CN115340828B - Lithium ion battery termination adhesive tape with corrosion resistance - Google Patents
Lithium ion battery termination adhesive tape with corrosion resistance Download PDFInfo
- Publication number
- CN115340828B CN115340828B CN202210787498.5A CN202210787498A CN115340828B CN 115340828 B CN115340828 B CN 115340828B CN 202210787498 A CN202210787498 A CN 202210787498A CN 115340828 B CN115340828 B CN 115340828B
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- sericite
- heating
- adhesive tape
- lithium ion
- parts
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- 239000002390 adhesive tape Substances 0.000 title claims abstract description 48
- 230000007797 corrosion Effects 0.000 title claims abstract description 35
- 238000005260 corrosion Methods 0.000 title claims abstract description 35
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 62
- 239000000758 substrate Substances 0.000 claims abstract description 46
- 239000010410 layer Substances 0.000 claims abstract description 40
- 229920001721 polyimide Polymers 0.000 claims abstract description 34
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims abstract description 33
- 238000002360 preparation method Methods 0.000 claims abstract description 31
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
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- 230000002194 synthesizing effect Effects 0.000 claims abstract description 5
- 239000000839 emulsion Substances 0.000 claims description 50
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- 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 claims description 25
- 239000003063 flame retardant Substances 0.000 claims description 25
- 239000007788 liquid Substances 0.000 claims description 25
- -1 modified acrylic ester Chemical class 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 22
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 15
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
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- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 10
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 10
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
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- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 claims description 10
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- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 7
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 5
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
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- 239000000203 mixture Substances 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 3
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- 238000004321 preservation Methods 0.000 claims description 3
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- 239000011780 sodium chloride Substances 0.000 claims description 3
- ZPHGMBGIFODUMF-UHFFFAOYSA-N thiophen-2-ylmethanol Chemical compound OCC1=CC=CS1 ZPHGMBGIFODUMF-UHFFFAOYSA-N 0.000 claims description 3
- 238000013329 compounding Methods 0.000 claims 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 15
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
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- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 125000003118 aryl group Chemical group 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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Classifications
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- C09J7/00—Adhesives in the form of films or foils
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- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/058—Construction or manufacture
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/33—Applications of adhesives in processes or use of adhesives in the form of films or foils for batteries or fuel cells
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/41—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the carrier layer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J2475/00—Presence of polyurethane
- C09J2475/001—Presence of polyurethane in the barrier layer
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- C09J2479/00—Presence of polyamine or polyimide
- C09J2479/08—Presence of polyamine or polyimide polyimide
- C09J2479/086—Presence of polyamine or polyimide polyimide in the substrate
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention belongs to the technical field of lithium battery packaging, and discloses a lithium ion battery termination adhesive tape with corrosion resistance, which comprises a substrate layer, a release layer and a pressure-sensitive adhesive layer, wherein the release layer and the adhesive layer are respectively arranged on two sides of the substrate layer, the substrate layer is a modified polyimide film, and the preparation method of the lithium ion battery termination adhesive tape comprises the following steps: s1, adding intercalated sericite in the process of synthesizing polyimide to prepare a tape substrate; s2, coating pressure-sensitive adhesive, and heating and curing to form an adhesive layer; s3, coating a release agent, and forming a release layer after UV curing; and S4, cooling by using equipment, rolling and cutting to obtain the finished product of the lithium ion battery termination adhesive tape. The adhesive tape substrate adopted by the invention is a modified polyimide film, and polyimide has high and low temperature resistance, ultraviolet radiation resistance, chemical solvent corrosion resistance and high insulating property, and the modification of the organosilicon intercalated sericite improves the corona resistance and the barrier property of the film, thereby improving the corrosion resistance of the adhesive tape.
Description
Technical Field
The invention relates to the technical field of lithium battery packaging, in particular to a lithium ion battery termination adhesive tape with corrosion resistance.
Background
The lithium battery has high energy density, long service life and small pollution, and can be used for multiple charging and discharging, and is widely used in the fields of mobile phones, notebook computers, wearable electronic equipment, energy storage devices and the like. Along with the improvement of the technology level, the safety requirements of various fields on the lithium battery are higher and higher, wherein the high requirements on the anti-falling performance of the lithium battery are put forward, and the stability and the safety of the lithium battery are determined by the anti-falling performance of the lithium battery. The anti-dropping performance of the lithium battery is mainly determined by the fit between the electrode group and the outer packaging material, if the fit between the electrode group and the outer packaging material of the battery is poor, when the battery moves horizontally or vertically, the electrode group and the outer packaging material can move relatively, and when serious, the electrode group is deformed to cause the short circuit of the battery, thereby bringing the fire, explosion and other risks of the battery.
The lithium battery stopping adhesive tape is a special pressure-sensitive adhesive product, and has special requirements on the aspects of substrate selection, adhesion, chemical corrosion resistance and the like besides the performance of pressure-sensitive adhesive. The batteries commonly used in the market at present mainly comprise nickel-chromium batteries, nickel-hydrogen batteries, lead-acid batteries, lithium batteries and the like. With the rapid development of electronic products, electric vehicles and electric bicycles, the demand of lithium batteries has been greatly increased. There is a great demand for adhesive tapes for use in the lithium battery industry. In the manufacturing process of the lithium battery, the positive electrode sheet, the diaphragm and the negative electrode sheet are wound into a battery core, and then electrolyte is injected. The core technology of its application is the electrolyte sealing of the cell, for which purpose a termination tape is used to improve the tightness of the packaging of the electrode into the cell.
The adhesive tape made of the common acrylic glue on the market is easy to corrode and permeate under the soaking of the strong polar solvent of the electrolyte, so that the adhesive tape loses viscosity, a metal tape of a battery cannot be effectively fixed, the battery is short-circuited, the service life of the battery is shortened, and serious potential safety hazards exist. Therefore, there is a need for a termination tape that is resistant to electrolyte corrosion to meet the needs of lithium battery packaging.
Disclosure of Invention
In order to solve the defects in the background art, the invention aims to provide the lithium ion battery termination adhesive tape with corrosion resistance, and the adhesive tape base material adopted by the invention is a modified polyimide film, and has high and low temperature resistance, ultraviolet radiation resistance, chemical solvent corrosion resistance and high insulation performance due to the fact that the adhesive tape base material contains imide rings, aromatic rings and other rigid structures, and on the other hand, the corona resistance and the blocking capability of the film are improved through the modification of organosilicon intercalated sericite, so that the corrosion of electrolyte and the impact of high-frequency power electrons are prevented, and the corrosion resistance of the adhesive tape is further improved.
The aim of the invention can be achieved by the following technical scheme:
the lithium ion battery termination adhesive tape with corrosion resistance comprises a substrate layer, a release layer and a pressure-sensitive adhesive layer, wherein the release layer and the adhesive layer are respectively arranged on two sides of the substrate layer, the substrate layer is a modified polyimide film, and the preparation method of the lithium ion battery termination adhesive tape comprises the following steps:
s1, adding intercalated sericite in the process of synthesizing polyimide by using diamine monomers and dianhydride monomers to prepare a modified polyimide film, so as to obtain a tape substrate;
s2, uniformly coating the pressure-sensitive adhesive on one side surface of the substrate, and heating for 3-5min by a baking oven at 75-85 ℃ to form an adhesive layer after high-temperature curing;
s3, turning over the substrate, uniformly coating a release agent on the surface of the other side of the substrate, standing for 20min, and placing under a UV (ultraviolet) light curing machine for light curing to form a release layer;
and S4, cooling by using equipment, rolling and cutting to obtain the finished product of the lithium ion battery termination adhesive tape.
Further preferably, the modified polyimide film comprises the following raw materials in parts by weight: 25-30 parts of 4,4 '-diaminodiphenyl ether, 15-20 parts of 4,4' -diaminodiphenyl sulfide, 40-50 parts of pyromellitic anhydride and 5-10 parts of intercalated sericite.
Further preferably, the preparation method of the modified polyimide film comprises the following steps:
(1) Dissolving 4,4 '-diaminodiphenyl ether and 4,4' -diaminodiphenyl sulfide in N, N-dimethylacetamide, and stirring in an oil bath at 40 ℃ for 40-80min;
(2) Adding intercalated sericite into N, N-dimethylacetamide, performing ultrasonic treatment for 10-30min to obtain an intercalated sericite dispersion liquid, adding the intercalated sericite dispersion liquid into the reaction system of the step (1), adding pyromellitic anhydride, and stirring in an oil bath at 40 ℃ for 8-12h to obtain a mixed solution of polyamide acid and inorganic particles;
(3) And (3) uniformly coating the mixed solution obtained in the step (2) on a substrate after defoaming, and then sending the substrate into an oven for step-heating thermal imidization treatment for 5-8h to obtain the modified polyimide film.
Further preferably, the step (3) of the step-up thermal imidization treatment is specifically: heating at 50-70deg.C, and maintaining for 1-3 hr after temperature stabilization; heating at 110-130deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization; heating at 190-210 deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization; heating at 240-260 deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization; heating at 310-330 deg.C, maintaining for 0.5-1.5 hr after temperature stabilization,
further preferably, the preparation method of the intercalated sericite comprises the following steps:
A. placing sericite into a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, then heating to 800 ℃ at a speed of 10 ℃/min, and then preserving heat for 1-3h to obtain activated sericite;
B. adding activated sericite into nitric acid with the concentration of 5mol/L according to the solid-to-liquid ratio of 2-4%, stirring and reacting for 4-6 hours at the temperature of 90-95 ℃, and filtering and washing for several times to obtain acidified sericite;
C. adding the acidified sericite into a sodium chloride saturated solution according to a solid-to-liquid ratio of 2-4%, stirring and reacting for 4-6 hours at 90-95 ℃, and filtering and washing for several times to obtain the sodium sericite;
D. dissolving 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in toluene, adding sodium sericite into 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane solution according to a solid-to-liquid ratio of 3-5%, performing ultrasonic treatment at 75-85 ℃ for 30-90min, and performing suction filtration and washing for several times to obtain intercalated sericite.
Further preferably, the pressure sensitive adhesive is mixed by modified acrylic ester emulsion and flame retardant polyurethane emulsion according to the mass ratio of 2-3:1.
Further preferably, the modified acrylate emulsion preparation method comprises the following steps:
firstly, adding deionized water and emulsifier sodium dodecyl sulfate into a high-speed mixer, rapidly stirring to enable the emulsifier to be uniformly dissolved, then, uniformly mixing and stirring butyl acrylate, methyl methacrylate, acrylic acid and N-methylol acrylamide, and slowly adding the mixture of the emulsifier and water to form a pre-emulsion; then NaHCO is added 3 Adding the ammonium persulfate into deionized water, continuously stirring to form a buffer solvent aqueous solution, adding the ammonium persulfate into the deionized water, and continuously stirring to form a homogeneous initiator aqueous solution; and finally, adding the pre-emulsion into a reactor, heating to 70 ℃, dripping 1/3 volume of aqueous solution of an initiator and 1/2 of aqueous solution of a buffering agent, uniformly adding the mixture within 30min, preserving heat until the emulsion is blue, heating to 80 ℃, adding the rest pre-emulsion and aqueous solution of the initiator within 3-4h, heating to 90 ℃, preserving heat for 1h, cooling to 40 ℃, discharging, adjusting pH to be neutral, and filtering to obtain the modified acrylic ester emulsion.
Further preferably, the method for preparing the flame retardant polyurethane emulsion comprises the following steps:
firstly, weighing polyether polyol, adding the polyether polyol into a reactor, heating to 60 ℃, then adding isocyanate, uniformly stirring, reacting for 1h at 60 ℃, 70 ℃ and 80 ℃, reacting for 2-3h at constant temperature in nitrogen atmosphere, cooling to 60 ℃, and removing bubbles in vacuum for 30min to obtain polyurethane prepolymer; weighing polyurethane prepolymer, adding trimethylolpropane and flame-retardant reaction monomer, reacting for 30min, and removing bubbles in vacuum for 30min to obtain flame-retardant polyurethane emulsion;
the flame-retardant reaction monomer is 10- (2, 5-dihydroxyphenyl-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide and N, N-bis (hydroxyethyl) aminomethylene diethyl phosphate, and is compounded by (6-oxo-6H-dibenzo [ C, E ] [1,2] oxaphospha-hex-6-yl) hydroxymethyl thiophene according to a molar ratio of 1:1:2.
Further preferably, the release agent is prepared from silane modified polyurethane, ethyl acetate, pentaerythritol tetraacrylate and a photoinitiator 1173 according to the mass ratio of 10:2-5: 2:0.5.
Further preferably, the silane-modified polyurethane comprises the following raw materials in parts by weight: 95-105 parts of 3-isocyanatopropyl triethoxysilane, 12-18 parts of toluene diisocyanate, 15-20 parts of pentaerythritol triacrylate, 0.5-1.2 parts of p-benzoquinone and 5-8 parts of dibutyltin dilaurate, and the preparation method comprises the following steps:
firstly, putting 3-isocyanatopropyl triethoxysilane into a reactor, heating to 60-70 ℃, then putting toluene diisocyanate into the reactor, carrying out heat preservation reaction for 5-10h, using the change condition of isocyanate groups in an infrared analysis system, putting p-benzoquinone into the system after the isocyanate groups are obviously weakened, mixing uniformly, then sequentially putting pentaerythritol triacrylate and dibutyltin dilaurate, and continuing to react for 1-3h to obtain silane modified polyurethane.
The invention has the beneficial effects that:
1. according to the invention, the modified polyimide film is adopted as a base material of the adhesive tape, and the organic silicon intercalation sericite is added in the process of synthesizing polyimide from diamine monomers and dianhydride monomers, so that the organic silicon intercalation sericite has high and low temperature resistance, ultraviolet radiation resistance, chemical solvent corrosion resistance and high insulating property due to the fact that the organic silicon intercalation sericite contains imide rings, aromatic rings and other rigid structures, meanwhile, the 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in the organic silicon intercalation sericite is adopted as a diamine monomer containing a siloxane structure, polyimide synthesized from dianhydride monomers can be obtained without split phase due to the fact that the chain of siloxane is very short, and therefore, the relative molecular mass of the polymer can not be influenced by adopting 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane, the corona resistance and the adhesive property can be increased, meanwhile, the high mechanical property can be kept, and the path is further prevented from being directly penetrated, the diffusion in the transverse direction is increased, and the diffusion time is prolonged, and the termination performance of the adhesive tape is improved.
2. The pressure-sensitive adhesive is prepared by mixing modified acrylic ester emulsion and flame-retardant polyurethane emulsion according to the mass ratio of 2-3:1, so that the pressure-sensitive adhesive has higher initial adhesion, wherein the modified acrylic ester emulsion is prepared from butyl acrylate and methyl propyl acrylateMethyl acrylate, acrylic acid and N-methylol acrylamide are taken as polymerization monomers, an acrylic ester emulsion is prepared by adopting a semi-continuous emulsion polymerization method, the viscosity of the polymerization emulsion is reduced, the cohesive strength of the pressure-sensitive adhesive is improved, and the acrylic ester emulsion pressure-sensitive adhesive with good emulsion stability and excellent adhesive strength is prepared; meanwhile, the reaction type flame-retardant polyurethane emulsion synthesized by adopting the polyurethane prepolymer and the compound flame-retardant reaction monomer contains P, N two elements, which not only can generate acidic substances to promote the dehydration and the char formation of the base material, but also can generate NO 2 The oxygen concentration in the non-combustible gas dilution combustion environment plays a role in inhibiting combustion, and the reactive flame retardant does not influence the adhesive force of the pressure-sensitive adhesive.
Drawings
FIG. 1 is an XRD diffraction pattern of sericite in example 1 of the present invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a lithium ion battery termination adhesive tape with corrosion resistance, which comprises a substrate layer, a release layer and a pressure-sensitive adhesive layer, wherein the release layer and the adhesive layer are respectively arranged at two sides of the substrate layer, and the substrate layer is a modified polyimide film.
1. Preparation of a substrate layer
Example 1
The modified polyimide film comprises the following raw materials in parts by weight: 25 parts of 4,4 '-diaminodiphenyl ether, 15 parts of 4,4' -diaminodiphenyl sulfide, 40 parts of pyromellitic anhydride and 5 parts of intercalated sericite, and the preparation method comprises the following steps:
(1) Dissolving 4,4 '-diaminodiphenyl ether and 4,4' -diaminodiphenyl sulfide in N, N-dimethylacetamide, and stirring in an oil bath at 40 ℃ for 40min;
(2) Adding intercalated sericite into N, N-dimethylacetamide, performing ultrasonic treatment for 10min to obtain an intercalated sericite dispersion liquid, adding the intercalated sericite dispersion liquid into the reaction system of the step (1), adding pyromellitic anhydride, and stirring in an oil bath at 40 ℃ for 8h to obtain a mixed solution of polyamide acid and inorganic particles;
(3) Uniformly coating the mixed solution obtained in the step (2) on a substrate after defoaming, and then sending the substrate into an oven for step-heating thermal imidization: heating at 50 ℃, and keeping for 1h after the temperature is stable; heating at 110 ℃, and keeping for 0.5h after the temperature is stable; heating at 190 ℃, and keeping for 0.5h after the temperature is stable; heating at 240 ℃, and keeping for 0.5h after the temperature is stable; heating at 310 ℃, and keeping the temperature for 0.5h after stabilizing the temperature, thus obtaining the modified polyimide film.
The preparation method of the intercalated sericite comprises the following steps:
A. placing sericite into a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, then heating to 800 ℃ at a speed of 10 ℃/min, and then preserving heat for 1-3h to obtain activated sericite;
B. adding activated sericite into nitric acid with the concentration of 5mol/L according to the solid-to-liquid ratio of 2%, stirring and reacting for 4-6 hours at 90 ℃, and filtering and washing for several times to obtain acidified sericite;
C. adding the acidified sericite into a saturated sodium chloride solution according to a solid-to-liquid ratio of 2%, stirring and reacting for 4-6 hours at 90 ℃, and carrying out suction filtration and washing for several times to obtain the sodium-modified sericite;
D. dissolving 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in toluene, adding sodium sericite into 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane solution according to a solid-to-liquid ratio of 3%, performing ultrasonic treatment at 75 ℃ for 30min, and performing suction filtration and washing for several times to obtain the intercalated sericite.
XRD analysis test is carried out on mica in the intercalation modification process, the sharpness degree and the peak intensity of diffraction peaks in a diffraction spectrogram can qualitatively analyze the crystallinity degree and the crystal distortion degree of crystals, meanwhile, whether corresponding molecules successfully enter the interlayer of lamellar mica or not can be directly reacted through calculating the change of interlayer spacing, and the degree of interlayer spacing expansion caused by intercalation treatment can be calculated, so that the XRD spectrogram of sericite before and after modification is shown in a figure 1, the test range is 20 degrees to 70 degrees, and four a, b, c, d curves in the figure are respectively activated, acidified, sodified and intercalated sericite.
As can be seen from XRD diffraction patterns of sericite, the sharpness of diffraction peaks of crystal faces is obviously reduced, the peaks are gradually widened, and the peak intensity is also gradually reduced, so that the crystallization degree of mica is reduced and the integrity of a crystal structure is destroyed from the raw material sericite to thermalized mica to acidified mica finally to intercalated mica. According to Bragg equation, the spacing between layers of lamellar structure can be directly calculated, and according to XRD spectrogram, as various activation processes are processed, the diffraction peak of mica obviously moves towards the direction of low diffraction angle (leftwards), the spacing between layers is continuously increased, and organosilicon is successfully inserted between lamellar layers of sericite, so that the spacing between layers of sericite is improved.
Example 2
The modified polyimide film comprises the following raw materials in parts by weight: 28 parts of 4,4 '-diaminodiphenyl ether, 16 parts of 4,4' -diaminodiphenyl sulfide, 45 parts of pyromellitic anhydride and 7 parts of intercalated sericite, and the preparation method comprises the following steps:
(1) Dissolving 4,4 '-diaminodiphenyl ether and 4,4' -diaminodiphenyl sulfide in N, N-dimethylacetamide, and stirring in an oil bath at 40 ℃ for 60min;
(2) Adding intercalated sericite into N, N-dimethylacetamide, performing ultrasonic treatment for 20min to obtain an intercalated sericite dispersion liquid, adding the intercalated sericite dispersion liquid into the reaction system of the step (1), adding pyromellitic anhydride, and stirring in an oil bath at 40 ℃ for 10h to obtain a mixed solution of polyamide acid and inorganic particles;
(3) Uniformly coating the mixed solution obtained in the step (2) on a substrate after defoaming, and then sending the substrate into an oven for step-heating thermal imidization: heating at 60 ℃, and keeping for 2 hours after the temperature is stable; heating at 120 ℃, and keeping for 1h after the temperature is stable; heating at 200 ℃, and keeping for 1h after the temperature is stable; heating at 250 ℃, and keeping for 1h after the temperature is stable; heating at 320 ℃, and keeping for 1h after the temperature is stable, thus obtaining the modified polyimide film.
The preparation method of the intercalated sericite comprises the following steps:
A. placing sericite into a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, then heating to 800 ℃ at a speed of 10 ℃/min, and then preserving heat for 2 hours to obtain activated sericite;
B. adding activated sericite into nitric acid with the concentration of 5mol/L according to the solid-to-liquid ratio of 3%, stirring and reacting for 4-6 hours at the temperature of 90-95 ℃, and filtering and washing for several times to obtain acidified sericite;
C. adding the acidified sericite into a saturated sodium chloride solution according to a solid-to-liquid ratio of 3%, stirring and reacting for 4-6 hours at 90-95 ℃, and carrying out suction filtration and washing for several times to obtain the sodium-modified sericite;
D. dissolving 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in toluene, adding sodium sericite into 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane solution according to a solid-to-liquid ratio of 4%, performing ultrasonic treatment at 80 ℃ for 60min, and performing suction filtration and washing for several times to obtain the intercalated sericite.
Example 3
The modified polyimide film comprises the following raw materials in parts by weight: 30 parts of 4,4 '-diaminodiphenyl ether, 20 parts of 4,4' -diaminodiphenyl sulfide, 50 parts of pyromellitic anhydride and 10 parts of intercalated sericite, and the preparation method comprises the following steps:
(1) Dissolving 4,4 '-diaminodiphenyl ether and 4,4' -diaminodiphenyl sulfide in N, N-dimethylacetamide, and stirring in an oil bath at 40 ℃ for 80min;
(2) Adding intercalated sericite into N, N-dimethylacetamide, performing ultrasonic treatment for 30min to obtain an intercalated sericite dispersion liquid, adding the intercalated sericite dispersion liquid into the reaction system of the step (1), adding pyromellitic anhydride, and stirring in an oil bath at 40 ℃ for 12h to obtain a mixed solution of polyamide acid and inorganic particles;
(3) Uniformly coating the mixed solution obtained in the step (2) on a substrate after defoaming, and then sending the substrate into an oven for step-heating thermal imidization: heating at 70 ℃, and keeping for 3 hours after the temperature is stable; heating at 130 ℃, and keeping for 1.5h after the temperature is stable; heating at 210 ℃, and keeping for 1.5h after the temperature is stable; heating at 260 ℃ and keeping for 1.5h after the temperature is stable; heating at 330 ℃, and keeping for 1.5h after the temperature is stable, thus obtaining the modified polyimide film.
The preparation method of the intercalated sericite comprises the following steps:
A. placing sericite into a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, then heating to 800 ℃ at a speed of 10 ℃/min, and then preserving heat for 3 hours to obtain activated sericite;
B. adding activated sericite into nitric acid with the concentration of 5mol/L according to the solid-to-liquid ratio of 4%, stirring and reacting for 6 hours at 95 ℃, and filtering and washing for several times to obtain acidified sericite;
C. adding the acidified sericite into a sodium chloride saturated solution according to a solid-to-liquid ratio of 4%, stirring and reacting for 6 hours at 95 ℃, and carrying out suction filtration and washing for several times to obtain the sodium-modified sericite;
D. dissolving 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in toluene, adding sodium sericite into 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane solution according to a solid-to-liquid ratio of 35%, performing ultrasonic treatment at 85 ℃ for 90min, and performing suction filtration and washing for several times to obtain the intercalated sericite.
2. Preparation of pressure sensitive adhesive
Example 4
The pressure-sensitive adhesive is prepared by mixing modified acrylic ester emulsion and flame-retardant polyurethane emulsion according to a mass ratio of 2:1.
The preparation method of the modified acrylic ester emulsion comprises the following steps:
firstly, adding deionized water and emulsifier sodium dodecyl sulfate into a high-speed mixer, rapidly stirring to enable the emulsifier to be uniformly dissolved, then, uniformly mixing and stirring butyl acrylate, methyl methacrylate, acrylic acid and N-methylol acrylamide, and slowly adding the mixture of the emulsifier and water to form a pre-emulsion; then NaHCO is added 3 Adding the ammonium persulfate into deionized water, continuously stirring to form a buffer solvent aqueous solution, adding the ammonium persulfate into the deionized water, and continuously stirring to form a homogeneous initiator aqueous solution; finally, the pre-emulsion is taken and added into a reactor to be heated to 70 ℃,dripping 1/3 volume of initiator aqueous solution and 1/2 volume of buffer aqueous solution, uniformly adding the solution within 30min, preserving heat until the emulsion is blue, heating to 80 ℃, adding the rest pre-emulsion and the initiator aqueous solution within 3-4h, heating to 90 ℃ and preserving heat for 1h, cooling to 40 ℃, discharging, regulating the pH to be neutral, and filtering to obtain the modified acrylate emulsion.
The preparation method of the flame-retardant polyurethane emulsion comprises the following steps:
firstly, weighing polyether polyol, adding the polyether polyol into a reactor, heating to 60 ℃, then adding isocyanate, uniformly stirring, reacting for 1h at 60 ℃, 70 ℃ and 80 ℃, reacting for 2-3h at constant temperature in nitrogen atmosphere, cooling to 60 ℃, and removing bubbles in vacuum for 30min to obtain polyurethane prepolymer; weighing polyurethane prepolymer, adding trimethylolpropane and flame-retardant reaction monomer, reacting for 30min, and removing bubbles in vacuum for 30min to obtain flame-retardant polyurethane emulsion;
the flame-retardant reaction monomer is 10- (2, 5-dihydroxyphenyl-10-hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide and N, N-bis (hydroxyethyl) aminomethylene diethyl phosphate, and is compounded by (6-oxo-6H-dibenzo [ C, E ] [1,2] oxaphospha-hex-6-yl) hydroxymethyl thiophene according to a molar ratio of 1:1:2.
Example 5
The pressure-sensitive adhesive is prepared by mixing modified acrylic ester emulsion and flame-retardant polyurethane emulsion according to a mass ratio of 3:1.
The preparation methods of the modified acrylic emulsion and the flame-retardant polyurethane emulsion are the same as in example 4.
3. Preparation of release agent
Example 6
The parting agent is prepared from silane modified polyurethane, ethyl acetate, pentaerythritol tetraacrylate and a photoinitiator 1173 according to the mass ratio of 10:2: 2:0.5.
The silane modified polyurethane comprises the following raw materials in parts by weight: 95 parts of 3-isocyanatopropyl triethoxysilane, 12 parts of toluene diisocyanate, 15 parts of pentaerythritol triacrylate, 0.5 part of p-benzoquinone and 5 parts of dibutyltin dilaurate, and the preparation method comprises the following steps:
firstly, putting 3-isocyanatopropyl triethoxysilane into a reactor, heating to 60 ℃, then putting toluene diisocyanate into the reactor, preserving heat and reacting for 5 hours, and using the change condition of isocyanate groups in an infrared analysis system, putting p-benzoquinone into the system after the isocyanate groups are obviously weakened, mixing uniformly, then sequentially putting pentaerythritol triacrylate and dibutyl tin dilaurate, and continuing reacting for 1 hour to obtain silane modified polyurethane.
Example 7
The parting agent is prepared from silane modified polyurethane, ethyl acetate, pentaerythritol tetraacrylate and a photoinitiator 1173 according to the mass ratio of 10:4: 2:0.5.
The silane modified polyurethane comprises the following raw materials in parts by weight: 100 parts of 3-isocyanatopropyl triethoxysilane, 15 parts of toluene diisocyanate, 18 parts of pentaerythritol triacrylate, 0.8 part of p-benzoquinone and 6 parts of dibutyl tin dilaurate, and the preparation method comprises the following steps:
firstly, putting 3-isocyanatopropyl triethoxysilane into a reactor, heating to 65 ℃, then putting toluene diisocyanate into the reactor, preserving heat and reacting for 8 hours, using the change condition of isocyanate groups in an infrared analysis system, putting p-benzoquinone into the system after the isocyanate groups are obviously weakened, mixing uniformly, then sequentially putting pentaerythritol triacrylate and dibutyl tin dilaurate, and continuing reacting for 2 hours to obtain silane modified polyurethane.
Example 8
The parting agent is prepared from silane modified polyurethane, ethyl acetate, pentaerythritol tetraacrylate and a photoinitiator 1173 according to the mass ratio of 10:5: 2:0.5.
The silane modified polyurethane comprises the following raw materials in parts by weight: 105 parts of 3-isocyanatopropyl triethoxysilane, 18 parts of toluene diisocyanate, 20 parts of pentaerythritol triacrylate, 1.2 parts of p-benzoquinone and 8 parts of dibutyl tin dilaurate, and the preparation method comprises the following steps:
firstly, putting 3-isocyanatopropyl triethoxysilane into a reactor, heating to 70 ℃, then putting toluene diisocyanate into the reactor, carrying out heat preservation reaction for 10 hours, using the change condition of isocyanate groups in an infrared analysis system, putting p-benzoquinone into the system after the isocyanate groups are obviously weakened, mixing uniformly, then sequentially putting pentaerythritol triacrylate and dibutyl tin dilaurate, and continuing to react for 3 hours to obtain silane modified polyurethane.
4. Preparation of lithium ion battery termination adhesive tape with corrosion resistance
Example 9
In this example, the substrate layer used the modified polyimide film prepared in example 1, the pressure-sensitive adhesive prepared in example 4, and the release agent prepared in example 6.
The preparation method of the lithium ion battery termination adhesive tape comprises the following steps:
uniformly coating pressure-sensitive adhesive on one side surface of a substrate, and heating for 5min by an oven at 85 ℃ to form an adhesive layer after high-temperature curing; and turning over the substrate, uniformly coating a release agent on the surface of the other side of the substrate, standing for 20min, and placing under a UV light curing machine for light curing to form a release layer. And cooling by using equipment, and then rolling and cutting to obtain the finished product of the lithium ion battery termination adhesive tape.
Example 10
In this example, the substrate layer used the modified polyimide film prepared in example 2, the pressure-sensitive adhesive prepared in example 4, and the release agent prepared in example 7.
The preparation method of the lithium ion battery termination adhesive tape comprises the following steps:
uniformly coating pressure-sensitive adhesive on one side surface of a substrate, and heating for 5min by a 75 ℃ oven to form an adhesive layer after high-temperature curing; and turning over the substrate, uniformly coating a release agent on the surface of the other side of the substrate, standing for 20min, and placing under a UV light curing machine for light curing to form a release layer. And cooling by using equipment, and then rolling and cutting to obtain the finished product of the lithium ion battery termination adhesive tape.
Example 11
In this example, the substrate layer used the modified polyimide film prepared in example 3, the pressure-sensitive adhesive prepared in example 5, and the release agent prepared in example 8.
The preparation method of the lithium ion battery termination adhesive tape comprises the following steps:
uniformly coating pressure-sensitive adhesive on one side surface of a substrate, and heating for 3min by an oven at 85 ℃ to form an adhesive layer after high-temperature curing; and turning over the substrate, uniformly coating a release agent on the surface of the other side of the substrate, standing for 20min, and placing under a UV light curing machine for light curing to form a release layer. And cooling by using equipment, and then rolling and cutting to obtain the finished product of the lithium ion battery termination adhesive tape.
Performance detection
The lithium ion battery termination tapes with corrosion resistance prepared in examples 9-11 were subjected to the following tests:
(1) Mechanical property test
The pressure-sensitive adhesive tape was tested for tensile strength and elongation at break using a universal test stretcher (model: 5969) manufactured by INSTRON corporation. The test environment is room temperature, the sample size is 150mm multiplied by l of sample bars with the length of 5mm, the test effective length is 100mm, and the test speed is 10mm/min; the data obtained are shown in table 1 below:
table 1 mechanical properties test results of lithium ion battery termination tapes with corrosion resistance
，
As can be seen from the above Table 1, the lithium ion battery termination adhesive tape with corrosion resistance has good mechanical properties, the tensile strength can reach 192.94MPa, and the elongation at break can reach 131.08%, because the modified polyimide film is adopted as the base material of the adhesive tape, the organosilicon intercalation sericite is added in the process of synthesizing polyimide from diamine monomers and dianhydride monomers, the 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in the organosilicon intercalation sericite is adopted as the diamine monomers containing a siloxane structure, and the polyimide synthesized from the dianhydride monomers can obtain the copolymer without split phases due to the short chain of siloxane, so that the relative molecular mass of the polymer can not be influenced by adopting the 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane, and the corona resistance and the adhesive performance can be increased, and meanwhile, the mechanical properties can be kept high.
(2) Gas barrier test
Moisture permeability test: cutting a sample film into an area with the size of A4, performing a water vapor permeation test for 24 hours by using a W3/031 water vapor permeation tester, and performing a test according to GB1037 test method-cup method for water vapor permeability of plastic film and sheet; air permeability test: cutting a sample film into an area with the size of A4, performing an oxygen permeation test for 24 hours by using a Classic2016 differential pressure gas permeation meter, and performing the test according to GB1038 "test method for gas permeation of plastic film and sheet-differential pressure method"; the data obtained are shown in table 2 below:
table 2 gas barrier test results of lithium ion battery termination tape with corrosion resistance
，
As can be seen from table 2, the lithium ion battery termination adhesive tape with corrosion resistance has good barrier performance, and the addition of the intercalated sericite benefits from the fact that the direct penetration of gas is blocked, so that the path is tortuous, the diffusion in the transverse direction is increased, the diffusion time is prolonged, and the barrier performance of the termination adhesive tape is improved.
(3) Peel strength and aging resistance
180 DEG peel strength, measured by a peel force tester according to GB/T2792-2014 standard (peel rate 300 mm/min);
ageing resistance, namely placing the adhesive tape for 7d at 50 ℃ for ageing treatment, and calculating the change rate of the peel strength according to a formula:
；
the data obtained are shown in table 3 below:
TABLE 3 test results of peel strength and aging resistance of lithium ion battery termination tape with corrosion resistance
，
As can be seen from the table 3, the lithium ion battery termination adhesive tape with corrosion resistance has stronger peel strength and ageing resistance, the pressure-sensitive adhesive is prepared by mixing modified acrylic ester emulsion and flame-retardant polyurethane emulsion according to the mass ratio of 2-3:1, so that the pressure-sensitive adhesive has higher initial adhesion, wherein the modified acrylic ester emulsion takes butyl acrylate, methyl methacrylate, acrylic acid and N-methylolacrylamide as polymerization monomers, and a semi-continuous emulsion polymerization method is adopted to prepare acrylic ester emulsion, so that the viscosity of the polymerization emulsion is reduced, the cohesive strength of the pressure-sensitive adhesive is improved, and the acrylic ester emulsion pressure-sensitive adhesive with good emulsion stability and excellent adhesive strength is prepared; meanwhile, the reaction type flame-retardant polyurethane emulsion synthesized by adopting the polyurethane prepolymer and the compound flame-retardant reaction monomer contains P, N two elements, which not only can generate acidic substances to promote the dehydration and the char formation of the base material, but also can generate NO 2 The oxygen concentration in the non-combustible gas dilution combustion environment plays a role in inhibiting combustion, and the reactive flame retardant does not influence the adhesive force of the pressure-sensitive adhesive.
(5) Heat and corrosion resistance
The adhesive tape was stuck on a stainless steel plate, baked in a oven at a constant temperature of 100℃and 120℃and 140℃for 2 hours, and peeled off in the oven (hot peeling). And observing whether residual glue marks exist on the stainless steel plate. The strip DG2161 is stuck on an aluminum foil, soaked in lithium battery electrolyte, placed for 3d at 80 ℃, cooled to room temperature, taken out of the aluminum foil to observe whether the adhesive tape has the phenomenon of tilting and falling off, stripped off and observed whether the adhesive surface is dissolved or not, and the adhesive residue is left on the aluminum foil. The data obtained are shown in table 4 below.
Table 4 test results of electrolyte resistance of lithium ion battery termination tape with corrosion resistance
，
As can be seen from the above Table 4, the lithium ion battery termination adhesive tape with corrosion resistance has stronger heat resistance and corrosion resistance, because the adhesive tape base material adopted by the invention is a modified polyimide film, on one hand, the adhesive tape base material has high and low temperature resistance, ultraviolet radiation resistance, chemical solvent corrosion resistance and high insulation performance due to the rigid structure comprising an imide ring, an aromatic ring and the like, and on the other hand, the corona resistance and the barrier performance of the film are improved through the modification of the organosilicon intercalated sericite, so that the corrosion of electrolyte and the impact of high-frequency power electronics are prevented, and the corrosion resistance of the adhesive tape is improved.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.
Claims (5)
1. The lithium ion battery termination adhesive tape with corrosion resistance is characterized by comprising a substrate layer, a release layer and a pressure-sensitive adhesive layer, wherein the release layer and the pressure-sensitive adhesive layer are respectively arranged on two sides of the substrate layer, the substrate layer is a modified polyimide film, and the preparation method of the lithium ion battery termination adhesive tape comprises the following steps:
s1, adding intercalated sericite in the process of synthesizing polyimide by using diamine monomers and dianhydride monomers to prepare a modified polyimide film, so as to obtain a tape substrate;
the preparation method of the modified polyimide film comprises the following steps:
(1) Dissolving 4,4 '-diaminodiphenyl ether and 4,4' -diaminodiphenyl sulfide in N, N-dimethylacetamide, and stirring in an oil bath at 40 ℃ for 40-80min;
(2) Adding intercalated sericite into N, N-dimethylacetamide, performing ultrasonic treatment for 10-30min to obtain an intercalated sericite dispersion liquid, adding the intercalated sericite dispersion liquid into the reaction system of the step (1), adding pyromellitic anhydride, and stirring in an oil bath at 40 ℃ for 8-12h to obtain a mixed solution of polyamide acid and inorganic particles;
(3) Uniformly coating the mixed solution obtained in the step (2) on a substrate after defoaming, and then sending the substrate into an oven for step-heating thermal imidization treatment for 5-8 hours to obtain the modified polyimide film;
the preparation method of the intercalated sericite comprises the following steps:
A. placing sericite into a muffle furnace, firstly heating to 200 ℃ at a speed of 5 ℃/min, then heating to 800 ℃ at a speed of 10 ℃/min, and then preserving heat for 1-3h to obtain activated sericite;
B. adding activated sericite into nitric acid with the concentration of 5mol/L according to the solid-to-liquid ratio of 2-4%, stirring and reacting for 4-6 hours at the temperature of 90-95 ℃, and filtering and washing for several times to obtain acidified sericite;
C. adding the acidified sericite into a sodium chloride saturated solution according to a solid-to-liquid ratio of 2-4%, stirring and reacting for 4-6 hours at 90-95 ℃, and filtering and washing for several times to obtain the sodium sericite;
D. dissolving 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane in toluene, adding sodium sericite into 1, 3-bis (3-aminopropyl) -1, 3-tetramethyl disiloxane solution according to a solid-to-liquid ratio of 3-5%, performing ultrasonic treatment at 75-85 ℃ for 30-90min, and performing suction filtration and washing for several times to obtain intercalated sericite;
s2, uniformly coating the pressure-sensitive adhesive on one side surface of the substrate, and heating for 3-5min by an oven at 75-85 ℃ to form a pressure-sensitive adhesive layer after high-temperature curing;
the pressure-sensitive adhesive is prepared by mixing modified acrylic ester emulsion and flame-retardant polyurethane emulsion according to the mass ratio of 2-3:1;
the preparation method of the modified acrylic ester emulsion comprises the following steps:
firstly, adding deionized water and emulsifier sodium dodecyl sulfate into a high-speed mixer, rapidly stirring to enable the emulsifier to be uniformly dissolved, then, uniformly mixing and stirring butyl acrylate, methyl methacrylate, acrylic acid and N-methylol acrylamide, and slowly adding the mixture of the emulsifier and water to form a pre-emulsion; then NaHCO is added 3 Adding the ammonium persulfate into deionized water, continuously stirring to form a buffer solvent aqueous solution, adding the ammonium persulfate into the deionized water, and continuously stirring to form a homogeneous initiator aqueous solution; finally, adding the pre-emulsion into a reactor, heating to 70 ℃, dripping 1/3 volume of initiator aqueous solution and 1/2 buffer aqueous solution, uniformly adding the mixture within 30min, preserving heat until the emulsion is blue, heating to 80 ℃, adding the rest pre-emulsion and the initiator aqueous solution within 3-4h, heating to 90 ℃ and preserving heat for 1h, cooling to 40 ℃, discharging, adjusting pH to be neutral, and filtering to obtain modified acrylate emulsion;
the preparation method of the flame-retardant polyurethane emulsion comprises the following steps:
firstly, weighing polyether polyol, adding the polyether polyol into a reactor, heating to 60 ℃, then adding isocyanate, uniformly stirring, reacting for 1h at 60 ℃, 70 ℃ and 80 ℃, reacting for 2-3h at constant temperature in nitrogen atmosphere, cooling to 60 ℃, and removing bubbles in vacuum for 30min to obtain polyurethane prepolymer; weighing polyurethane prepolymer, adding trimethylolpropane and flame-retardant reaction monomer, reacting for 30min, and removing bubbles in vacuum for 30min to obtain flame-retardant polyurethane emulsion;
the flame-retardant reaction monomer is 10- (2, 5-dihydroxyphenyl) -10 hydrogen-9-oxa-10-phosphaphenanthrene-10-oxide, and is prepared by compounding (6-oxo-6H-dibenzo [ C, E ] [1,2] oxaphospha-hex-6-yl) hydroxymethyl thiophene according to a molar ratio of 1:1:2;
s3, turning over the substrate, uniformly coating a release agent on the surface of the other side of the substrate, standing for 20min, and placing under a UV (ultraviolet) light curing machine for light curing to form a release layer;
and S4, cooling by using equipment, rolling and cutting to obtain the finished product of the lithium ion battery termination adhesive tape.
2. The lithium ion battery termination adhesive tape with corrosion resistance according to claim 1, wherein the modified polyimide film comprises the following raw materials in parts by weight: 25-30 parts of 4,4 '-diaminodiphenyl ether, 15-20 parts of 4,4' -diaminodiphenyl sulfide, 40-50 parts of pyromellitic anhydride and 5-10 parts of intercalated sericite.
3. The lithium ion battery terminal adhesive tape with corrosion resistance according to claim 1, wherein the step-up thermal imidization treatment in the step (3) is specifically: heating at 50-70deg.C, and maintaining for 1-3 hr after temperature stabilization; heating at 110-130deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization; heating at 190-210 deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization; heating at 240-260 deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization; heating at 310-330 deg.C, and maintaining for 0.5-1.5 hr after temperature stabilization.
4. The lithium ion battery termination adhesive tape with corrosion resistance according to claim 1, wherein the release agent comprises silane modified polyurethane, ethyl acetate, pentaerythritol tetraacrylate and a photoinitiator 1173 in a mass ratio of 10:2-5: 2:0.5.
5. The lithium ion battery termination adhesive tape with corrosion resistance according to claim 4, wherein the silane modified polyurethane comprises the following raw materials in parts by weight: 95-105 parts of 3-isocyanatopropyl triethoxysilane, 12-18 parts of toluene diisocyanate, 15-20 parts of pentaerythritol triacrylate, 0.5-1.2 parts of p-benzoquinone and 5-8 parts of dibutyltin dilaurate, and the preparation method comprises the following steps:
firstly, putting 3-isocyanatopropyl triethoxysilane into a reactor, heating to 60-70 ℃, then putting toluene diisocyanate into the reactor, carrying out heat preservation reaction for 5-10h, using the change condition of isocyanate groups in an infrared analysis system, putting p-benzoquinone into the system after the isocyanate groups are obviously weakened, mixing uniformly, then sequentially putting pentaerythritol triacrylate and dibutyltin dilaurate, and continuing to react for 1-3h to obtain silane modified polyurethane.
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