CN109353691B - Lithium ion battery flexible packaging material and inner layer adhesive thereof - Google Patents
Lithium ion battery flexible packaging material and inner layer adhesive thereof Download PDFInfo
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- CN109353691B CN109353691B CN201811046935.8A CN201811046935A CN109353691B CN 109353691 B CN109353691 B CN 109353691B CN 201811046935 A CN201811046935 A CN 201811046935A CN 109353691 B CN109353691 B CN 109353691B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/40—Applications of laminates for particular packaging purposes
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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
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/26—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers modified by chemical after-treatment
Abstract
The invention discloses a lithium ion battery flexible packaging material and an inner layer adhesive thereof, wherein the inner layer adhesive is a two-component curing system and mainly comprises acid modified polyisobutylene and epoxy resin. The adhesive can greatly improve the bonding property between the aluminum foil and the CPP, is particularly suitable for being used as an inner layer adhesive for an aluminum-plastic film, and has excellent electrolyte corrosion resistance, heat resistance and sealing property. The inner-layer adhesive can obviously enhance the bonding property, the heat resistance and the electrolyte resistance of the aluminum plastic film, and provides a packaging material of a soft package lithium battery.
Description
Technical Field
The invention relates to the technical field of lithium ion battery flexible packaging, in particular to a lithium ion battery flexible packaging material and an inner layer adhesive thereof.
Background
In recent years, the demand of lithium ion batteries is continuously increasing with the development of new energy automobiles, 3C digital products and micro electronic technologies. As an important component of the lithium ion battery, the aluminum plastic film mainly plays a role in packaging electrolyte and protecting the battery, and the cost of the aluminum plastic film accounts for about 15% -20% of the whole lithium battery core. However, due to technical barriers, the aluminum plastic film market in China is almost monopolized by manufacturers in Japan and Korea.
The aluminum plastic film is a composite material film and mainly comprises an outer layer (a nylon layer), an outer adhesive layer (an outer adhesive layer), an aluminum foil layer, an inner adhesive layer (an inner adhesive layer) and a heat sealing layer (a CPP layer). The development of the inner layer glue is always the biggest problem of localization of the aluminum-plastic film. The inner glue layer is close to the electrolyte inside the battery, so that the inner glue layer needs to have excellent electrolyte corrosion resistance, heat resistance and air tightness. At present, the inner layer glue of the domestic aluminum plastic film needs to be imported from Japan or Korea, and the domestic inner layer glue can not simultaneously meet all the performances, so that the development of the novel inner layer glue for the aluminum plastic film is used for solving the problem.
Disclosure of Invention
The invention aims to provide a lithium ion battery flexible packaging material and an inner layer adhesive thereof aiming at the defects of the prior art, wherein the inner layer adhesive can obviously enhance the bonding property, the heat resistance and the electrolyte resistance of an aluminum plastic film.
The inner layer adhesive for the aluminum plastic film is composed of an agent A and an agent B, wherein the agent A is 20-100g/L of anhydride modified polyisobutylene powder, the agent B is epoxy resin, and the epoxy equivalent is 150-250.
The mass fraction ratio of the anhydride modified polyisobutene is as follows:
the acid anhydride is one or more of phthalic anhydride and maleic anhydride.
The initiator is one or more of azodiisobutyronitrile and dicumyl peroxide.
the antioxidant is tetra [ β - (3, 5-di-tert-butyl 4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
The epoxy resin is one or more of bisphenol A and bisphenol F.
The presence of two substituted methyl groups in the polyisobutene leads to slow molecular chain movement and a small free volume. And thus its diffusion coefficient and gas permeability are low, so that the polyisobutylene has excellent airtightness. More importantly, the polyisobutylene has excellent chemical resistance and can resist the corrosion of 60 percent concentration hydrofluoric acid. Therefore, the invention takes the polyisobutylene as a matrix, uses the anhydride chemical substance to modify the polyisobutylene to enable the polyisobutylene to have the capability of crosslinking polymerization, and uses the epoxy resin as a curing agent to crosslink and modify the anhydride groups on the polyisobutylene to obtain the final inner-layer adhesive for the soft package of the lithium battery.
The use method of the agent A/the agent B is as follows:
dissolving 5-50g of the agent A in 200-400g of a cyclohexane solvent at the dissolving temperature of 50-100 ℃, then adding 1-30g of the agent B into the agent A, fully stirring to obtain an inner layer adhesive for the aluminum-plastic film, coating the inner layer adhesive on the surface of an aluminum foil treated by a trivalent chromium agent, controlling the thickness of a dry film of the adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive layer and a CPP film through hot pressing at the hot pressing temperature of 50-100 ℃, and curing in an oven at the temperature of 50-80 ℃ for 4-7 days to prepare a semi-finished product of the aluminum-plastic film. The ratio of the agent A to the agent B is controlled to be 2-10: 1, the total solid content of the inner layer glue is controlled between 10 percent and 30 percent.
The flexible packaging material for the lithium battery is a six-layer composite film structure layer, and the structure of the flexible packaging material for the lithium battery is sequentially provided with an outer layer, an outer bonding layer, a chromium treatment layer, an aluminum foil layer, an inner bonding layer and a CPP layer from outside to inside.
The outer layer is a biaxially oriented nylon layer with a thickness of 15-25 μm.
The outer bonding layer is polyurethane adhesive, and the thickness of the outer adhesive is 2-5 mu m.
The chromium treatment layer can be an existing hexavalent chromium treatment layer, is preferably a trivalent chromium treatment layer, is obtained by compounding trivalent chromium and high polymer resin, has the thickness of 200-1000 nm, and contains groups capable of reacting with epoxy groups, such as hydroxyl, amino, acid anhydride and the like on the surface of the trivalent chromium coating.
The inner layer adhesive is a compound system of modified polyisobutylene and an epoxy resin curing agent. Anhydride groups contained in the polyisobutylene adhesive can generate a crosslinking reaction with hydroxyl amino and epoxy groups in the trivalent chromium medicament, so that the adhesive force of the trivalent chromium coating and the inner layer adhesive is greatly enhanced. The CPP is polypropylene with a multilayer composite film structure, and the outer layer of the CPP is polypropylene modified by maleic anhydride, so that the side where the inner layer adhesive is connected with the CPP is high molecular polymer modified by the maleic anhydride, and the two types of the CPP can be bonded by melting under the hot pressing condition according to the similar compatibility principle; meanwhile, an epoxy group contained in the curing agent in the inner layer adhesive can perform a crosslinking reaction with the maleic anhydride modified polypropylene layer of the CPP outer layer to form a tight occlusion structure, so that the adhesive can enable the CPP and the aluminum foil to form a tight integrated structure.
Foretell CPP layer is two-layer complex film structure, and its and inlayer gluing agent laminating one side is maleic anhydride modified polypropylene, and one side is curtain coating polypropylene in addition.
Advantageous effects
By adopting the technical scheme, the invention provides the high-molecular adhesive compounded by the anhydride modified polyisobutylene and the epoxy resin, and the adhesive has excellent electrolyte corrosion resistance, adhesive property and sealing property, is particularly suitable for the aluminum plastic film for the lithium battery, and makes up the current situation that the inner layer adhesive for the aluminum plastic film is deficient in China.
Drawings
Fig. 1 is a schematic structural diagram of the flexible packaging material (aluminum-plastic film) of the lithium ion battery.
The following description is made with reference to the accompanying drawings:
1 is the skin, 2 outer gluey tie coats, and 3 are trivalent chromium processing layers, and 4 are the aluminium foil layer, and 5 are trivalent chromium processing layers, and 6 are inlayer gluey tie coats, and 7 are the CPP layer.
Detailed Description
Example 1
Dissolving 30g A agent in 402g cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 5g B agent, fully stirring to obtain inner layer adhesive with solid content of 8%, uniformly coating the adhesive on the surface of an aluminum foil, controlling the thickness of dry adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to prepare an aluminum-plastic film semi-finished product, then hot pressing nylon and the aluminum-plastic film semi-finished product by a polyurethane outer layer adhesive at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Example 2
Dissolving 30g A agent in 257g cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 5g B agent, fully stirring to obtain inner layer adhesive with the solid content of 12%, uniformly coating the adhesive on the surface of an aluminum foil, controlling the thickness of dry adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to prepare an aluminum-plastic film semi-finished product, then hot pressing nylon and the aluminum-plastic film semi-finished product by outer layer adhesive purchased from the market at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Example 3
Dissolving 30g A agent in 198g cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 5g of B agent, fully stirring to obtain 15% solid content inner layer adhesive, uniformly coating the adhesive on the surface of an aluminum foil, controlling the thickness of dry adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to prepare an aluminum-plastic film semi-finished product, then hot pressing nylon and the aluminum-plastic film semi-finished product by using commercially available outer layer adhesive at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Example 4
Dissolving 30g A agent in 159g of cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 5g of B agent, fully stirring to obtain 18% solid content inner layer adhesive, uniformly coating the adhesive on the surface of an aluminum foil, controlling the thickness of dry adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to prepare an aluminum-plastic film semi-finished product, then hot pressing the nylon and the aluminum-plastic film semi-finished product by using commercially available outer layer adhesive at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Example 5
Dissolving 30g A agent in 140g cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 5g B agent, fully stirring to obtain 20% solid content inner layer adhesive, uniformly coating the adhesive on the surface of an aluminum foil, controlling the thickness of dry adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to prepare an aluminum-plastic film semi-finished product, then hot pressing the nylon and the aluminum-plastic film semi-finished product by using commercially available outer layer adhesive at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Example 6
Dissolving 29.2g A in 198g of cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 5.8g B agents, fully stirring to obtain inner layer glue, uniformly coating the glue on the surface of an aluminum foil, controlling the thickness of dry glue to be 4 mu m, compounding the aluminum foil coated with the glue and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to obtain an aluminum-plastic film semi-finished product, then hot pressing the nylon and the aluminum-plastic film semi-finished product by outer layer glue purchased from the market at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Example 7
Dissolving 30.7g A in 230g of cyclohexane, stirring and dissolving in a 80 ℃ micro-reaction kettle, then adding 4.3g B agents, fully stirring to obtain inner layer glue, uniformly coating the glue on the surface of an aluminum foil, controlling the thickness of dry glue to be 4 mu m, compounding the aluminum foil coated with the glue and CPP by a hot pressing method at the hot pressing temperature of 100 ℃ to obtain an aluminum-plastic film semi-finished product, then hot pressing the nylon and the aluminum-plastic film semi-finished product by outer layer glue purchased from the market at the hot pressing temperature of 80 ℃, and curing in a 70 ℃ oven for 7 days.
The cured aluminum-plastic film was cut into a sample strip having a width of 15mm, the sample strip was subjected to a peel strength test with reference to the standard ASTM 254, the test was repeated five times or more, and the corresponding average value was recorded.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Comparative example 1
Preparing inner layer glue SD-TZ sold in Nippon chestnut village company, uniformly coating the glue on the surface of an aluminum foil, controlling the thickness of dry glue to be 4 mu m, compounding the aluminum foil coated with the glue and CPP by a hot pressing method, wherein the hot pressing temperature is 70 ℃, and curing the aluminum foil in a 70 ℃ oven for 7 days to prepare the semi-finished product of the aluminum-plastic film.
And cutting the cured semi-finished product of the aluminum-plastic film into a sample strip with the width of 15mm, testing the peel strength of the sample strip according to the standard ASTM 254, repeatedly testing for more than five times, and recording the corresponding average value.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
Comparative example 2
Preparing inner layer adhesive VK112 of a commercially available Toyobo Co, uniformly coating the adhesive on the surface of an aluminum foil, controlling the thickness of a dry adhesive to be 4 mu m, compounding the aluminum foil coated with the adhesive and CPP by a hot pressing method at the hot pressing temperature of 70 ℃, and curing in an oven at the temperature of 70 ℃ for 7 days to prepare the semi-finished product of the aluminum-plastic film.
And cutting the cured semi-finished product of the aluminum-plastic film into a sample strip with the width of 15mm, testing the peel strength of the sample strip according to the standard ASTM 254, repeatedly testing for more than five times, and recording the corresponding average value.
The cured aluminum-plastic film specimens were placed in an electrolyte environment at 85 ℃ and tested for peel strength every 1, 3, 5, 7 days, with reference to standard ASTM 254, and the test was repeated five times or more and the corresponding average value was recorded.
The initial tensile force and the tensile force after electrolyte immersion for the above examples and comparative examples are shown in Table 2:
table 2: adhesion of the samples of each example to the control
Experiments show that when the solid content of the inner layer adhesive exceeds 18%, the viscosity of the AB adhesive is high, and the AB adhesive is not suitable for coating aluminum foil by a precision coating machine in a factory. When the solid content of the inner layer adhesive is lower than 8%, the strength between the aluminum foil and the CPP is lower, and the performance requirement of the aluminum-plastic film cannot be met.
From Table 1, the balance of properties of the aluminum plastic film sample strip of example 3 is the best, the solid content is 15%, and A: b is 5: the 1-time AB glue is most suitable for a lithium battery flexible packaging film. The performance of the AB adhesive exceeds the bonding strength of aluminum foil and CPP required by the domestic aluminum plastic film manufacturers for lithium batteries, and the bonding strength of the aluminum foil and the CPP is 6N/15mm after the sample strips are soaked in electrolyte for one day. The performance is even slightly better than that of the commercial Japanese product.
Claims (3)
1. An inner layer adhesive of a lithium ion battery flexible packaging material is characterized by being a two-component curing system and mainly comprising an agent A and an agent B; the agent A is 20-100g/L of anhydride modified polyisobutylene powder, the agent B is epoxy resin, and the epoxy equivalent is 150-250; the total solid content of the inner layer adhesive is controlled to be 12-18%, and the mass fraction ratio of the anhydride modified polyisobutylene resin is as follows:
the epoxy resin comprises a main component, an auxiliary component and an auxiliary component, wherein the acid anhydride is one or more of phthalic anhydride and maleic anhydride, the initiator is one or more of azobisisobutyronitrile and dicumyl peroxide, the antioxidant is tetra [ β - (3, 5-di-tert-butyl 4-hydroxyphenyl) propionic acid ] pentaerythritol ester, and the epoxy resin is one or more of bisphenol A and bisphenol F.
2. The inner layer adhesive of the lithium ion battery flexible packaging material as claimed in claim 1, wherein the curing temperature of the inner layer adhesive is 50-80 ℃, and the curing time is 4-7 days.
3. A soft packaging material for a lithium ion battery comprises an outer layer, an outer layer bonding layer, a chromium treatment layer, an aluminum foil layer, a chromium treatment layer, an inner layer bonding layer and a CPP layer from outside to inside in sequence, and is characterized in that the inner layer bonding layer adopts the inner layer adhesive as defined in any one of claims 1 to 2.
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CN111157446B (en) * | 2019-12-31 | 2023-01-31 | 安普瑞斯(南京)有限公司 | Method and device for testing tensile stress change trend of aluminum plastic film based on gradual change |
CN111440593B (en) * | 2020-04-07 | 2021-01-15 | 郑州卓而泰新材料科技有限公司 | Lithium battery aluminum plastic film inner layer adhesive and preparation method thereof |
CN114163938B (en) * | 2021-12-08 | 2023-09-15 | 烟台德邦科技股份有限公司 | Base material-free hot melt adhesive film for soft package lithium battery and preparation method and application thereof |
CN115074056B (en) * | 2022-06-29 | 2023-03-21 | 惠州市广麟材耀科技有限公司 | Aluminum-plastic film inner layer adhesive for lithium battery packaging and preparation method thereof |
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