CN114316450A - Thermal protection material for lithium ion battery and preparation method thereof - Google Patents
Thermal protection material for lithium ion battery and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 90
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 143
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 83
- 238000004073 vulcanization Methods 0.000 claims abstract description 46
- 150000002978 peroxides Chemical class 0.000 claims abstract description 42
- 229920002943 EPDM rubber Polymers 0.000 claims abstract description 41
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 41
- 239000000945 filler Substances 0.000 claims abstract description 34
- 229910052582 BN Inorganic materials 0.000 claims abstract description 33
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000006229 carbon black Substances 0.000 claims abstract description 32
- 239000002105 nanoparticle Substances 0.000 claims abstract description 31
- 239000004965 Silica aerogel Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 229910052573 porcelain Inorganic materials 0.000 claims abstract description 24
- 238000007723 die pressing method Methods 0.000 claims abstract description 23
- 229920001971 elastomer Polymers 0.000 claims description 44
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 41
- 239000010445 mica Substances 0.000 claims description 41
- 229910052618 mica group Inorganic materials 0.000 claims description 41
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 41
- 239000000377 silicon dioxide Substances 0.000 claims description 41
- 235000012239 silicon dioxide Nutrition 0.000 claims description 27
- 150000001875 compounds Chemical class 0.000 claims description 26
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 22
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 20
- 229910052744 lithium Inorganic materials 0.000 claims description 20
- 230000001681 protective effect Effects 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- RNPXCFINMKSQPQ-UHFFFAOYSA-N dicetyl hydrogen phosphate Chemical compound CCCCCCCCCCCCCCCCOP(O)(=O)OCCCCCCCCCCCCCCCC RNPXCFINMKSQPQ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 5
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 3
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 3
- 239000012969 di-tertiary-butyl peroxide Substances 0.000 claims description 3
- DIRFUJHNVNOBMY-UHFFFAOYSA-N fenobucarb Chemical compound CCC(C)C1=CC=CC=C1OC(=O)NC DIRFUJHNVNOBMY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 239000003963 antioxidant agent Substances 0.000 claims 1
- 230000003078 antioxidant effect Effects 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 15
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 4
- 239000003063 flame retardant Substances 0.000 abstract description 4
- 125000006850 spacer group Chemical group 0.000 abstract 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 23
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 23
- 229920001276 ammonium polyphosphate Polymers 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 17
- 238000012360 testing method Methods 0.000 description 15
- 239000002994 raw material Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000004880 explosion Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000000779 smoke Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
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- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- JPMIIZHYYWMHDT-UHFFFAOYSA-N octhilinone Chemical compound CCCCCCCCN1SC=CC1=O JPMIIZHYYWMHDT-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 238000011076 safety test Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
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- 230000001629 suppression Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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Images
Classifications
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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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- Compositions Of Macromolecular Compounds (AREA)
- Battery Mounting, Suspending (AREA)
Abstract
The invention discloses a thermal protection material for a lithium ion battery, which is characterized by comprising the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 20-70 parts of white carbon black, 5-10 parts of KH-550, 0.5-10 parts of peroxide vulcanizing agent, 2-8 parts of anti-aging agent, 0.2-5 parts of accelerator, 5-15 parts of boron nitride nanoparticles, 15-40 parts of silica aerogel and 20-80 parts of porcelain forming filler. The invention also discloses a preparation method of the thermal protection material, which comprises the steps of mixing, die pressing, microwave vulcanization and the like. The thermal protection material provided by the invention has a thermal conductivity coefficient higher than that of ethylene propylene diene monomer at normal temperature, can form a ceramic body with certain strength through thermal reaction at high temperature, not only reduces the thermal conductivity coefficient, but also effectively improves the flame retardant property of the thermal protection material, and can prevent the occurrence of chain reaction when the battery unit is out of control due to heat by using the material as a spacer between the single batteries of the battery pack.
Description
Technical Field
The invention belongs to the field of battery safety protection, and particularly relates to a thermal protection material for a lithium ion battery and a preparation method thereof.
Background
Under the conditions of increasingly scarce natural resources and continuously deteriorated ecological environment, low-emission and energy-saving electric vehicles are favored by the public and are supported by the government. The lithium ion battery has the advantages of high energy density, long cycle life, small self-discharge, no pollution and the like, and is widely applied to new energy automobiles as a power battery pack. However, when the lithium ion battery is used as a battery of an electric vehicle, the internal temperature of the battery is significantly increased due to large charging and discharging current and poor heat dissipation conditions, and even the temperature of the lithium ion battery can be increased to about 700 ℃ under the conditions of thermal abuse, electrical abuse and mechanical abuse, so that safety accidents such as fire and explosion are easily caused. In recent years, because safety runaway accidents of lithium ion batteries of electric vehicles frequently occur, all parties worry about and pay attention to the accidents. Against this background, countries in the world have very strict standards for the safety performance of batteries, such as safety tests of external burning of batteries (a phenomenon that the temperature accumulation finally causes the damage of the storage battery due to the occurrence of an external fire source which heats the module), thermal runaway (a phenomenon that the current and the temperature of the batteries are subjected to an accumulated mutual enhancement effect during the charging/discharging process of the batteries to cause the damage of the storage battery), and the like. In the battery pack module, a plurality of battery cells are mutually attached, when one of the battery cells is thermally out of control, other battery cells connected in series or in parallel with the battery cell are likely to be thermally out of control, the SEI film is subjected to decomposition reaction to generate high-temperature gas, and the shell is broken to cause battery explosion.
Aiming at the problem that a series of exothermic reactions occur to cause thermal runaway of a lithium battery, the solution mainly comprises two aspects: firstly, the safety of internal materials is improved, including the selection and modification of SEI film materials, the flame retardant property of electrolyte, the optimization of electrode materials and the like; the second is an external safety device which comprises a safety pressure relief valve, a temperature sensitive electrode (PTC electrode), a heat sealing electrode and a heat management device. The protective material can separate the batteries in the battery pack, effectively reduce the heat transfer quantity among the batteries, delay the propagation of thermal runaway in the battery pack and reduce the number of damaged batteries is an important technical approach for solving the safety problem of the lithium ion battery pack.
Disclosure of Invention
Aiming at the defects of the current lithium ion battery thermal protection technology, the invention provides a thermal protection material for a lithium ion battery and a preparation method thereof, wherein the thermal protection material is low-temperature heat-conducting high-temperature ceramic heat-insulating.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows.
The thermal protection material for the lithium ion battery comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 20-70 parts of white carbon black, 5-10 parts of KH-550, 0.5-10 parts of peroxide vulcanizing agent, 2-8 parts of anti-aging agent, 0.2-5 parts of accelerator, 5-15 parts of boron nitride nanoparticles, 15-40 parts of silica aerogel and 20-80 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 60-70 parts of white carbon black, 8-10 parts of KH-550, 9-10 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4-5 parts of accelerator, 12-15 parts of boron nitride nanoparticles, 30-40 parts of silica aerogel and 60-80 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 20 parts of white carbon black, KH-5505 parts, 0.5 part of peroxide vulcanizing agent, 2 parts of anti-aging agent, 0.2 part of accelerator, 5 parts of boron nitride nanoparticles, 15 parts of silica aerogel and 20 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 70 parts of white carbon black, 10 parts of KH-55010 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 5 parts of accelerator, 15 parts of boron nitride nanoparticles, 40 parts of silica aerogel and 80 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 70 parts of white carbon black, 10 parts of KH-55010 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 5 parts of accelerator, 15 parts of boron nitride nanoparticles, 40 parts of silica aerogel and 80 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4 parts of accelerator, 12 parts of boron nitride nanoparticles, 30 parts of silica aerogel and 60 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 45 parts of white carbon black, KH-5508 parts, 6 parts of peroxide vulcanizing agent, 4 parts of anti-aging agent, 2 parts of accelerator, 10 parts of boron nitride nanoparticles, 25 parts of silica aerogel and 50 parts of porcelain forming filler;
preferably, in the thermal protection material, the peroxide vulcanizing agent is one or a mixture of DCP, DTBP and BPMC; more preferably DCP;
preferably, in the thermal protection material, the accelerator is one or a mixture of several of PDM, TAIC and TAC; more preferably PDM;
preferably, in the thermal protection material, the porcelain forming filler is a mixture of APP, zinc borate, silica, montmorillonite and mica;
more preferably, in the porcelain forming filler, the mass ratio of silica, mica and montmorillonite is 50: (10-30): (40-20); further preferably 50:20-30:20-30, still further preferably 50:30:20 or 50:20: 30;
further preferably, in the porcelain forming filler, the APP accounts for 5-15% of the total mass of the silica, the mica and the montmorillonite; further preferably 12% to 15%, still further preferably 12% or 15%;
still further preferably, in the porcelain forming filler, the mass of the zinc borate is 10-20% of the total mass of the silica, the mica and the montmorillonite; further preferably 15% to 20%, still further preferably 15% or 20%;
preferably, the anti-aging agent in the thermal protection material is MMBZ;
preferably, the propylene content of the EPDM in the thermal protection material is 30-50 wt%;
a method of making a thermal protective material for a lithium ion battery, wherein the method comprises the steps of:
(1) adding APP, zinc borate, silicon dioxide, montmorillonite and mica into a high-speed mixer, mixing for 10min at the rotating speed of 800-;
(2) mixing Ethylene Propylene Diene Monomer (EPDM), white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 at 20-50 ℃ for 5-8min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(3) mixing the first mixed rubber obtained in the step (2) with the product obtained in the step (1), an accelerator and a peroxide vulcanizing agent at 40-60 ℃ for 3-5min, thinly passing through a lower sheet, and cooling to obtain a second mixed rubber;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (5) placing the product obtained in the step (4) into microwave vulcanization equipment for microwave vulcanization to obtain the thermal protection material for the lithium battery.
Preferably, in the step (5), the temperature of the microwave vulcanization is 110-130 ℃, and the time of the microwave vulcanization is 4-12 min.
The invention also provides a lithium ion battery pack, which comprises a plurality of batteries arranged together, wherein adjacent batteries of the battery pack are separated by the thermal protection material provided by the invention.
The beneficial effects of the invention at least comprise the following aspects:
in a high-temperature or open-fire ablation environment, eutectic melting and eutectic reaction can occur among the ceramic forming fillers in the thermal protection material, so that a compact ceramic body with certain strength is formed, the ceramic body has certain supporting capacity, the complete shape can be still maintained even in an explosion and high-temperature combustion environment, and the flame retardant property and smoke suppression property of the material are improved.
The ceramic layer generated by the thermal protection material burning at high temperature or open fire can effectively obstruct the heat transmission, and effectively reduce the peripheral temperature of adjacent lithium ion batteries, thereby improving the safety performance and playing a good thermal runaway protection role.
Furthermore, in the formula design of the thermal protection material, the silicon dioxide aerogel particles are connected through the boron nitride nanoparticles to form a heat conduction network, so that the heat conduction coefficient of Ethylene Propylene Diene Monomer (EPDM) under the normal temperature condition is effectively improved; and when the boron nitride nanoparticles are in a high-temperature environment, the crystal form of the boron nitride nanoparticles is changed, and the EPDM thermal decomposition product gas damages a heat conduction network, so that the heat conductivity coefficient is reduced under the high-temperature condition, and the flame retardance and the thermal protection performance of the material are not influenced.
Drawings
FIG. 1 is a microscopic topography of a thermal protective material after pyrolysis.
Detailed Description
The invention is illustrated below with reference to specific examples. It will be understood by those skilled in the art that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention in any way.
The raw materials and reagents used in the following examples are all commercially available products unless otherwise specified. Wherein, the purchase conditions of part of the reagents are as follows:
white carbon black: chemical Limited, Kathon, Jinan;
boron nitride nanoparticles: chemical products, Inc. of Jixin, Henan;
silica aerogel: changsha fudakang chemical Co., Ltd;
APP (ammonium polyphosphate): shandong Yunjing chemical Co., Ltd;
zinc borate: henan Shengkun chemical products, Inc.;
montmorillonite: shandong Xiang constant chemical industry Co., Ltd;
mica: guangzhou Jiaqi biotechnology limited;
ethylene propylene diene monomer: mitsui chemical (shanghai) limited.
Example 1
The thermal protection material for the lithium battery is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 20 parts of white carbon black, KH-5505 parts, 0.5 part of peroxide vulcanizing agent, 2 parts of anti-aging agent, 0.2 part of accelerator, 5 parts of boron nitride nanoparticles, 15 parts of silica aerogel and 20 parts of porcelain forming filler;
wherein the porcelain-forming filler is a mixture of APP, zinc borate, silicon dioxide, montmorillonite and mica;
wherein the mass ratio of the silicon dioxide, the mica and the montmorillonite is 50: 10: 40;
wherein the mass of the APP is 5 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
wherein the mass of the zinc borate is 10 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
the preparation method of the thermal protection material for the lithium battery in the embodiment comprises the following steps:
(1) according to the mass parts, APP, zinc borate, silica, montmorillonite and mica are added into a high-speed mixer, mixed for 10min at the rotating speed of 800r/min, and then discharged for later use;
(2) mixing Ethylene Propylene Diene Monomer (EPDM), white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 at 20 ℃ for 5min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(3) mixing an accelerator, a peroxide vulcanizing agent, the first rubber compound obtained in the step (2) and the product obtained in the step (1) at 40 ℃ for 3min, thinly passing through a lower sheet, and cooling to obtain a second rubber compound;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (4) placing the product obtained in the step (4) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 110 ℃, and the vulcanization time is 4 min. And obtaining the thermal protection material for the lithium battery.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Example 2
The thermal protection material for the lithium battery is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 30 parts of white carbon black, KH-5507 parts, 3 parts of peroxide vulcanizing agent, 3 parts of anti-aging agent, 1 part of accelerator, 8 parts of boron nitride nanoparticles, 20 parts of silica aerogel and 30 parts of porcelain forming filler;
wherein the porcelain-forming filler is a mixture of APP, zinc borate, silicon dioxide, montmorillonite and mica;
wherein the mass ratio of the silicon dioxide, the mica and the montmorillonite is 50:20:30, of a nitrogen-containing gas;
wherein the mass of the APP is 8 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
wherein the mass of the zinc borate is 13 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
the preparation method of the thermal protection material for the lithium battery in the embodiment comprises the following steps:
(1) according to the mass parts, APP, zinc borate, silica, montmorillonite and mica are added into a high-speed mixer, mixed for 10min at the rotating speed of 1000r/min, and then discharged for later use;
(2) mixing EPDM, white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 for 5min at the temperature of 30 ℃, thinly passing through a lower sheet, and cooling to obtain a first rubber compound;
(3) mixing an accelerator, a peroxide vulcanizing agent, the first rubber compound obtained in the step (2) and the product obtained in the step (1) at 45 ℃ for 3min, thinly passing through a lower sheet, and cooling to obtain a second rubber compound;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (4) placing the product obtained in the step (4) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 115 ℃, and the vulcanization time is 6 min. And obtaining the thermal protection material for the lithium battery.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Example 3
The thermal protection material for the lithium battery is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 40 parts of white carbon black, KH-5507 parts, 5 parts of peroxide vulcanizing agent, 4 parts of anti-aging agent, 2 parts of accelerator, 10 parts of boron nitride nanoparticles, 25 parts of silica aerogel and 40 parts of porcelain forming filler;
wherein the porcelain-forming filler is a mixture of APP, zinc borate, silicon dioxide, montmorillonite and mica;
wherein the mass ratio of the silicon dioxide, the mica and the montmorillonite is 50: 25: 25;
wherein the mass of the APP is 10 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
wherein the mass of the zinc borate is 15 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
the preparation method of the thermal protection material for the lithium battery in the embodiment comprises the following steps:
(1) according to the mass parts, APP, zinc borate, silica, montmorillonite and mica are added into a high-speed mixer, mixed for 10min at the rotating speed of 1500r/min, and then discharged for later use;
(2) mixing EPDM, white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 at 50 ℃ for 6min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(3) mixing an accelerator, a peroxide vulcanizing agent, the first rubber compound obtained in the step (2) and the product obtained in the step (1) at 50 ℃ for 4min, thinly passing through a lower sheet, and cooling to obtain a second rubber compound;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (4) placing the product obtained in the step (4) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 120 ℃, and the vulcanization time is 8 min. And obtaining the thermal protection material for the lithium battery.
Wherein the peroxide vulcanizing agent is DTBP;
the accelerator is TAIC;
the anti-aging agent is MMBZ.
Example 4
The thermal protection material for the lithium battery is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 70 parts of white carbon black, 10 parts of KH-55010 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 5 parts of accelerator, 15 parts of boron nitride nanoparticles, 40 parts of silica aerogel and 80 parts of porcelain forming filler;
wherein the porcelain-forming filler is a mixture of APP, zinc borate, silicon dioxide, montmorillonite and mica;
wherein the mass ratio of the silicon dioxide, the mica and the montmorillonite is 50:30: 20;
wherein the mass of the APP is 15 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
wherein the mass of the zinc borate is 20 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
the preparation method of the thermal protection material for the lithium battery in the embodiment comprises the following steps:
(1) according to the mass parts, APP, zinc borate, silica, montmorillonite and mica are added into a high-speed mixer, mixed for 10min at the rotating speed of 1500r/min, and then discharged for later use;
(2) mixing EPDM, white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 at 50 ℃ for 8min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(3) mixing an accelerator, a peroxide vulcanizing agent, the first rubber compound obtained in the step (2) and the product obtained in the step (1) at 60 ℃ for 5min, thinly passing through a lower sheet, and cooling to obtain a second rubber compound;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (4) placing the product obtained in the step (4) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 130 ℃, and the vulcanization time is 12 min. And obtaining the thermal protection material for the lithium battery.
Wherein the peroxide vulcanizing agent is BPMC;
the accelerator is TAC;
the anti-aging agent is MMBZ.
Example 5
The thermal protection material for the lithium battery is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4 parts of accelerator, 12 parts of boron nitride nanoparticles, 30 parts of silica aerogel and 60 parts of porcelain forming filler;
wherein the porcelain-forming filler is a mixture of APP, zinc borate, silicon dioxide, montmorillonite and mica;
wherein the mass part ratio of the silicon dioxide, the mica and the montmorillonite is 50:20:30, of a nitrogen-containing gas;
wherein the mass of the APP is 12 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
wherein the mass of the zinc borate is 15 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
the preparation method of the thermal protection material for the lithium battery in the embodiment comprises the following steps:
(1) according to the mass parts, APP, zinc borate, silica, montmorillonite and mica are added into a high-speed mixer, mixed for 10min at the rotating speed of 1200r/min, and then discharged for later use;
(2) mixing EPDM, white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 for 8min at the temperature of 30 ℃, thinly passing through a lower sheet, and cooling to obtain a first rubber compound;
(3) mixing an accelerator, a peroxide vulcanizing agent, the first rubber compound obtained in the step (2) and the product obtained in the step (1) at 40 ℃ for 5min, thinly passing through a lower sheet, and cooling to obtain a second rubber compound;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (5) placing the product obtained in the step (4) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 120 ℃, and the vulcanization time is 10 min. And obtaining the thermal protection material for the lithium battery.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Comparative example 1
The thermal protection material of the comparative example is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4 parts of accelerator, 12 parts of boron nitride nanoparticles and 30 parts of silica aerogel.
The preparation method of the thermal protection material of the comparative example comprises the following steps:
(1) mixing EPDM, white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 for 8min at the temperature of 30 ℃, thinly passing through a lower sheet, and cooling to obtain a first rubber compound;
(2) mixing an accelerator, a peroxide vulcanizing agent and the first mixed rubber obtained in the step (1) at 40 ℃ for 5min according to the mass parts, thinly passing through a lower sheet, and cooling to obtain a second mixed rubber;
(3) die pressing the second rubber compound obtained in the step (2) at normal temperature to obtain a die pressing product with a set shape and size;
(4) and (4) placing the product obtained in the step (3) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 120 ℃, and the vulcanization time is 10 min. Obtaining the thermal protection material.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Comparative example 2
The thermal protection material of the comparative example is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4 parts of accelerator and 12 parts of boron nitride nanoparticles.
The preparation method of the thermal protection material of the comparative example comprises the following steps:
(1) mixing EPDM, white carbon black, an anti-aging agent, boron nitride nanoparticles and KH-550 at 30 ℃ for 8min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(2) mixing an accelerator, a peroxide vulcanizing agent and the first mixed rubber obtained in the step (1) at 40 ℃ for 5min according to the mass parts, thinly passing through a lower sheet, and cooling to obtain a second mixed rubber;
(3) die pressing the second rubber compound obtained in the step (2) at normal temperature to obtain a die pressing product with a set shape and size;
(4) and (4) placing the product obtained in the step (3) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 120 ℃, and the vulcanization time is 10 min. Obtaining the thermal protection material.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Comparative example 3
The thermal protection material of the comparative example is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent and 4 parts of accelerator.
The preparation method of the thermal protection material of the comparative example comprises the following steps:
(1) mixing EPDM, white carbon black, an anti-aging agent and KH-550 for 8min at the temperature of 30 ℃, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(2) mixing an accelerator, a peroxide vulcanizing agent and the first mixed rubber obtained in the step (1) at 40 ℃ for 5min according to the mass parts, thinly passing through a lower sheet, and cooling to obtain a second mixed rubber;
(3) die pressing the second rubber compound obtained in the step (2) at normal temperature to obtain a die pressing product with a set shape and size;
(4) and (4) placing the product obtained in the step (3) in microwave vulcanization equipment for microwave vulcanization, wherein the microwave vulcanization temperature is 120 ℃, and the vulcanization time is 10 min. Obtaining the thermal protection material.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Comparative example 4
The thermal protection material of the comparative example is prepared from the following raw materials in parts by mass: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4 parts of accelerator, 30 parts of silica aerogel and 60 parts of porcelain forming filler;
wherein the porcelain-forming filler is a mixture of APP, zinc borate, silicon dioxide, montmorillonite and mica;
wherein the mass ratio of the silicon dioxide, the mica and the montmorillonite is 50:20:30, of a nitrogen-containing gas;
wherein the mass of the APP is 12 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
wherein the mass of the zinc borate is 15 percent of the total mass of the silicon dioxide, the mica and the montmorillonite;
the preparation method of the thermal protection material applied to the lithium battery comprises the following steps:
(1) according to the mass parts, APP, zinc borate, silica, montmorillonite and mica are added into a high-speed mixer, mixed for 10min at the rotating speed of 1200r/min, and then discharged for later use;
(2) mixing EPDM, white carbon black, an anti-aging agent, silica aerogel and KH-550 at 30 ℃ for 8min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(3) mixing an accelerator, a peroxide vulcanizing agent, the first rubber compound obtained in the step (2) and the product obtained in the step (1) at 40 ℃ for 5min, thinly passing through a lower sheet, and cooling to obtain a second rubber compound;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (5) placing the product obtained in the step (4) into microwave vulcanization equipment for microwave vulcanization, wherein the vulcanization temperature is 120 ℃, and the vulcanization time is 10 min. Obtaining the thermal protection material.
Wherein the peroxide vulcanizing agent is DCP;
the accelerant is PDM;
the anti-aging agent is MMBZ.
Test example: performance testing
The thermal protective materials prepared in examples 1 to 5 and comparative examples 1 to 4 were subjected to performance tests:
(1) mechanical Property test
The dumbbell-shaped test sample is cut according to the national standard GB/T528-.
Table 1: mechanical property test results of thermal protective materials prepared in examples 1 to 5 and comparative examples 1 to 4
According to the test results in table 1, it can be seen that the thermal protection material prepared by the invention still maintains a certain mechanical property, and can meet the basic physical and mechanical property requirements of the battery pack protection material.
(2) Oxygen index test
The test is carried out according to the oxygen index test standard GB/T10707-. Sample size: 100mm long, 6.5mm wide and 3mm thick.
Table 2: oxygen index of thermal protective material prepared in examples 1 to 5 and comparative examples 1 to 4
According to the oxygen index test result shown in the table 2, the ceramic filler can effectively block the heat transmission in the combustion environment, and the flame retardant property of the thermal protection material is improved.
(3) Determination of thermal conductivity
The thermal conductivity of the material was tested by laser method according to ASTM E1461. The sample is cylindrical sheet, and the size is as follows: the diameter is 12.7 +/-0.1 mm, and the thickness is 0.5-4 mm.
Table 3: thermal conductivity of thermal protective material prepared in examples 1 to 5 and comparative examples 1 to 4
The test results in table 3 show that the heat conduction channel formed by the boron nitride and silica aerogel system designed by the invention can effectively improve the heat conductivity coefficient of EPDM, and the heat diffusion condition of the thermal protection material can be improved at normal temperature; in a high-temperature environment, the boron nitride and the ceramic filler are subjected to thermal reaction, the crystal form is transformed, and a ceramic body is formed, and the formed ceramic layer has a low heat conductivity coefficient, which shows that the formula of the invention does not influence the heat insulation performance of the thermal protection material at a high temperature.
(4) Test for vitrifying Properties
A sample with the size of 80mm multiplied by 10mm multiplied by 4mm is placed into a muffle furnace through cutting, the temperature is raised to 600 ℃ at the heating rate of 10 ℃/min and then is preserved for 1h, then the temperature is lowered to the room temperature, the sample is taken out, and the bending strength of the ceramic body is measured according to the GB/T14390-.
Table 4: properties of ceramicized products of thermal protective materials obtained in examples 1 to 5 and comparative examples 1 to 4
The test results in table 4 show that the formula designed by the invention can form a self-supporting compact ceramic body with certain strength, effectively block the transmission of heat between adjacent battery packs and improve the safety of the battery packs. FIG. 1 is an SEM image of a cross section of a ceramic body formed by the thermal protective material prepared in example 5 after being heated in a muffle furnace, and from a microscopic morphology, a sample forms a dense ceramic body in a high-temperature environment.
(5) Smoke Rate test
The characteristic signal transmittance of the thermal protection material at 800 ℃ is measured according to Q/AY69A-2003 coating layer smoke determination method-infrared, visible light and laser transmittance method.
Table 5: characteristic signal transmittance of thermal protective material obtained in examples 1 to 5 and comparative examples 1 to 4
The test results in table 5 show that the formation of the ceramic layer effectively reduces the gas generation amount, destroys and blocks the volatilization channel of the gas, reduces the smoke generation amount, and improves the transmittance of the characteristic signal.
Application experiment of thermal protective material
In the experiment, the heating rod is used as a heat source to trigger the battery to generate thermal runaway. A4 mm thick sheet of thermal protective material prepared in example 5 was placed between two 6A ternary lithium batteries, a heating rod was placed against one of the batteries, the heating rod, and the sheet were fixedly connected together in a wire-wound manner, and then heated.
As a result, the first battery started burning after 15min and 26s, then explosion occurred at 17min and 12s, the thermal protection material connected with the first battery started burning, flame gradually decreased after 19min and 26s, and flame extinguished after 22min and 45 s.
Claims (10)
1. The thermal protection material for the lithium ion battery is characterized by comprising the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 20-70 parts of white carbon black, 5-10 parts of KH-550, 0.5-10 parts of peroxide vulcanizing agent, 2-8 parts of anti-aging agent, 0.2-5 parts of accelerator, 5-15 parts of boron nitride nanoparticles, 15-40 parts of silica aerogel and 20-80 parts of porcelain forming filler.
2. The thermal protection material of claim 1, wherein the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 60-70 parts of white carbon black, 8-10 parts of KH-550, 9-10 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4-5 parts of accelerator, 12-15 parts of boron nitride nanoparticles, 30-40 parts of silica aerogel and 60-80 parts of porcelain forming filler;
preferably, the thermal protection material comprises the following components in parts by weight: 100 parts of ethylene propylene diene monomer, 60 parts of white carbon black, KH-5508 parts, 9 parts of peroxide vulcanizing agent, 8 parts of anti-aging agent, 4 parts of accelerator, 12 parts of boron nitride nano particles, 30 parts of silica aerogel and 60 parts of porcelain forming filler.
3. The thermal protective material according to claim 1 or 2, wherein the peroxide curing agent is one or a mixture of several selected from DCP, DTBP and BPMC;
preferably, the accelerator is one or a mixture of several selected from PDM, TAIC and TAC.
4. The thermal protection material according to any one of claims 1 to 3, characterized in that said ceramic-forming filler is a mixture of APP, zinc borate, silica, montmorillonite and mica;
preferably, in the porcelain forming filler, the mass ratio of the silica to the mica to the montmorillonite is 50: 10-30: 40-20 parts of; more preferably 50:20-30:20-30, still more preferably 50:30:20 or 50:20:30
Preferably, in the porcelain forming filler, the APP accounts for 5-15% of the total mass of the silica, the mica and the montmorillonite; further preferably 12% to 15%, still further preferably 12% or 15%;
preferably, in the porcelain forming filler, the mass of the zinc borate is 10-20% of the total mass of the silica, the mica and the montmorillonite; further preferably 15% to 20%, still further preferably 15% or 20%.
5. The thermal protection material according to any one of claims 1 to 4, wherein the antioxidant is MMBZ.
6. The thermal protection material according to any one of claims 1 to 5, wherein the propylene content of the ethylene propylene diene rubber is 30 to 50 wt%.
7. A method of preparing a thermal protective material according to any one of claims 1 to 6, comprising the steps of:
(1) adding APP, zinc borate, silicon dioxide, montmorillonite and mica into a high-speed mixer, mixing for 10min at the rotating speed of 800-;
(2) mixing ethylene propylene diene monomer, white carbon black, an anti-aging agent, boron nitride nanoparticles, silica aerogel and KH-550 at 20-50 ℃ for 5-8min, thinly passing through a lower sheet, and cooling to obtain a first mixed rubber;
(3) mixing the first mixed rubber obtained in the step (2) with the product obtained in the step (1), an accelerator and a peroxide vulcanizing agent at 40-60 ℃ for 3-5min, thinly passing through a lower sheet, and cooling to obtain a second mixed rubber;
(4) die pressing the second rubber compound obtained in the step (3) at normal temperature to obtain a die pressing product with a set shape and size;
(5) and (5) placing the product obtained in the step (4) into microwave vulcanization equipment for microwave vulcanization to obtain the thermal protection material for the lithium battery.
8. The production method according to claim 7, wherein in the step (1), the rotation speed is 1200 r/min;
preferably, in the step (2), mixing is carried out for 8min at the temperature of 30 ℃;
preferably, in step (3), the mixture is kneaded at 40 ℃ for 5 min.
9. The preparation method according to claim 7 or 8, wherein the temperature of the microwave vulcanization in the step (5) is 110-; preferably, the temperature of the microwave vulcanization is 120 ℃, and the time of the microwave vulcanization is 10 min.
10. A lithium ion battery comprising a plurality of cells arranged together, wherein adjacent cells of the battery are separated by the thermal protective material of any one of claims 1-6 or the thermal protective material prepared by the preparation method of any one of claims 7-9.
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