safe, have good mechanical property and thermal stability when overcharging.
Embodiment
First take 3 ~ 5g Sodium Polyacrylate powder, be placed in rectangular vessel, add the water of 300 ~ 500mL in container, control temperature is 75 ~ 85 DEG C, and rotating speed is 700 ~ 900r/min, and mix and blend 30 ~ 50min makes it fully dissolve; After it fully dissolves, to add weight fraction be wherein 0.1 ~ 0.5% diethylenetriamines crosslinking agent and weight fraction is 0.2 ~ 0.4% polyethylene glycol dispersant, and be warming up to 90 ~ 110 DEG C, control rotating speed is 1000 ~ 1500r/min, magnetic agitation 40 ~ 50min, obtains mixture; Improving rotating speed is subsequently 1600 ~ 2000r/min, adds 1 ~ 2g sodium peroxide powder while stirring in said mixture, and added rear stopping and having stirred, constant temperature keeps 30 ~ 40min, makes mixture surface form uniform micropore; Keep after 30 ~ 40min until constant temperature, add 2 ~ 3g aluminium oxide and 1 ~ 3g magnesium oxide respectively in mixture, and 100 ~ 120mL ethanol solution is added in mixture, 1000 ~ 1200r/min rotating speed lower magnetic force stir 40 ~ 60min, to be mixed complete after, pour in thermal response still, set temperature is 160 ~ 180 DEG C, reaction 12 ~ 14h, makes its Uniform Doped wherein, obtains colloid mixture; Then the colloid mixture of above-mentioned gained is put into double screw extruder and carry out extruding pelletization, obtain the polyacrylic resin particle after blending and modifying, modified polyacrylic resin particle is added in hopper, again from die head die orifice out, through vane cooling, inflation, batching by surely steeping frame collapser carry-over pinch rolls, obtaining Sodium Polyacrylate film; Again the Sodium Polyacrylate film of above-mentioned preparation is placed in irradiation bottle, after vacuumizing, then passes into argon gas to it, the above-mentioned airtight irradiation bottle being full of argon gas is placed in room, gamma-ray irradiation source and carries out irradiation, exposure time is 20 ~ 30min; Finally to be irradiated complete after, take out and put into deionized water and carry out flushing 3 ~ 5 times, after removing surperficial homopolymers, dry 3 ~ 5h, namely obtains a kind of lithium battery modified polyacrylate sodium doped aluminium barrier film under vacuo.
Example 1
First take 3g Sodium Polyacrylate powder, be placed in rectangular vessel, add the water of 300mL in container, control temperature is 75 DEG C, and rotating speed is 700r/min, and mix and blend 30min makes it fully dissolve; After it fully dissolves, to add weight fraction be wherein 0.1% diethylenetriamines crosslinking agent and weight fraction is 0.2% polyethylene glycol dispersant, and be warming up to 90 DEG C, control rotating speed is 1000r/min, magnetic agitation 40min, obtains mixture; Improving rotating speed is subsequently 1600r/min, adds 1g sodium peroxide powder while stirring in said mixture, and added rear stopping and having stirred, constant temperature keeps 30min, makes mixture surface form uniform micropore; Keep after 30min until constant temperature, add 2g aluminium oxide and 1g magnesium oxide respectively in mixture, and 100mL ethanol solution is added in mixture, 1000r/min rotating speed lower magnetic force stir 40min, to be mixed complete after, pour in thermal response still, set temperature is 160 DEG C, reaction 12h, makes its Uniform Doped wherein, obtains colloid mixture; Then the colloid mixture of above-mentioned gained is put into double screw extruder and carry out extruding pelletization, obtain the polyacrylic resin particle after blending and modifying, modified polyacrylic resin particle is added in hopper, again from die head die orifice out, through vane cooling, inflation, batching by surely steeping frame collapser carry-over pinch rolls, obtaining Sodium Polyacrylate film; Again the Sodium Polyacrylate film of above-mentioned preparation is placed in irradiation bottle, after vacuumizing, then passes into argon gas to it, the above-mentioned airtight irradiation bottle being full of argon gas is placed in room, gamma-ray irradiation source and carries out irradiation, exposure time is 20min; Finally to be irradiated complete after, take out and put into deionized water and carry out flushing 3 times, after removing surperficial homopolymers, dry 3h under vacuo, namely obtains a kind of lithium battery modified polyacrylate sodium doped aluminium barrier film.
The lithium battery diaphragm prepared is placed between positive pole and negative pole; extend original 50% in useful life of barrier film; better protection can be provided when internal short-circuit after using; sufficient fail safe can be provided when overcharging; there are good mechanical property and thermal stability; barrier film security performance is high, and thermal contraction performance is good, good to electrolyte compatibility.
Example 2
First take 4g Sodium Polyacrylate powder, be placed in rectangular vessel, add the water of 400mL in container, control temperature is 80 DEG C, and rotating speed is 800r/min, and mix and blend 40min makes it fully dissolve; After it fully dissolves, to add weight fraction be wherein 0.3% diethylenetriamines crosslinking agent and weight fraction is 0.3% polyethylene glycol dispersant, and be warming up to 100 DEG C, control rotating speed is 1250r/min, magnetic agitation 45min, obtains mixture; Improving rotating speed is subsequently 1800r/min, adds 1.5g sodium peroxide powder while stirring in said mixture, and added rear stopping and having stirred, constant temperature keeps 35min, makes mixture surface form uniform micropore; Keep after 35min until constant temperature, add 2.5g aluminium oxide and 2g magnesium oxide respectively in mixture, and 110mL ethanol solution is added in mixture, 1100r/min rotating speed lower magnetic force stir 50min, to be mixed complete after, pour in thermal response still, set temperature is 170 DEG C, reaction 13h, makes its Uniform Doped wherein, obtains colloid mixture; Then the colloid mixture of above-mentioned gained is put into double screw extruder and carry out extruding pelletization, obtain the polyacrylic resin particle after blending and modifying, modified polyacrylic resin particle is added in hopper, again from die head die orifice out, through vane cooling, inflation, batching by surely steeping frame collapser carry-over pinch rolls, obtaining Sodium Polyacrylate film; Again the Sodium Polyacrylate film of above-mentioned preparation is placed in irradiation bottle, after vacuumizing, then passes into argon gas to it, the above-mentioned airtight irradiation bottle being full of argon gas is placed in room, gamma-ray irradiation source and carries out irradiation, exposure time is 25min; Finally to be irradiated complete after, take out and put into deionized water and carry out flushing 4 times, after removing surperficial homopolymers, dry 4h under vacuo, namely obtains a kind of lithium battery modified polyacrylate sodium doped aluminium barrier film.
The lithium battery diaphragm prepared is placed between positive pole and negative pole; extend original 55% in useful life of barrier film; better protection can be provided when internal short-circuit after using; sufficient fail safe can be provided when overcharging; there are good mechanical property and thermal stability; barrier film security performance is high, and thermal contraction performance is good, good to electrolyte compatibility.
Example 3
First take 5g Sodium Polyacrylate powder, be placed in rectangular vessel, add the water of 500mL in container, control temperature is 85 DEG C, and rotating speed is 900r/min, and mix and blend 50min makes it fully dissolve; After it fully dissolves, to add weight fraction be wherein 0.5% diethylenetriamines crosslinking agent and weight fraction is 0.4% polyethylene glycol dispersant, and be warming up to 110 DEG C, control rotating speed is 1500r/min, magnetic agitation 50min, obtains mixture; Improving rotating speed is subsequently 2000r/min, adds 2g sodium peroxide powder while stirring in said mixture, and added rear stopping and having stirred, constant temperature keeps 40min, makes mixture surface form uniform micropore; Keep after 40min until constant temperature, add 3g aluminium oxide and 3g magnesium oxide respectively in mixture, and 120mL ethanol solution is added in mixture, 1200r/min rotating speed lower magnetic force stir 60min, to be mixed complete after, pour in thermal response still, set temperature is 180 DEG C, reaction 14h, makes its Uniform Doped wherein, obtains colloid mixture; Then the colloid mixture of above-mentioned gained is put into double screw extruder and carry out extruding pelletization, obtain the polyacrylic resin particle after blending and modifying, modified polyacrylic resin particle is added in hopper, again from die head die orifice out, through vane cooling, inflation, batching by surely steeping frame collapser carry-over pinch rolls, obtaining Sodium Polyacrylate film; Again the Sodium Polyacrylate film of above-mentioned preparation is placed in irradiation bottle, after vacuumizing, then passes into argon gas to it, the above-mentioned airtight irradiation bottle being full of argon gas is placed in room, gamma-ray irradiation source and carries out irradiation, exposure time is 30min; Finally to be irradiated complete after, take out and put into deionized water and carry out flushing 5 times, after removing surperficial homopolymers, dry 5h under vacuo, namely obtains a kind of lithium battery modified polyacrylate sodium doped aluminium barrier film.
The lithium battery diaphragm prepared is placed between positive pole and negative pole; extend original 60% in useful life of barrier film; better protection can be provided when internal short-circuit after using; sufficient fail safe can be provided when overcharging; there are good mechanical property and thermal stability; barrier film security performance is high, and thermal contraction performance is good, good to electrolyte compatibility.
Claims (1)
1. a lithium battery preparation method for modified polyacrylate sodium doped aluminium barrier film, is characterized in that concrete preparation process is:
(1) take 3 ~ 5g Sodium Polyacrylate powder, be placed in rectangular vessel, add the water of 300 ~ 500mL in container, control temperature is 75 ~ 85 DEG C, and rotating speed is 700 ~ 900r/min, and mix and blend 30 ~ 50min makes it fully dissolve;
(2) after it fully dissolves, to add weight fraction be wherein 0.1 ~ 0.5% diethylenetriamines crosslinking agent and weight fraction is 0.2 ~ 0.4% polyethylene glycol dispersant, and be warming up to 90 ~ 110 DEG C, control rotating speed is 1000 ~ 1500r/min, magnetic agitation 40 ~ 50min, obtains mixture;
(3) improving rotating speed is 1600 ~ 2000r/min, adds 1 ~ 2g sodium peroxide powder while stirring in said mixture, and added rear stopping and having stirred, constant temperature keeps 30 ~ 40min, makes mixture surface form uniform micropore;
(4) keep after 30 ~ 40min until constant temperature, add 2 ~ 3g aluminium oxide and 1 ~ 3g magnesium oxide respectively in mixture, and 100 ~ 120mL ethanol solution is added in mixture, 1000 ~ 1200r/min rotating speed lower magnetic force stir 40 ~ 60min, to be mixed complete after, pour in thermal response still, set temperature is 160 ~ 180 DEG C, reaction 12 ~ 14h, makes its Uniform Doped wherein, obtains colloid mixture;
(5) colloid mixture of above-mentioned gained is put into double screw extruder and carry out extruding pelletization, obtain the polyacrylic resin particle after blending and modifying, modified polyacrylic resin particle is added in hopper, again from die head die orifice out, through vane cooling, inflation, batching by surely steeping frame collapser carry-over pinch rolls, obtaining Sodium Polyacrylate film;
(6) the Sodium Polyacrylate film of above-mentioned preparation is placed in irradiation bottle, after vacuumizing, then passes into argon gas to it, the above-mentioned airtight irradiation bottle being full of argon gas is placed in room, gamma-ray irradiation source and carries out irradiation, exposure time is 20 ~ 30min;
(7) to be irradiated complete after, take out and put into deionized water and carry out flushing 3 ~ 5 times, after removing surperficial homopolymers, dry 3 ~ 5h, namely obtains a kind of lithium battery modified polyacrylate sodium doped aluminium barrier film under vacuo.
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| CN201510676321.8A CN105206776A (en) | 2015-10-19 | 2015-10-19 | Preparation method of modified sodium polyacrylate doped aluminum oxide diaphragm for lithium battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109638204A (en) * | 2018-12-17 | 2019-04-16 | 吉林大学 | A kind of high-intensitive, compound lithium battery diaphragm and preparation method thereof |
| CN112909430A (en) * | 2019-12-03 | 2021-06-04 | 恒大新能源技术(深圳)有限公司 | Lithium ion battery diaphragm and preparation method thereof and lithium ion battery |
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| CN101931085A (en) * | 2009-06-22 | 2010-12-29 | 宁波大学 | Preparation method for fuel cell compound proton exchange membrane enhanced by using SiO2 three-dimensional ultra-thin membrane |
| CN103920398A (en) * | 2014-04-25 | 2014-07-16 | 天津工业大学 | Hollow fiber membrane and preparation method thereof |
| CN104037379A (en) * | 2014-06-06 | 2014-09-10 | 中国第一汽车股份有限公司 | Composite polymer fiber diaphragm and preparation method thereof |
| CN104910489A (en) * | 2015-06-13 | 2015-09-16 | 常州大学 | High-density polyethylene microporous membrane with molecular sieve function |
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2015
- 2015-10-19 CN CN201510676321.8A patent/CN105206776A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5371227A (en) * | 1976-12-07 | 1978-06-24 | Seiko Instr & Electronics | Method of manufacturing separator for alkaline battery |
| CN1329638A (en) * | 1998-12-08 | 2002-01-02 | Lg化学株式会社 | Separator for secondary battery and porous film made of polyolefin blend and process for preparing the same |
| CN101931085A (en) * | 2009-06-22 | 2010-12-29 | 宁波大学 | Preparation method for fuel cell compound proton exchange membrane enhanced by using SiO2 three-dimensional ultra-thin membrane |
| CN103920398A (en) * | 2014-04-25 | 2014-07-16 | 天津工业大学 | Hollow fiber membrane and preparation method thereof |
| CN104037379A (en) * | 2014-06-06 | 2014-09-10 | 中国第一汽车股份有限公司 | Composite polymer fiber diaphragm and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109638204A (en) * | 2018-12-17 | 2019-04-16 | 吉林大学 | A kind of high-intensitive, compound lithium battery diaphragm and preparation method thereof |
| CN112909430A (en) * | 2019-12-03 | 2021-06-04 | 恒大新能源技术(深圳)有限公司 | Lithium ion battery diaphragm and preparation method thereof and lithium ion battery |
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Application publication date: 20151230 |