CN108400272A - A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil - Google Patents
A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil Download PDFInfo
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- CN108400272A CN108400272A CN201810177300.5A CN201810177300A CN108400272A CN 108400272 A CN108400272 A CN 108400272A CN 201810177300 A CN201810177300 A CN 201810177300A CN 108400272 A CN108400272 A CN 108400272A
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- China
- Prior art keywords
- kenyaite
- aerosil
- diaphragm
- micro mist
- lithium battery
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- Granted
Links
- 229910002012 Aerosil® Inorganic materials 0.000 title claims abstract description 78
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 46
- -1 polypropylene Polymers 0.000 title claims abstract description 46
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 45
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 27
- 239000003595 mist Substances 0.000 claims abstract description 56
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 239000012779 reinforcing material Substances 0.000 claims abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 56
- 239000007788 liquid Substances 0.000 claims description 48
- 238000006243 chemical reaction Methods 0.000 claims description 39
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 35
- 239000006185 dispersion Substances 0.000 claims description 31
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 15
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 claims description 15
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 14
- 239000011240 wet gel Substances 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 230000007062 hydrolysis Effects 0.000 claims description 10
- 238000006460 hydrolysis reaction Methods 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 9
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 239000003292 glue Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 7
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 2
- 229910003978 SiClx Inorganic materials 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 9
- 238000000576 coating method Methods 0.000 abstract description 9
- 239000012528 membrane Substances 0.000 abstract description 9
- 239000011159 matrix material Substances 0.000 abstract description 8
- 230000006870 function Effects 0.000 description 25
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 10
- 239000000377 silicon dioxide Substances 0.000 description 9
- 239000004575 stone Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 235000013339 cereals Nutrition 0.000 description 6
- 238000005660 chlorination reaction Methods 0.000 description 6
- 229910010272 inorganic material Inorganic materials 0.000 description 6
- 239000011147 inorganic material Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- JKMXKNVVELCAQT-UHFFFAOYSA-N O[Si][Na] Chemical compound O[Si][Na] JKMXKNVVELCAQT-UHFFFAOYSA-N 0.000 description 5
- 150000001336 alkenes Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical compound [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- JCCZVLHHCNQSNM-UHFFFAOYSA-N [Na][Si] Chemical compound [Na][Si] JCCZVLHHCNQSNM-UHFFFAOYSA-N 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000005213 imbibition Methods 0.000 description 3
- 239000002346 layers by function Substances 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- 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
- H01M50/431—Inorganic 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)
- Inorganic Chemistry (AREA)
- Cell Separators (AREA)
Abstract
The present invention relates to lithium battery diaphragm preparation fields, disclose a kind of lithium battery polypropylene diaphragm being compounded with kenyaite aerosil, the diaphragm is combined by membrane matrix polypropylene and reinforcing material kenyaite aerosil micro mist, and the quality accounting of the kenyaite aerosil micro mist is 1 10%.The lithium battery polypropylene diaphragm of the present invention can also make diaphragm have outstanding absorbency, thermal stability and anti-spine ability under the premise of being not provided with coating.
Description
Technical field
The present invention relates to field lithium battery diaphragm preparation fields more particularly to one kind being compounded with kenyaite-titanium dioxide
The lithium battery polypropylene diaphragm of silica aerogel.
Background technology
In lithium ion battery, the effect of diaphragm is isolation positive and negative pole material to prevent short circuit, and can to electrolyte into
The migration of row absorption, non-lithium ion provides facility.Therefore, diaphragm plays a key role the performance of lithium ion battery.
New energy has obtained significant progress in automobile industry at present, due to applying in automotive field, lithium ion power electricity
The safety in pond is increasingly important.But the electric current that the lithium ion battery of high-energy density is carried is larger, in battery work, overcharges
When, a large amount of heat is will produce, battery is easy to thermal runaway and causes combustion explosion.Diaphragm in the prior art is mainly polyene
Hydrocarbon material, heat resistanceheat resistant shrinkage is poor, be heated when be easy shrink or fusing, generate big cavity, cause positive and negative anodes contact and it is short
Road.In addition, lithium ion is easy the Li dendrite more sharp in positive and negative anodes Surface Creation in transition process repeatedly, being also easy will
Relatively thin diaphragm pierces through and causes short circuit.
For the above problem, current common practice the most is to coat one layer of inorganic material (as aoxidized on the surface of diaphragm
The inorganic ceramic materials such as silicon, zirconium oxide, aluminium oxide) coating, plays the role of improving diaphragm thermal stability and other physical properties.
Diaphragm thermal stability and other physical properties can be effectively improved really even so, but membrane surface coated is covered,
The porosity of coating is not high enough, and the imbibition rate of diaphragm is caused to be had a greatly reduced quality, and influences the migration of lithium ion, leads to the internal resistance liter of battery
Height, on the other hand, the later stage coating of coating are also easy to fall off in the later stage, to limit the performance of lithium ion battery.
Invention content
In order to solve the above technical problem, the present invention provides one kind being compounded with kenyaite-aerosil
Lithium battery polypropylene diaphragm, lithium battery polypropylene diaphragm of the invention under the premise of being not provided with coating remains to that diaphragm is made to have
There are outstanding absorbency, thermal stability and anti-spine ability.
The specific technical solution of the present invention is：A kind of lithium battery being compounded with kenyaite-aerosil is poly-
Propylene diaphragm is combined by membrane matrix polypropylene and reinforcing material kenyaite-aerosil micro mist, described
The quality accounting of kenyaite-aerosil micro mist is 1-10%.
It is typically in diaphragm table in the prior art for the physical properties such as the thermal stability for improving diaphragm and anti-spine ability
Face coats one layer of inorganic coating.Although diaphragm thermal stability and other physical properties so can be effectively improved really, every
Film surface coated is covered, and the porosity of coating is not high enough, and the imbibition rate of diaphragm is caused to be had a greatly reduced quality, and influences moving for lithium ion
Move, cause the internal resistance of battery to increase, on the other hand, the later stage coat coating be also easy to fall off in the later stage, to limit lithium from
The performance of sub- battery.
And in the present invention, it is by kenyaite-aerosil this special inorganic material in diaphragm material
Just carried out during material polypropylene synthesis it is compound, and during the biaxial stretching of diaphragm, since inorganic material is organic
Texture material is different, and in the effect of two-way drafting force, the inorganic material in polypropylene can move gradually to the nearly surface layer of diaphragm diaphragm
It moves and along the parallel integrated distribution of draw direction, is respectively formed two layers of organic/inorganic materials on the nearly surface layer in two surfaces of diaphragm and melts
The functional layer of conjunction.The effect for functioning as conventional membrane floating coat of the functional layer can play the thermostabilization for improving diaphragm
Property and the effect with anti-spine ability, but it combines together with diaphragm, it is not easily to fall off.Also, due to kenyaite-
Aerosil porosity is high, has larger specific surface area, can have preferable imbibition ability to electrolyte, be conducive to
The migration repeatedly of lithium ion, to solve above-mentioned technical problem in the prior art.
Preferably, the thickness of the diaphragm is 30-50 microns.
Preferably, the grain size of the kenyaite-aerosil micro mist is 0.1-5 microns.
Preferably, the preparation method of the diaphragm is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, it is micro- then to add kenyaite-aerosil
Powder, ultrasonic disperse are concentrated under reduced pressure, after vacuum drying, obtain the kenyaite-aerosil for being adsorbed with titanium trichloride
Micro mist.
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to respectively
In hexane, ultrasonic disperse obtains function modified liquid.
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization is polymerize respectively
Reaction is granulated after purified, dry, and function polypropylene agglomerate is made；Function polypropylene particles are biaxially drawn through melting
After stretching, diaphragm is made.
In step 1), the present invention utilizes the high porosity of kenyaite-aerosil micro mist, to tri-chlorination
Titanium is adsorbed, and then again mixes it with triethyl aluminum, and function modified liquid is made.Finally it polymerize with propylene monomer, with tradition
It is direct above-mentioned substance be subjected to the method that polymerize of mixing compare, the advantages of this method is that water hydroxyl silicon sodium can be utilized
The catalyst titanium trichloride of stone-aerosil micro mist adsorpting polymerization reaction, makes it fill out and is carried in the hole of aeroge,
Polymerisation is carried out again, and the locus of polymerization of propylene monomer is happened in hole, so that organic matter can fully intert entrance
The interlayer structure of kenyaite, increasing its interlamellar spacing, (kenyaite is layered crystal, but its interlamellar spacing is smaller, causes
Its dispersibility in organic system is bad, is specifically described as detailed below).The polypropylene being obtained by this method, inorganic material exist
Dispersibility in organic matrix more preferably is not easy to reunite.
Preferably, the matter of the kenyaite-aerosil micro mist, titanium trichloride, triethyl aluminum
Amount is than being 5-7:3-5:1-3.
Preferably, in step 3), polymeric reaction temperature is 75-85 DEG C, reaction pressure 2.8-3.2MPa, reaction
Time is 5-7h.
Preferably, the preparation method of the kenyaite-aerosil micro mist is as follows：
A) kenyaite is added in the ethyl orthosilicate of its 2-4 times of quality, is stirred evenly, add kenyaite
The absolute ethyl alcohol of 4-6 times of the water and kenyaite quality of 3-4 times of quality, ultrasonic disperse obtain dispersion liquid, by the pH of dispersion liquid
It is adjusted to faintly acid, makes it that reaction be hydrolyzed.
B hexamethyldisilazane) is added into the dispersion liquid after hydrolysis, and the pH of dispersion liquid is then adjusted to alkalescent, it is raw
At colloidal sol, aging is stood, after washing away unreacting substance with ethyl alcohol, compound wet gel is made.
C original solvent in wet gel) is displaced after vacuum dried, grinding, drying with n-hexane, and water hydroxyl silicon is made
Sodium stone-aerosil micro mist.
Kenyaite is layered crystal, can effectively promote the thermal stability and physics of material after compound with organic material
Performance.But its interlamellar spacing is smaller, causes its dispersibility in organic system bad, is easy to reunite.For this purpose, the present invention first will
Kenyaite is scattered in ethyl orthosilicate, and liquid ethyl orthosilicate is made to penetrate sufficiently into the stratiform of kenyaite
Between structure.Then silica dioxide gel is prepared using sol-gel method.In this process, ethyl orthosilicate is carried out in interlayer
Violent hydrolysis generates silicon dioxide colloid, adjacent layer structure is strutted, and increases interlamellar spacing.And in order into one
The stability for consolidating silicon dioxide colloid in interlayer is walked, the present invention also added hexamethyldisilazane, utilize its silazine link point
Abundant silicone hydroxyl carries out condensation reaction not and on kenyaite, silicon dioxide colloid, is bridged so that dioxide/silica gel
Body can firmly " support " between kenyaite lamella.It is solidifying that above-mentioned substance combination forms kenyaite-silica
Aeroge is made after removing solvent in glue.
Preferably, step A) in, the kenyaite passes through surface preparation：By weight, by 4-6 parts
Kenyaite is uniformly mixed with the sodium bicarbonate solution of 8-12 parts of a concentration of 10-20wt%, is heated to 60-70 DEG C of processing 1-
2h then takes out solid, and vacuum microwave radiates 1-3h, the kenyaite being surface-treated at 250-350 DEG C.
The present invention has carried out surface preparation to kenyaite, has technical effect that：
1, high temperature microwave radiation can remove the crystallization water of kenyaite interlayer, and Free up Memory is conducive to other substances
Penetrate into.
2, alkali process has been carried out to the surface of kenyaite, the chemical and physical dual of vacuum microwave radiation is surface-treated
Afterwards, the surface of kenyaite is corroded, and in the later stage by it with after polypropylene composite materials, polyacrylic molecule, atom are more prone to
It diffuses into inside kenyaite single layer structure, after long-time, has in previously described functional layer (after diaphragm is made in stretching)
Machine object gradually forms the interface phase fully merged with inorganic matter two-phase interface, since the fusion degree of the interface phase will be far superior to
The simple composite of conventional inorganics and organic matter, therefore its physical property also can be more outstanding.If by without above-mentioned processing
Kenyaite and polypropylene progress are compound, possibly can not form above-mentioned interface phase or form the time needs of interface phase more
Long.
Preferably, step A) in, the pH value of dispersion liquid is adjusted to 4-5, hydrolysis 1-2 days；Step B) in,
The pH of dispersion liquid is adjusted to 8-9, stands aging 1-2 days.
Preferably, step B) in, the quality of the hexamethyldisilazane is the 0.1- of kenyaite quality
0.3 times.
It is compared with the prior art, the beneficial effects of the invention are as follows：The lithium battery polypropylene diaphragm of the present invention is being not provided with painting
Under the premise of layer, it can also make diaphragm that there is outstanding absorbency, thermal stability and anti-spine ability.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil, by membrane matrix poly- third
Alkene and reinforcing material kenyaite-aerosil micro mist are combined, the kenyaite-silica airsetting
The quality accounting of glue micro mist is 5%.
Wherein, the preparation method of the kenyaite-aerosil micro mist is as follows：
A) by weight, 5 parts of kenyaites are uniformly mixed with the sodium bicarbonate solution of 10 parts of a concentration of 15wt%,
65 DEG C of processing 1.5h are heated to, then take out solid, vacuum microwave radiates 2h, the water hydroxyl silicon being surface-treated at 300 DEG C
Sodium stone.
The kenyaite of surface treatment is added in the ethyl orthosilicate of its 3 times of quality, is stirred evenly, adds water hydroxyl
The absolute ethyl alcohol of 5 times of the water and kenyaite quality of 3.5 times of silicon sodium stone quality, ultrasonic disperse obtains dispersion liquid, by dispersion liquid
PH be adjusted to 4.5, make its be hydrolyzed reaction 36h.
B the hexamethyldisilazane of 0.2 times of kenyaite quality) is added into the dispersion liquid after hydrolysis, then will be divided
The pH of dispersion liquid is adjusted to 8.5, generates colloidal sol, stands aging 36h, and after washing away unreacting substance with ethyl alcohol, compound wet gel is made.
C original solvent in wet gel) is displaced with n-hexane, after vacuum dried, grinding, drying, obtained grain size is
0.1-1 microns of kenyaite-aerosil micro mist.
The preparation method of the diaphragm is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, it is micro- then to add kenyaite-aerosil
Powder, ultrasonic disperse are concentrated under reduced pressure, after vacuum drying, obtain the kenyaite-aerosil for being adsorbed with titanium trichloride
Micro mist.
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to respectively
In hexane, ultrasonic disperse obtains function modified liquid.Wherein, the kenyaite-aerosil micro mist, tri-chlorination
Titanium, triethyl aluminum mass ratio be 6:4:2.
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization is polymerize respectively
Reaction, polymeric reaction temperature are 80 DEG C, reaction pressure 3.0MPa, reaction time 6h.After reaction after purifying, drying, into
Row is granulated, and function polypropylene agglomerate is made；By function polypropylene particles after melting biaxial stretching, it is 40 microns that thickness, which is made,
Diaphragm.
After tested, the porosity of diaphragm made from the present embodiment is 46%, air penetrability 33cm3/sec, and longitudinal stretching is strong
Degree is 152MPa, and transverse tensile strength 101MPa, it is 6.1N that needle, which pierces intensity,.
Embodiment 2
A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil, by membrane matrix poly- third
Alkene and reinforcing material kenyaite-aerosil micro mist are combined, the kenyaite-silica airsetting
The quality accounting of glue micro mist is 3%.
Wherein, the preparation method of the kenyaite-aerosil micro mist is as follows：
A) by weight, 4 parts of kenyaites are uniformly mixed with the sodium bicarbonate solution of 9 parts of a concentration of 15wt%,
65 DEG C of processing 2h are heated to, then take out solid, vacuum microwave radiates 2.5h, the water hydroxyl silicon being surface-treated at 280 DEG C
Sodium stone.
The kenyaite of surface treatment is added in the ethyl orthosilicate of its 2.5 times of quality, is stirred evenly, adds water
The absolute ethyl alcohol of 4.5 times of the water and kenyaite quality of 3 times of hydroxyl silicon sodium stone quality, ultrasonic disperse obtain dispersion liquid, will disperse
The pH of liquid is adjusted to 4, makes it that reaction 1 day be hydrolyzed.
B the hexamethyldisilazane of 0.23 times of kenyaite quality) is added into the dispersion liquid after hydrolysis, then will be divided
The pH of dispersion liquid is adjusted to 8, generates colloidal sol, stands aging 1 day, and after washing away unreacting substance with ethyl alcohol, compound wet gel is made.
C original solvent in wet gel) is displaced with n-hexane, after vacuum dried, grinding, drying, obtained grain size is
2-4 microns of kenyaite-aerosil micro mist.
The preparation method of the diaphragm is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, it is micro- then to add kenyaite-aerosil
Powder, ultrasonic disperse are concentrated under reduced pressure, after vacuum drying, obtain the kenyaite-aerosil for being adsorbed with titanium trichloride
Micro mist.
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to respectively
In hexane, ultrasonic disperse obtains function modified liquid.Wherein, the kenyaite-aerosil micro mist, tri-chlorination
Titanium, triethyl aluminum mass ratio be 5.5:3.5:1.5.
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization is polymerize respectively
Reaction, polymeric reaction temperature are 78 DEG C, reaction pressure 2.9MPa, reaction time 6h.After reaction after purifying, drying, into
Row is granulated, and function polypropylene agglomerate is made；By function polypropylene particles after melting biaxial stretching, it is 45 microns that thickness, which is made,
Diaphragm.
After tested, the porosity of diaphragm made from the present embodiment is 40%, air penetrability 29cm3/sec, and longitudinal stretching is strong
Degree is 160MPa, and transverse tensile strength 107MPa, it is 6.5N that needle, which pierces intensity,.
Embodiment 3
A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil, by membrane matrix poly- third
Alkene and reinforcing material kenyaite-aerosil micro mist are combined, the kenyaite-silica airsetting
The quality accounting of glue micro mist is 8%.
Wherein, the preparation method of the kenyaite-aerosil micro mist is as follows：
A) by weight, 5 parts of kenyaites are uniformly mixed with the sodium bicarbonate solution of 11 parts of a concentration of 10wt%,
60 DEG C of processing 2h are heated to, then take out solid, vacuum microwave radiates 2.5h, the water hydroxyl silicon being surface-treated at 320 DEG C
Sodium stone.
The kenyaite of surface treatment is added in the ethyl orthosilicate of its 3.5 times of quality, is stirred evenly, adds water
The absolute ethyl alcohol of 5 times of the water and kenyaite quality of 4 times of hydroxyl silicon sodium stone quality, ultrasonic disperse obtains dispersion liquid, by dispersion liquid
PH be adjusted to 5, make its be hydrolyzed reaction 2 days.
B the hexamethyldisilazane of 0.2 times of kenyaite quality) is added into the dispersion liquid after hydrolysis, then will be divided
The pH of dispersion liquid is adjusted to 9, generates colloidal sol, stands aging 2 days, and after washing away unreacting substance with ethyl alcohol, compound wet gel is made.
C original solvent in wet gel) is displaced with n-hexane, after vacuum dried, grinding, drying, obtained grain size is
1-3 microns of kenyaite-aerosil micro mist.
The preparation method of the diaphragm is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, it is micro- then to add kenyaite-aerosil
Powder, ultrasonic disperse are concentrated under reduced pressure, after vacuum drying, obtain the kenyaite-aerosil for being adsorbed with titanium trichloride
Micro mist.
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to respectively
In hexane, ultrasonic disperse obtains function modified liquid.Wherein, the kenyaite-aerosil micro mist, tri-chlorination
Titanium, triethyl aluminum mass ratio be 6:3.5:1.5.
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization is polymerize respectively
Reaction, polymeric reaction temperature are 82 DEG C, reaction pressure 3.1MPa, reaction time 5.5h.After reaction after purifying, drying,
It is granulated, function polypropylene agglomerate is made；By function polypropylene particles after melting biaxial stretching, it is 35 micro- that thickness, which is made,
The diaphragm of rice.
After tested, the porosity of diaphragm made from the present embodiment is 42%, air penetrability 32cm3/sec, and longitudinal stretching is strong
Degree is 158MPa, and transverse tensile strength 103MPa, it is 6.3N that needle, which pierces intensity,.
Embodiment 4
A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil, by membrane matrix poly- third
Alkene and reinforcing material kenyaite-aerosil micro mist are combined, the kenyaite-silica airsetting
The quality accounting of glue micro mist is 1%.
Wherein, the preparation method of the kenyaite-aerosil micro mist is as follows：
A) by weight, 4 parts of kenyaites are uniformly mixed with the sodium bicarbonate solution of 8 parts of a concentration of 20wt%,
60 DEG C of processing 2h are heated to, then take out solid, vacuum microwave radiates 3h, the water hydroxyl silicon sodium being surface-treated at 250 DEG C
Stone.
The kenyaite of surface treatment is added in the ethyl orthosilicate of its 2 times of quality, is stirred evenly, adds water hydroxyl
The absolute ethyl alcohol of 4 times of the water and kenyaite quality of 3 times of silicon sodium stone quality, ultrasonic disperse obtains dispersion liquid, by dispersion liquid
PH is adjusted to 4, makes it that reaction 1 day be hydrolyzed.
B the hexamethyldisilazane of 0.1 times of kenyaite quality) is added into the dispersion liquid after hydrolysis, then will be divided
The pH of dispersion liquid is adjusted to 8, generates colloidal sol, stands aging 1 day, and after washing away unreacting substance with ethyl alcohol, compound wet gel is made.
C original solvent in wet gel) is displaced with n-hexane, after vacuum dried, grinding, drying, obtained grain size is
0.1-1 microns of kenyaite-aerosil micro mist.
The preparation method of the diaphragm is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, it is micro- then to add kenyaite-aerosil
Powder, ultrasonic disperse are concentrated under reduced pressure, after vacuum drying, obtain the kenyaite-aerosil for being adsorbed with titanium trichloride
Micro mist.
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to respectively
In hexane, ultrasonic disperse obtains function modified liquid.Wherein, the kenyaite-aerosil micro mist, tri-chlorination
Titanium, triethyl aluminum mass ratio be 5:3:1.
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization is polymerize respectively
Reaction, polymeric reaction temperature are 75 DEG C, reaction pressure 2.8MPa, reaction time 7h.After reaction after purifying, drying, into
Row is granulated, and function polypropylene agglomerate is made；By function polypropylene particles after melting biaxial stretching, it is 30 microns that thickness, which is made,
Diaphragm.
After tested, the porosity of diaphragm made from the present embodiment is 53%, air penetrability 39cm3/sec, and longitudinal stretching is strong
Degree is 131MPa, and transverse tensile strength 85MPa, it is 5.6N that needle, which pierces intensity,.
Embodiment 5
A kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil, by membrane matrix poly- third
Alkene and reinforcing material kenyaite-aerosil micro mist are combined, the kenyaite-silica airsetting
The quality accounting of glue micro mist is 10%.
Wherein, the preparation method of the kenyaite-aerosil micro mist is as follows：
A) by weight, 6 parts of kenyaites are uniformly mixed with the sodium bicarbonate solution of 12 parts of a concentration of 10wt%,
70 DEG C of processing 1h are heated to, then take out solid, vacuum microwave radiates 1h, the water hydroxyl silicon sodium being surface-treated at 350 DEG C
Stone.
The kenyaite of surface treatment is added in the ethyl orthosilicate of its 4 times of quality, is stirred evenly, adds water hydroxyl
The absolute ethyl alcohol of 6 times of the water and kenyaite quality of 4 times of silicon sodium stone quality, ultrasonic disperse obtains dispersion liquid, by dispersion liquid
PH is adjusted to 5, makes it that reaction 2 days be hydrolyzed.
B the hexamethyldisilazane of 0.3 times of kenyaite quality) is added into the dispersion liquid after hydrolysis, then will be divided
The pH of dispersion liquid is adjusted to 9, generates colloidal sol, stands aging 2 days, and after washing away unreacting substance with ethyl alcohol, compound wet gel is made.
C original solvent in wet gel) is displaced with n-hexane, after vacuum dried, grinding, drying, obtained grain size is
3-5 microns of kenyaite-aerosil micro mist.
The preparation method of the diaphragm is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, it is micro- then to add kenyaite-aerosil
Powder, ultrasonic disperse are concentrated under reduced pressure, after vacuum drying, obtain the kenyaite-aerosil for being adsorbed with titanium trichloride
Micro mist.
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to respectively
In hexane, ultrasonic disperse obtains function modified liquid.Wherein, the kenyaite-aerosil micro mist, tri-chlorination
Titanium, triethyl aluminum mass ratio be 7:5:3.
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization is polymerize respectively
Reaction, polymeric reaction temperature are 85 DEG C, reaction pressure 3.2MPa, reaction time 5h.After reaction after purifying, drying, into
Row is granulated, and function polypropylene agglomerate is made；By function polypropylene particles after melting biaxial stretching, it is 50 microns that thickness, which is made,
Diaphragm.
After tested, the porosity of diaphragm made from the present embodiment is 36%, air penetrability 26cm3/sec, and longitudinal stretching is strong
Degree is 171MPa, and transverse tensile strength 111MPa, it is 6.8N that needle, which pierces intensity,.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention
Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not imposed any restrictions to the present invention, every according to the present invention
Technical spirit still falls within the technology of the present invention side to any simple modification, change and equivalent transformation made by above example
The protection domain of case.
Claims (10)
1. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil, it is characterised in that：By diaphragm
Base-material polypropylene and reinforcing material kenyaite-aerosil micro mist are combined, the kenyaite-dioxy
The quality accounting of SiClx aeroge micro mist is 1-10%.
2. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil as described in claim 1,
It is characterized in that, the thickness of the diaphragm is 30-50 microns.
3. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil as described in claim 1,
It is characterized in that, the grain size of the kenyaite-aerosil micro mist is 0.1-5 microns.
4. a kind of lithium battery polypropylene being compounded with kenyaite-aerosil as claimed in claim 1 or 2 every
Film, it is characterised in that preparation method is as follows：
1) titanium trichloride is dissolved in ethyl alcohol, is stirred evenly, then add kenyaite-aerosil micro mist, surpassed
Sound disperses, and is concentrated under reduced pressure, after vacuum drying, obtains the kenyaite-aerosil micro mist for being adsorbed with titanium trichloride；
2) kenyaite for being adsorbed with titanium trichloride-aerosil micro mist and triethyl aluminum are added to hexane respectively
In, ultrasonic disperse obtains function modified liquid；
3) propylene and function modified liquid are added to using hexane as in the reaction kettle of solvent, heating pressurization polymerize anti-respectively
It answers, after purified, dry, is granulated, function polypropylene agglomerate is made；By function polypropylene particles through melting biaxial stretching
Afterwards, diaphragm is made.
5. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil as claimed in claim 4,
It is characterized in that, the mass ratio of the kenyaite-aerosil micro mist, titanium trichloride, triethyl aluminum is 5-7:
3-5:1-3。
6. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil as claimed in claim 4,
It is characterized in that, in step 3), polymeric reaction temperature is 75-85 DEG C, reaction pressure 2.8-3.2MPa, reaction time 5-
7h。
7. a kind of lithium battery polypropylene being compounded with kenyaite-aerosil as described in claim 1 or 3 every
Film, which is characterized in that the preparation method of the kenyaite-aerosil micro mist is as follows：
A) kenyaite is added in the ethyl orthosilicate of its 2-4 times of quality, is stirred evenly, add kenyaite quality
The absolute ethyl alcohol of 3-4 times of 4-6 times of water and kenyaite quality, ultrasonic disperse obtain dispersion liquid, and the pH of dispersion liquid is adjusted to
Faintly acid makes it that reaction be hydrolyzed；
B hexamethyldisilazane) is added into the dispersion liquid after hydrolysis, the pH of dispersion liquid is then adjusted to alkalescent, is generated molten
Glue stands aging, and after washing away unreacting substance with ethyl alcohol, compound wet gel is made；
C original solvent in wet gel) is displaced after vacuum dried, grinding, drying with n-hexane, and kenyaite-is made
Aerosil micro mist.
8. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil as claimed in claim 7,
It is characterized in that, step A) in, the kenyaite passes through surface preparation：By weight, by 4-6 parts of kenyaites
It is uniformly mixed with the sodium bicarbonate solution of 8-12 parts of a concentration of 10-20wt%, is heated to 60-70 DEG C of processing 1-2h, then takes out
Solid, vacuum microwave radiates 1-3h, the kenyaite being surface-treated at 250-350 DEG C.
9. a kind of lithium battery polypropylene diaphragm being compounded with kenyaite-aerosil as claimed in claim 7,
It is characterized in that, step A) in, the pH value of dispersion liquid is adjusted to 4-5, hydrolysis 1-2 days；Step B) in, by dispersion liquid
PH is adjusted to 8-9, stands aging 1-2 days.
10. a kind of lithium battery polypropylene being compounded with kenyaite-aerosil as claimed in claim 7 every
Film, which is characterized in that step B) in, the quality of the hexamethyldisilazane is 0.1-0.3 times of kenyaite quality.
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| CN201810177300.5A CN108400272B (en) | 2018-03-05 | 2018-03-05 | Lithium battery polypropylene diaphragm compounded with kenyaite-silicon dioxide aerogel |
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| CN109254468A (en) * | 2018-11-09 | 2019-01-22 | 广东彩乐智能包装科技有限公司 | Have both electrochromism and the flexible device of electroluminescent function and preparation method thereof |
| CN111430782A (en) * | 2020-05-08 | 2020-07-17 | 曹亚琼 | A kind of silicon aerogel modified lithium ion battery separator and preparation method |
| CN111430783A (en) * | 2020-05-08 | 2020-07-17 | 曹亚琼 | Lithium ion battery diaphragm |
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Effective date of registration: 20240426 Address after: 413000, formerly Ping'an Mixing Plant, S317, Lengshi Community, Lengshi Town, Anhua County, Yiyang City, Hunan Province Patentee after: Hunan Guoyang Industrial Technology Co.,Ltd. Country or region after: China Address before: 322100 Room 302, unit 2, building 1, Siji District 5, Beiyuan street, Yiwu City, Jinhua City, Zhejiang Province Patentee before: Yiwu kunyue Toys Co.,Ltd. Country or region before: China |
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