CN108630837A - It is a kind of to be used to pack aluminum-plastic composite membrane of lithium ion battery and preparation method thereof - Google Patents

It is a kind of to be used to pack aluminum-plastic composite membrane of lithium ion battery and preparation method thereof Download PDF

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CN108630837A
CN108630837A CN201810397895.5A CN201810397895A CN108630837A CN 108630837 A CN108630837 A CN 108630837A CN 201810397895 A CN201810397895 A CN 201810397895A CN 108630837 A CN108630837 A CN 108630837A
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段国凡
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Du Haimei
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Wuhu Sheng Innovation Mstar Technology Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/10—Primary casings; Jackets or wrappings
    • H01M50/116—Primary casings; Jackets or wrappings characterised by the material
    • H01M50/124—Primary casings; Jackets or wrappings characterised by the material having a layered structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
    • B32B27/285—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08F2/00—Processes of polymerisation
    • C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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    • C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
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    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/04—Polyurethanes
    • C09J175/06—Polyurethanes from polyesters
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/22—Light metals
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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    • B32B2307/70—Other properties
    • B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B2307/70—Other properties
    • B32B2307/726—Permeability to liquids, absorption
    • B32B2307/7265—Non-permeable
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2553/00—Packaging equipment or accessories not otherwise provided for
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C08J2371/02—Polyalkylene oxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
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    • C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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    • C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

The invention discloses a kind of aluminum-plastic composite membranes for packing lithium ion battery, it is modified aluminium foil layer including surface, the surface, which is modified on the inner surface of aluminium foil layer, is provided with modified heat-sealing film layer, the modification seals film layer and is fixedly connected with surface modification aluminium foil layer by modified binder, and modified heat-sealing film includes following raw material：Vinyl acetate, the tert-butyl alcohol, vinyl monomer, 6 tert-butyl-m-cresols, polyoxyethylene laurate, phthalic acid two (2 ethyl hexyl) ester, m-xylene diamine, adipic acid, polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and carborundum double substrate material, nano cupric oxide, modified binder include following raw material：Hydroxyl telechelic polyester component, terminal isocyanate group component, bisphenol A type epoxy resin E44, phenolic resin, graphite powder, silica flour.The present invention also provides a kind of preparation methods for packing the aluminum-plastic composite membrane of lithium ion battery.The aluminum-plastic composite membrane of the present invention considerably improves the peel strength between internal layer and secondary internal layer.

Description

It is a kind of to be used to pack aluminum-plastic composite membrane of lithium ion battery and preparation method thereof
Technical field
The present invention relates to new material technology field, specially a kind of aluminum-plastic composite membrane for packing lithium ion battery and its Preparation method.
Background technology
New material refers to some newly-developed or researching and developing, having preeminent performance materials, is had more than traditional material For excellent performance.In recent years, new material is increasingly paid attention to, and country also payes attention to new material industry development.
New material technology is then the will according to people, passes through physical study, design of material, material processing, test evaluation etc. A series of research process create the technology for the new material that can meet various needs.
Aluminum-plastic composite membrane is mainly used in the packaging of lithium ion battery as a kind of new material, and still, existing plastic-aluminum is multiple Film is closed in the presence of since the adhesive property of binder is poor, making aluminium foil layer and the peel strength sealed between film layer relatively low, leads to heat Sealer layer is easy the technical issues of being detached from from the surface of aluminium foil layer.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides it is a kind of for pack lithium ion battery aluminum-plastic composite membrane and its Preparation method has and improves the advantages that peel strength is with corrosion resistance is improved, solves existing aluminum-plastic composite membrane, due to viscous The adhesive property for tying agent is poor, keeps aluminium foil layer and the peel strength sealed between film layer relatively low, and heat-sealing film layer is caused to be easy from aluminium The technical issues of surface of layers of foil is detached from.
(2) technical solution
For the purpose realized above-mentioned raising peel strength with improve corrosion resistance, the present invention provides the following technical solutions：
A kind of aluminum-plastic composite membrane for packing lithium ion battery, including surface are modified aluminium foil layer, the surface modified aluminium Modified heat-sealing film layer is provided on the inner surface of layers of foil, which seals film layer and be modified aluminium foil by modified binder and surface Layer is fixedly connected；
The surface is modified the raw material that aluminium foil includes following parts by weight proportioning：20-30 parts of citric acid, deionized water 20- 30 parts, 5-8 parts of sodium hydroxide, 2-3 parts of sodium metasilicate, N, 10-12 parts of N- double hydroxyethyls coconut oleamide, acid dimethyl sodium 8-10 parts；
The modified heat-sealing film includes the raw material of following parts by weight proportioning：10-20 parts of vinyl acetate, tert-butyl alcohol 20- 30 parts, 2-5 parts of vinyl monomer, 1-2 parts of sodium hydroxide, 0.5-1 parts of perbenzoic acid, 0.1-0.5 parts of 6- tert-butyl-m-cresols, 0.01-0.05 parts of polyoxyethylene laurate, 2-5 parts of phthalic acid two (2- ethyl hexyls) ester, 35-50 parts of methanol, hydroxide 5-8 parts of sodium, 65-80 parts of ultra-pure water, 20-30 parts of acetone, 8-10 parts of m-xylene diamine, 20-30 parts of polyethylene glycol, adipic acid 10- 5-8 parts of 15 parts, 10-15 parts of polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and carborundum double substrate material, 5-8 parts of nano cupric oxide, carbon 0.05-0.1 parts of sour hydrogen sodium；
The modified binder includes the raw material of following parts by weight proportioning：9-12 parts of hydroxyl telechelic polyester component, end isocyanide 1-2 parts of perester radical component, 2-3 parts of bisphenol A type epoxy resin E44,8-10 parts of ethyl acetate, 2-5 parts of phenolic resin, anhydrous second 35-40 parts of alcohol, 3-6 parts of ethylenediamine, 10-15 parts of deionized water, 5-10 parts of phenol, 2-4 parts of graphite powder, 2-3 parts of silica flour；
The peel strength of the aluminum-plastic composite membrane is 14.9-16.3N/m.
Preferably, the peel strength of the aluminum-plastic composite membrane is 16.3N/m.
Preferably, the surface is modified the raw material that aluminium foil includes following parts by weight proportioning：25 parts of citric acid, deionized water 25 parts, 6 parts of sodium hydroxide, 2.5 parts of sodium metasilicate, N, 11 parts of N- double hydroxyethyl coconuts oleamide, 9 parts of acid dimethyl sodium.
Preferably, the modified heat-sealing film includes the raw material of following parts by weight proportioning：15 parts of vinyl acetate, the tert-butyl alcohol 25 parts, 4 parts of vinyl monomer, 1.5 parts of sodium hydroxide, 0.8 part of perbenzoic acid, 0.3 part of 6- tert-butyl-m-cresols, polyoxyethylene 0.03 part of laurate, 3 parts of phthalic acid two (2- ethyl hexyls) ester, 41 parts of methanol, 6 parts of sodium hydroxide, 80 parts of ultra-pure water, third 25 parts of ketone, 9 parts of m-xylene diamine, 25 parts of polyethylene glycol, 12 parts of adipic acid, 12 parts of polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and charcoal 7 parts of SiClx double substrate material, 6 parts of nano cupric oxide, 0.08 part of sodium bicarbonate.
Preferably, the modified binder includes the raw material of following parts by weight proportioning：10 parts of hydroxyl telechelic polyester component, end 1.5 parts of isocyanate group component, 2.5 parts of bisphenol A type epoxy resin E44,9 parts of ethyl acetate, 3 parts of phenolic resin, absolute ethyl alcohol 38 parts, 5 parts of ethylenediamine, 12 parts of deionized water, 8 parts of phenol, 3 parts of graphite powder, 2.5 parts of silica flour.
Another technical problem to be solved by the present invention is that providing a kind of for packing the aluminum-plastic composite membrane of lithium ion battery Preparation method includes the following steps：
1) preparation of modified heat-sealing film
(1) vinyl acetate of 10-20 mass parts is added in the t-butanol solvent of 20-30 mass parts, is stirred , the vinyl monomer for adding 2-5 mass parts after being uniformly mixed, is subsequently added into sodium hydroxide, the 0.5-1 of 1-2 mass parts The polyoxyethylene of the perbenzoic acid of mass parts, the 6- tert-butyl-m-cresols of 0.1-0.5 mass parts, 0.01-0.05 mass parts Phthalic acid two (2- ethyl hexyls) ester of laurate, 2-5 mass parts occurs at pressure 4-5MPa, 80-90 DEG C of temperature Vinyl-vinyl acetate copolymer is made in free radicals copolymerization reaction；
(2) vinyl-vinyl acetate copolymer obtained in step (1) is added to the methanol solvate of 30-40 mass parts In, the sodium hydroxide alkali catalyst of 5-8 mass parts is added, under nitrogen protection, being heated with stirring in system has methanol steaming Steam distillation goes out, and the methanol of 5-8 mass parts is added in reaction process, is uniformly carried out with keeping reacting, reacts 5-6h, be cooled to room temperature, By the way that at hydroxyl, EVOH copolymers are made in the acetyl group alcoholysis in vinyl-vinyl acetate copolymer；
(3) EVOH copolymers made from the milli-Q water step (3) of 50-60 mass parts are used, it is water-soluble to remove sodium acetate etc. Property impurity remove the oil-soluble impurities such as methyl acetate then with 12-14h is extracted in the acetone of 20-30 mass parts, EVOH is made Component；
(4) m-xylene diamine of 8-10 mass parts is added in reaction kettle, is subsequently added into the ultrapure of 15-20 mass parts Water adds the polyethylene glycol of 20-30 mass parts, is uniformly mixed, and the adipic acid of 10-15 mass parts is then added, in nitrogen It under the protection of gas atmosphere, is stirred, keeps reaction temperature at 50 DEG C hereinafter, adding the polytetrafluoro of 10-15 mass parts The nano cupric oxide of ethylene, the carbon fiber reinforced carbon of 5-8 mass parts and carborundum double substrate material and 5-8 mass parts, stirring are mixed It closes uniformly, when reaction temperature no longer changes, the sodium bicarbonate that 0.05-0.1 mass parts are added is added, and is uniformly mixed, and adjusts Acid-base value is saved to 7.0-7.5, reaction terminates, and crystallinity nylon resin component is made；
(5) crystallinity nylon resin made from EVOH components made from step (3) and step (4) is added to batch mixer, The blender of batch mixer is opened, mixing speed 550-600r/min, mixing time 30-60min obtain mixture；
(6) mixture made from step (5) is put into calender, the calendered film come out from calender bottom roller passes through successively Cross first group deflect from roller, second group deflect from roller and third group deflects from roller, first group of channel temperature for deflecting from roller is 20-30 DEG C, the Two groups deflect from roller and third group to deflect from the channel temperature of roller be 140-150 DEG C, calendered film is using first group of chill roll, second Group chill roll and the cooling of third group chill roll, the temperature of first group of chill roll is 70-75 DEG C, and the temperature of second group of chill roll is 60-65 DEG C, the temperature of third group chill roll is 50-55 DEG C, and trimming and volume area are carried out after cooling, obtains modified heat-sealing film；
2) preparation of modified binder
(1) the hydroxyl telechelic polyester component of 9-12 mass parts and the terminal isocyanate group component mixed preparing of 1-2 mass parts are taken Obtain polyurethane adhesive component；Then take the bisphenol A type epoxy resin E44 of 2-3 mass parts spare；
(2) in N2Under protection, using the ethyl acetate of 8-10 mass parts to the bisphenol A type epoxy resin E44 of 2-3 mass parts It is dissolved, solution temperature is 50-60 DEG C, and epoxy resin E44 is made；
(3) epoxy resin E44 obtained is added to step (1) prepared polyurethane adhesive after dissolving step (2) In, it is thoroughly mixed uniformly, binder is made；
(4) phenolic resin for taking 2-5 mass parts is added in the absolute ethyl alcohol of 8-10 mass parts, stirs evenly；
(5) ethylenediamine for taking 3-6 mass parts is added in the deionized water of 10-15 mass parts, stirs evenly, with step (4) phenolic aldehyde ethanol solution made from mixes, and stirs evenly, and binder made from step (3) is added, and ultrasonic 30-60min distills, Absolute ethyl alcohol is removed, adhesive aid is obtained；
(6) phenol of 5-10 mass parts is added in the absolute ethyl alcohol of 25-30 mass parts, is uniformly mixed, slowly It is 50-60 DEG C, insulated and stirred 50-60min to increase temperature, is subsequently added into the quartz of the graphite powder and 2-3 mass parts of 2-4 mass parts Powder continues insulated and stirred 30-40min, and adhesive aid obtained in step (5) is then added, and it is 80-90 DEG C to increase temperature, is protected Temperature stirring 20-30 minutes, is cooled to room temperature, obtains modified binder；
3) surface is modified the preparation of aluminium foil
(1) citric acid of 20-30 mass parts is added in the deionized water of 20-30 mass parts, is being stirred, slowly Be added 5-8 mass parts sodium hydroxide, after being stirred, then add the sodium metasilicate of 2-3 mass parts, 10-12 mass parts N, The acid dimethyl sodium of N- double hydroxyethyl coconut oleamides and 8-10 mass parts, is uniformly mixed, and degreaser is made；
(2) soft aluminium foil is immersed in degreaser made from step (1) and impregnates 80-100min, removed on aluminium foil surface Grease impurities；
(3) aluminium foil after step (2) oil removing is placed in vacuum drying chamber and is dried in vacuo 30- in 100-105 DEG C 50min obtains modified aluminium foil；
4) modified binder prepared by the coating inside surfaces step 2) of aluminium foil layer is modified on surface, coating thickness is Modification heat-sealing film layer prepared by step 1) is then pressed together on the surface of modified binder, through fast press 80 by 5-8um again Under the conditions of DEG C, 1-2min is pressed, places into 80-100 DEG C of baking oven and cures for 24 hours, obtain aluminum-plastic composite membrane.
(3) advantageous effect
Compared with prior art, the present invention provides a kind of aluminum-plastic composite membrane and its preparations for packing lithium ion battery Method has following advantageous effect：
1, the aluminum-plastic composite membrane is modified by the surface to aluminium foil, on the inner surface that surface is modified aluminium foil layer Be provided with modified heat-sealing film layer, modified heat-sealing film layer is fixedly connected by modified binder and surface modification aluminium foil layer, by 9-12 parts of hydroxyl telechelic polyester component, terminal isocyanate group component, bisphenol A type epoxy resin E44 and phenol are added in modified binder Urea formaldehyde is directly added into polyurethane gluing due to containing secondary hydroxyl in bisphenol A type epoxy resin and phenolic resin as polyalcohol The hydroxyl telechelic polyester component of agent by solidification, obtains Graft Epoxy Resin and phenolic resin with isocyanate component Polyurethane network polymer, the polyurethane network polymer considerably improve the adhesive property of modified binder, and then significantly The peel strength between modified aluminium foil layer and modified heat-sealing film layer is improved, solves existing aluminum-plastic composite membrane, due to bonding The adhesive property of agent is poor, keeps aluminium foil layer and the peel strength sealed between film layer relatively low, and heat-sealing film layer is caused to be easy from aluminium foil The technical issues of surface of layer is detached from.
2, aluminum-plastic composite membrane, by being added with polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and charcoal in modified heat-sealing film layer SiClx double substrate material and nano cupric oxide resistant material, polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and carborundum Double substrate micro material Material and nano cupric oxide after chemical reaction finally form layer protecting film structure, the guarantor on the surface of modified heat-sealing film layer Protection film structure can effectively prevent destruction of the electrolyte of lithium ion battery to heat-sealing film layer internal structure, and then effective ground resistance It is rotten to solve the easy electrolyte by lithium ion battery of heat-sealing film layer for only corrosion of the electrolyte of lithium ion battery to aluminium foil layer Erosion, internal structure are destroyed, and then electrolyte leads to the barrier property of aluminum-plastic composite membrane through heat-sealing film layer corrosive aluminum foil layer The technical issues of reduction.
3, the preparation method of the aluminum-plastic composite membrane, by preparing modified binder, modified heat-sealing film layer and modified aluminium respectively Then modified heat-sealing film layer is bonded in surface by modified binder and is modified on the inner surface of aluminium foil layer by layers of foil, the preparation side Aluminum-plastic composite membrane prepared by method not only has excellent barrier property, corrosion resistance and exhaust performance, but also significantly increases Peel strength between the internal layer and secondary internal layer of aluminum-plastic composite membrane.
Specific implementation mode
Below in conjunction with the embodiment of the present invention, technical solution in the embodiment of the present invention is clearly and completely retouched It states, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the present invention In embodiment, every other implementation obtained by those of ordinary skill in the art without making creative efforts Example, shall fall within the protection scope of the present invention.
Embodiment one：
(1) vinyl acetate of 10 mass parts is added in the t-butanol solvent of 20 mass parts, is stirred, then added The vinyl monomer for entering 2 mass parts after being uniformly mixed, is subsequently added into the sodium hydroxide of 1 mass parts, the peroxide of 0.5 mass parts Change the adjacent benzene of benzoic acid, the 6- tert-butyl-m-cresols of 0.1 mass parts, the polyoxyethylene laurate of 0.01 mass parts, 2 mass parts At pressure 4MPa, 80 DEG C of temperature free radicals copolymerization reaction occurs for dioctyl phthalate two (2- ethyl hexyls) ester, and ethylene-acetate second is made Enoate copolymer；
(2) vinyl-vinyl acetate copolymer obtained in step (1) is added in the methanol solvate of 30 mass parts, The sodium hydroxide alkali catalyst of 5 mass parts is added, under nitrogen protection, being heated with stirring in system has methanol steam to evaporate Go out, the methanol of 5 mass parts is added in reaction process, is uniformly carried out with keeping reacting, react 5h, be cooled to room temperature, by by second EVOH copolymers are made at hydroxyl in acetyl group alcoholysis in alkene-vinyl acetate copolymer；
(3) it is water-soluble miscellaneous to remove sodium acetate etc. for EVOH copolymers made from the milli-Q water step (3) with 50 mass parts Matter removes the oil-soluble impurities such as methyl acetate then with 12h is extracted in the acetone of 20 mass parts, and EVOH components are made；
(4) m-xylene diamine of 8 mass parts is added in reaction kettle, is subsequently added into the ultra-pure water of 15 mass parts, then add The polyethylene glycol for entering 20 mass parts, is uniformly mixed, and the adipic acid of 10 mass parts is then added, in the protection of nitrogen atmosphere Under, be stirred, keep reaction temperature at 50 DEG C hereinafter, add the polytetrafluoroethylene (PTFE) of 10 mass parts, 5 mass parts charcoal The nano cupric oxide of fiber reinforced carbon and carborundum double substrate material and 5 mass parts, is uniformly mixed, when reaction temperature no longer When variation, the sodium bicarbonate that 0.05 mass parts are added is added, and is uniformly mixed, and adjusts acid-base value to 7.0, and reaction terminates, system Obtain crystallinity nylon resin component；
(5) crystallinity nylon resin made from EVOH components made from step (3) and step (4) is added to batch mixer, The blender of batch mixer is opened, mixing speed 550r/min, mixing time 30min obtain mixture；
(6) mixture made from step (5) is put into calender, the calendered film come out from calender bottom roller passes through successively Cross first group deflect from roller, second group deflect from roller and third group deflects from roller, first group of channel temperature for deflecting from roller is 20 DEG C, second group Deflect from roller and third group to deflect from the channel temperature of roller be 140 DEG C, calendered film is using first group of chill roll, second group of chill roll It is cooled down with third group chill roll, the temperature of first group of chill roll is 70 DEG C, and the temperature of second group of chill roll is 60 DEG C, and third group is cold But the temperature of roller is 50 DEG C, and trimming and volume area are carried out after cooling, obtains modified heat-sealing film；
(7) the terminal isocyanate group component mixed preparing of the hydroxyl telechelic polyester component for taking 9 mass parts and 1 mass parts is gathered Urethane adhesive components；Then take the bisphenol A type epoxy resin E44 of 2 mass parts spare；
(8) in N2Under protection, carried out using the bisphenol A type epoxy resin E44 of 2 mass parts of ethyl acetate pair of 8 mass parts Dissolving, solution temperature are 50 DEG C, and epoxy resin E44 is made；
(9) epoxy resin E44 obtained is added to step (7) prepared polyurethane adhesive after dissolving step (8) In, it is thoroughly mixed uniformly, binder is made；
(10) phenolic resin for taking 2 mass parts is added in the absolute ethyl alcohol of 8 mass parts, stirs evenly；
(11) ethylenediamine for taking 3 mass parts is added in the deionized water of 10 mass parts, stirs evenly, with step (10) Phenolic aldehyde ethanol solution mixing obtained, stirs evenly, and binder made from step (9), ultrasonic 30min is added, and distillation removes nothing Water-ethanol obtains adhesive aid；
(12) phenol of 5 mass parts is added in the absolute ethyl alcohol of 25 mass parts, is uniformly mixed, slowly increase temperature Degree is 50 DEG C, insulated and stirred 50min, is subsequently added into the silica flour of the graphite powder and 2 mass parts of 2 mass parts, continues insulated and stirred Then adhesive aid obtained in step (11) is added in 30min, it is 80 DEG C to increase temperature, and insulated and stirred 20 minutes is cooled to often Temperature obtains modified binder；
(13) citric acid of 20 mass parts is added in the deionized water of 20 mass parts, is being stirred, 5 is added slowly The sodium hydroxide of mass parts, after being stirred, then add the sodium metasilicate of 2 mass parts, 10 mass parts N, N- double hydroxyethyl coconut palms The acid dimethyl sodium of seed oil amide and 8 mass parts, is uniformly mixed, and degreaser is made；
(14) soft aluminium foil is immersed in degreaser made from step (13) and impregnates 80min, remove the oil on aluminium foil surface Fat impurity；
(15) aluminium foil after step (14) oil removing is placed in vacuum drying chamber and is dried in vacuo 30min in 100 DEG C, that is, made Aluminium foil must be modified；
(16) modified binder prepared by the coating inside surfaces step (12) of aluminium foil layer is modified on surface, coating is thick Degree is 5um, the modification heat-sealing film layer prepared by step (6) is then pressed together on to the surface of modified binder again, through fast press Under the conditions of 80 DEG C, 1min is pressed, places into 80 DEG C of baking oven and cures for 24 hours, obtain aluminum-plastic composite membrane.
Embodiment two：
(1) vinyl acetate of 15 mass parts is added in the t-butanol solvent of 25 mass parts, is stirred, then added The vinyl monomer for entering 4 mass parts after being uniformly mixed, is subsequently added into the sodium hydroxide of 1.5 mass parts, the mistake of 0.8 mass parts Aoxidize the neighbour of benzoic acid, the 6- tert-butyl-m-cresols of 0.3 mass parts, the polyoxyethylene laurate of 0.03 mass parts, 3 mass parts At pressure 4.5MPa, 85 DEG C of temperature free radicals copolymerization reaction occurs for phthalic acid two (2- ethyl hexyls) ester, and ethylene-second is made Vinyl acetate copolymer；
(2) vinyl-vinyl acetate copolymer obtained in step (1) is added in the methanol solvate of 35 mass parts, The sodium hydroxide alkali catalyst of 6 mass parts is added, under nitrogen protection, being heated with stirring in system has methanol steam to evaporate Go out, the methanol of 6 mass parts added in reaction process, with keep react uniformly carry out, react 5.5h, be cooled to room temperature, pass through by EVOH copolymers are made at hydroxyl in acetyl group alcoholysis in vinyl-vinyl acetate copolymer；
(3) it is water-soluble miscellaneous to remove sodium acetate etc. for EVOH copolymers made from the milli-Q water step (3) with 55 mass parts Matter removes the oil-soluble impurities such as methyl acetate then with 13h is extracted in the acetone of 25 mass parts, and EVOH components are made；
(4) m-xylene diamine of 9 mass parts is added in reaction kettle, is subsequently added into the ultra-pure water of 15-20 mass parts, then The polyethylene glycol of 25 mass parts is added, is uniformly mixed, the adipic acid of 12 mass parts is then added, in the protection of nitrogen atmosphere Under, be stirred, keep reaction temperature at 50 DEG C hereinafter, add the polytetrafluoroethylene (PTFE) of 12 mass parts, 7 mass parts charcoal The nano cupric oxide of fiber reinforced carbon and carborundum double substrate material and 6 mass parts, is uniformly mixed, when reaction temperature no longer When variation, the sodium bicarbonate that 0.08 mass parts are added is added, and is uniformly mixed, and adjusts acid-base value to 7.0, and reaction terminates, system Obtain crystallinity nylon resin component；
(5) crystallinity nylon resin made from EVOH components made from step (3) and step (4) is added to batch mixer, The blender of batch mixer is opened, mixing speed 550r/min, mixing time 30min obtain mixture；
(6) mixture made from step (5) is put into calender, the calendered film come out from calender bottom roller passes through successively Cross first group deflect from roller, second group deflect from roller and third group deflects from roller, first group of channel temperature for deflecting from roller is 25 DEG C, second group Deflect from roller and third group to deflect from the channel temperature of roller be 145 DEG C, calendered film is using first group of chill roll, second group of chill roll It is cooled down with third group chill roll, the temperature of first group of chill roll is 72 DEG C, and the temperature of second group of chill roll is 62 DEG C, and third group is cold But the temperature of roller is 52 DEG C, and trimming and volume area are carried out after cooling, obtains modified heat-sealing film；
(7) the terminal isocyanate group component mixed preparing of the hydroxyl telechelic polyester component for taking 10 mass parts and 1.5 mass parts obtains To polyurethane adhesive component；Then take the bisphenol A type epoxy resin E44 of 2.5 mass parts spare；
(8) in N2Under protection, using 9 mass parts 2.5 mass parts of ethyl acetate pair bisphenol A type epoxy resin E44 into Row dissolving, solution temperature are 55 DEG C, and epoxy resin E44 is made；
(9) epoxy resin E44 obtained is added to step (7) prepared polyurethane adhesive after dissolving step (8) In, it is thoroughly mixed uniformly, binder is made；
(10) phenolic resin for taking 3 mass parts is added in the absolute ethyl alcohol of 9 mass parts, stirs evenly；
(11) ethylenediamine for taking 5 mass parts is added in the deionized water of 12 mass parts, stirs evenly, with step (10) Phenolic aldehyde ethanol solution mixing obtained, stirs evenly, and binder made from step (9), ultrasonic 50min is added, and distillation removes nothing Water-ethanol obtains adhesive aid；
(12) phenol of 8 mass parts is added in the absolute ethyl alcohol of 29 mass parts, is uniformly mixed, slowly increase temperature Degree is 55 DEG C, insulated and stirred 55min, is subsequently added into the silica flour of the graphite powder and 2.5 mass parts of 3 mass parts, continues heat preservation and stirs 35min is mixed, adhesive aid obtained in step (11) is then added, it is 85 DEG C to increase temperature, and insulated and stirred 25 minutes is cooled to Room temperature obtains modified binder；
(13) citric acid of 25 mass parts is added in the deionized water of 25 mass parts, is being stirred, 6 is added slowly The sodium hydroxide of mass parts, after being stirred, then add the sodium metasilicate of 2.5 mass parts, 11 mass parts N, N- double hydroxyethyls The acid dimethyl sodium of coconut oleamide and 9 mass parts, is uniformly mixed, and degreaser is made；
(14) soft aluminium foil is immersed in degreaser made from step (13) and impregnates 90min, remove the oil on aluminium foil surface Fat impurity；
(15) aluminium foil after step (14) oil removing is placed in vacuum drying chamber and is dried in vacuo 40min in 102 DEG C, that is, made Aluminium foil must be modified；
(16) modified binder prepared by the coating inside surfaces step (12) of aluminium foil layer is modified on surface, coating is thick Degree is 6um, the modification heat-sealing film layer prepared by step (6) is then pressed together on to the surface of modified binder again, through fast press Under the conditions of 80 DEG C, 1.5min is pressed, places into 90 DEG C of baking oven and cures for 24 hours, obtain aluminum-plastic composite membrane.
Embodiment three：
(1) vinyl acetate of 20 mass parts is added in the t-butanol solvent of 30 mass parts, is stirred, then added The vinyl monomer for entering 5 mass parts after being uniformly mixed, is subsequently added into the peroxidating of the sodium hydroxide, 1 mass parts of 2 mass parts The adjacent benzene two of benzoic acid, the 6- tert-butyl-m-cresols of 0.5 mass parts, the polyoxyethylene laurate of 0.05 mass parts, 5 mass parts At pressure 5MPa, 80-90 DEG C of temperature free radicals copolymerization reaction occurs for formic acid two (2- ethyl hexyls) ester, and ethylene-acetate is made Vinyl ester copolymers；
(2) vinyl-vinyl acetate copolymer obtained in step (1) is added in the methanol solvate of 40 mass parts, The sodium hydroxide alkali catalyst of 8 mass parts is added, under nitrogen protection, being heated with stirring in system has methanol steam to evaporate Go out, the methanol of 8 mass parts is added in reaction process, is uniformly carried out with keeping reacting, react 6h, be cooled to room temperature, by by second EVOH copolymers are made at hydroxyl in acetyl group alcoholysis in alkene-vinyl acetate copolymer；
(3) it is water-soluble miscellaneous to remove sodium acetate etc. for EVOH copolymers made from the milli-Q water step (3) with 60 mass parts Matter removes the oil-soluble impurities such as methyl acetate then with 14h is extracted in the acetone of 30 mass parts, and EVOH components are made；
(4) m-xylene diamine of 10 mass parts is added in reaction kettle, is subsequently added into the ultra-pure water of 20 mass parts, then add The polyethylene glycol for entering 30 mass parts, is uniformly mixed, and the adipic acid of 15 mass parts is then added, in the protection of nitrogen atmosphere Under, be stirred, keep reaction temperature at 50 DEG C hereinafter, add the polytetrafluoroethylene (PTFE) of 15 mass parts, 8 mass parts charcoal The nano cupric oxide of fiber reinforced carbon and carborundum double substrate material and 8 mass parts, is uniformly mixed, when reaction temperature no longer When variation, the sodium bicarbonate that 0.1 mass parts are added is added, and is uniformly mixed, and adjusts acid-base value to 7.5, and reaction terminates, and is made Crystallinity nylon resin component；
(5) crystallinity nylon resin made from EVOH components made from step (3) and step (4) is added to batch mixer, The blender of batch mixer is opened, mixing speed 600r/min, mixing time 60min obtain mixture；
(6) mixture made from step (5) is put into calender, the calendered film come out from calender bottom roller passes through successively Cross first group deflect from roller, second group deflect from roller and third group deflects from roller, first group of channel temperature for deflecting from roller is 30 DEG C, second group Deflect from roller and third group to deflect from the channel temperature of roller be 150 DEG C, calendered film is using first group of chill roll, second group of chill roll It is cooled down with third group chill roll, the temperature of first group of chill roll is 75 DEG C, and the temperature of second group of chill roll is 65 DEG C, and third group is cold But the temperature of roller is 55 DEG C, and trimming and volume area are carried out after cooling, obtains modified heat-sealing film；
(7) the terminal isocyanate group component mixed preparing of the hydroxyl telechelic polyester component for taking 12 mass parts and 2 mass parts obtains Polyurethane adhesive component；Then take the bisphenol A type epoxy resin E44 of 3 mass parts spare；
(8) in N2Under protection, carried out using the bisphenol A type epoxy resin E44 of 3 mass parts of ethyl acetate pair of 10 mass parts Dissolving, solution temperature are 60 DEG C, and epoxy resin E44 is made；
(9) epoxy resin E44 obtained is added to step (7) prepared polyurethane adhesive after dissolving step (8) In, it is thoroughly mixed uniformly, binder is made；
(10) phenolic resin for taking 5 mass parts is added in the absolute ethyl alcohol of 10 mass parts, stirs evenly；
(11) ethylenediamine for taking 6 mass parts is added in the deionized water of 15 mass parts, stirs evenly, with step (10) Phenolic aldehyde ethanol solution mixing obtained, stirs evenly, and binder made from step (9), ultrasonic 60min is added, and distillation removes nothing Water-ethanol obtains adhesive aid；
(12) phenol of 10 mass parts is added in the absolute ethyl alcohol of 30 mass parts, is uniformly mixed, slowly increased Temperature is 60 DEG C, insulated and stirred 60min, is subsequently added into the silica flour of the graphite powder and 3 mass parts of 4 mass parts, continues heat preservation and stirs 40min is mixed, adhesive aid obtained in step (11) is then added, it is 90 DEG C to increase temperature, and insulated and stirred 30 minutes is cooled to Room temperature obtains modified binder；
(13) citric acid of 30 mass parts is added in the deionized water of 30 mass parts, is being stirred, 8 is added slowly The sodium hydroxide of mass parts, after being stirred, then add the sodium metasilicate of 3 mass parts, 12 mass parts N, N- double hydroxyethyl coconut palms The acid dimethyl sodium of seed oil amide and 10 mass parts, is uniformly mixed, and degreaser is made；
(14) soft aluminium foil is immersed in degreaser made from step (13) and impregnates 100min, remove the oil on aluminium foil surface Fat impurity；
(15) aluminium foil after step (14) oil removing is placed in vacuum drying chamber and is dried in vacuo 50min in 105 DEG C, that is, made Aluminium foil must be modified；
(16) modified binder prepared by the coating inside surfaces step (12) of aluminium foil layer is modified on surface, coating is thick Degree is 8um, the modification heat-sealing film layer prepared by step (6) is then pressed together on to the surface of modified binder again, through fast press Under the conditions of 80 DEG C, 2min is pressed, places into 100 DEG C of baking oven and cures for 24 hours, obtain aluminum-plastic composite membrane.
Experimental example：In testing example one, embodiment two and embodiment three between modified aluminium foil layer and modified heat-sealing film layer Peel strength, test result is shown in Table 1；
Embodiment one, embodiment two and the aluminum-plastic composite membrane prepared by embodiment three are respectively fabricated to eight battery samples, Carry out following three groups of tests：
Test one：Four battery samples are taken to be toasted at 60 DEG C for 24 hours, whether visual inspection aluminum-plastic composite membrane leakage, gas occurs Swollen situation and the delamination for whether being modified aluminium foil layer and modified heat-sealing film layer, test result are shown in Table 2；
Test two：It takes four battery samples to be placed in 60 DEG C, 96h is kept in the environment of relative humidity 90%, carry out test aluminium Whether there is or not bulging, leakage situation and the delamination for whether being modified aluminium foil layer and modified heat-sealing film layer, test results for modeling composite membrane It is shown in Table 3；
Criterion：Lithium ion battery be packed for the peel strength between the internal layer of aluminum-plastic composite membrane and secondary internal layer >= 2.5N/m；After 60 DEG C of bakings for 24 hours of battery sample made of aluminum-plastic composite membrane, there is not allowed that leakage, inflatable situation；Using aluminium It moulds after battery sample high temperature and humidity, water-bath made of composite membrane are tested without bulging, leakage.
Table 1
Embodiment Peel strength (N/m) between modified aluminium foil layer and modified heat-sealing film layer
Embodiment 1 15.6
Embodiment 2 16.3
Embodiment 3 14.9
Table 2
Table 3
The beneficial effects of the invention are as follows：Embodiment one, embodiment two and the modification aluminium foil layer of embodiment three are sealed with modified Peel strength between film layer is respectively 15.6N/m, 16.3N/m and 14.9N/m, is all higher than 2.5N/m, so the aluminium of the present invention Modeling composite membrane considerably improves the peel strength that lithium ion battery is packed between the internal layer of aluminum-plastic composite membrane and secondary internal layer；
Each four groups of battery samples are at 60 DEG C made of aluminum-plastic composite membrane using embodiment one, embodiment two with embodiment three For 24 hours, visual inspection does not occur leakage and inflatable situation for baking；Using the aluminium of embodiment one, embodiment two and embodiment three Each four groups of battery samples are placed in 60 DEG C made of modeling composite membrane is each, keep 96h in the environment of relative humidity 90%, without bulging, Leakage situation, so the aluminum-plastic composite membrane of the present invention has excellent barrier property, corrosion resistance and exhaust performance.
Typical case：(1) vinyl acetate of 15 mass parts is added in the t-butanol solvent of 25 mass parts, is stirred , the vinyl monomer of 4 mass parts is added, after being uniformly mixed, is subsequently added into sodium hydroxide, 0.8 matter of 1.5 mass parts Measure the perbenzoic acid of part, the 6- tert-butyl-m-cresols of 0.3 mass parts, the polyoxyethylene laurate of 0.03 mass parts, 3 matter At pressure 4.5MPa, 85 DEG C of temperature free radicals copolymerization reaction, system occur for phthalic acid two (2- ethyl hexyls) ester for measuring part Obtain vinyl-vinyl acetate copolymer；
(2) vinyl-vinyl acetate copolymer obtained in step (1) is added in the methanol solvate of 35 mass parts, The sodium hydroxide alkali catalyst of 6 mass parts is added, under nitrogen protection, being heated with stirring in system has methanol steam to evaporate Go out, the methanol of 6 mass parts added in reaction process, with keep react uniformly carry out, react 5.5h, be cooled to room temperature, pass through by EVOH copolymers are made at hydroxyl in acetyl group alcoholysis in vinyl-vinyl acetate copolymer；
(3) it is water-soluble miscellaneous to remove sodium acetate etc. for EVOH copolymers made from the milli-Q water step (3) with 55 mass parts Matter removes the oil-soluble impurities such as methyl acetate then with 13h is extracted in the acetone of 25 mass parts, and EVOH components are made；
(4) m-xylene diamine of 9 mass parts is added in reaction kettle, is subsequently added into the ultra-pure water of 15-20 mass parts, then The polyethylene glycol of 25 mass parts is added, is uniformly mixed, the adipic acid of 12 mass parts is then added, in the protection of nitrogen atmosphere Under, be stirred, keep reaction temperature at 50 DEG C hereinafter, add the polytetrafluoroethylene (PTFE) of 12 mass parts, 7 mass parts charcoal The nano cupric oxide of fiber reinforced carbon and carborundum double substrate material and 6 mass parts, is uniformly mixed, when reaction temperature no longer When variation, the sodium bicarbonate that 0.08 mass parts are added is added, and is uniformly mixed, and adjusts acid-base value to 7.0, and reaction terminates, system Obtain crystallinity nylon resin component；
(5) crystallinity nylon resin made from EVOH components made from step (3) and step (4) is added to batch mixer, The blender of batch mixer is opened, mixing speed 550r/min, mixing time 30min obtain mixture；
(6) mixture made from step (5) is put into calender, the calendered film come out from calender bottom roller passes through successively Cross first group deflect from roller, second group deflect from roller and third group deflects from roller, first group of channel temperature for deflecting from roller is 25 DEG C, second group Deflect from roller and third group to deflect from the channel temperature of roller be 145 DEG C, calendered film is using first group of chill roll, second group of chill roll It is cooled down with third group chill roll, the temperature of first group of chill roll is 72 DEG C, and the temperature of second group of chill roll is 62 DEG C, and third group is cold But the temperature of roller is 52 DEG C, and trimming and volume area are carried out after cooling, obtains modified heat-sealing film；
(7) the terminal isocyanate group component mixed preparing of the hydroxyl telechelic polyester component for taking 10 mass parts and 1.5 mass parts obtains To polyurethane adhesive component；Then take the bisphenol A type epoxy resin E44 of 2.5 mass parts spare；
(8) in N2Under protection, using 9 mass parts 2.5 mass parts of ethyl acetate pair bisphenol A type epoxy resin E44 into Row dissolving, solution temperature are 55 DEG C, and epoxy resin E44 is made；
(9) epoxy resin E44 obtained is added to step (7) prepared polyurethane adhesive after dissolving step (8) In, it is thoroughly mixed uniformly, binder is made；
(10) phenolic resin for taking 3 mass parts is added in the absolute ethyl alcohol of 9 mass parts, stirs evenly；
(11) ethylenediamine for taking 5 mass parts is added in the deionized water of 12 mass parts, stirs evenly, with step (10) Phenolic aldehyde ethanol solution mixing obtained, stirs evenly, and binder made from step (9), ultrasonic 50min is added, and distillation removes nothing Water-ethanol obtains adhesive aid；
(12) phenol of 8 mass parts is added in the absolute ethyl alcohol of 29 mass parts, is uniformly mixed, slowly increase temperature Degree is 55 DEG C, insulated and stirred 55min, is subsequently added into the silica flour of the graphite powder and 2.5 mass parts of 3 mass parts, continues heat preservation and stirs 35min is mixed, adhesive aid obtained in step (11) is then added, it is 85 DEG C to increase temperature, and insulated and stirred 25 minutes is cooled to Room temperature obtains modified binder；
(13) citric acid of 25 mass parts is added in the deionized water of 25 mass parts, is being stirred, 6 is added slowly The sodium hydroxide of mass parts, after being stirred, then add the sodium metasilicate of 2.5 mass parts, 11 mass parts N, N- double hydroxyethyls The acid dimethyl sodium of coconut oleamide and 9 mass parts, is uniformly mixed, and degreaser is made；
(14) soft aluminium foil is immersed in degreaser made from step (13) and impregnates 90min, remove the oil on aluminium foil surface Fat impurity；
(15) aluminium foil after step (14) oil removing is placed in vacuum drying chamber and is dried in vacuo 40min in 102 DEG C, that is, made Aluminium foil must be modified；
(16) modified binder prepared by the coating inside surfaces step (12) of aluminium foil layer is modified on surface, coating is thick Degree is 6um, the modification heat-sealing film layer prepared by step (6) is then pressed together on to the surface of modified binder again, through fast press Under the conditions of 80 DEG C, 1.5min is pressed, places into 90 DEG C of baking oven and cures for 24 hours, obtain aluminum-plastic composite membrane.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of variations, modification, replace And modification, the scope of the present invention is defined by the appended.

Claims (6)

1. a kind of aluminum-plastic composite membrane for packing lithium ion battery, including surface are modified aluminium foil layer, which is characterized in that the table Face, which is modified on the inner surface of aluminium foil layer, is provided with modified heat-sealing film layer, and modification heat-sealing film layer passes through modified binder and surface Modified aluminium foil layer is fixedly connected；
The surface is modified the raw material that aluminium foil includes following parts by weight proportioning：20-30 parts of citric acid, 20-30 parts of deionized water, 5-8 parts of sodium hydroxide, 2-3 parts of sodium metasilicate, N, 10-12 parts of N- double hydroxyethyls coconut oleamide, acid dimethyl sodium 8-10 Part；
The modified heat-sealing film includes the raw material of following parts by weight proportioning：10-20 parts of vinyl acetate, 20-30 parts of the tert-butyl alcohol, 2-5 parts of vinyl monomer, 1-2 parts of sodium hydroxide, 0.5-1 parts of perbenzoic acid, 0.1-0.5 parts of 6- tert-butyl-m-cresols, polyoxy 0.01-0.05 parts of ethylene laurate, 2-5 parts of phthalic acid two (2- ethyl hexyls) ester, 35-50 parts of methanol, sodium hydroxide 5-8 Part, 65-80 parts of ultra-pure water, 20-30 parts of acetone, 8-10 parts of m-xylene diamine, 20-30 parts of polyethylene glycol, 10-15 parts of adipic acid, 5-8 parts of 10-15 parts of polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and carborundum double substrate material, 5-8 parts of nano cupric oxide, bicarbonate 0.05-0.1 parts of sodium；
The modified binder includes the raw material of following parts by weight proportioning：It is 9-12 parts of hydroxyl telechelic polyester component, isocyanate terminated 1-2 parts of base component, 2-3 parts of bisphenol A type epoxy resin E44,8-10 parts of ethyl acetate, 2-5 parts of phenolic resin, absolute ethyl alcohol 35- 40 parts, 3-6 parts of ethylenediamine, 10-15 parts of deionized water, 5-10 parts of phenol, 2-4 parts of graphite powder, 2-3 parts of silica flour；
The peel strength of the aluminum-plastic composite membrane is 14.9-16.3N/m.
2. a kind of aluminum-plastic composite membrane for packing lithium ion battery according to claim 1, which is characterized in that the aluminium The peel strength for moulding composite membrane is 16.3N/m.
3. a kind of aluminum-plastic composite membrane for packing lithium ion battery according to claim 1, which is characterized in that the table Face is modified the raw material that aluminium foil includes following parts by weight proportioning：25 parts of citric acid, 25 parts of deionized water, 6 parts of sodium hydroxide, inclined silicon 2.5 parts of sour sodium, N, 11 parts of N- double hydroxyethyl coconuts oleamide, 9 parts of acid dimethyl sodium.
4. a kind of aluminum-plastic composite membrane for packing lithium ion battery according to claim 1, which is characterized in that described to change Property heat-sealing film include following parts by weight proportioning raw material：15 parts of vinyl acetate, 25 parts of the tert-butyl alcohol, 4 parts of vinyl monomer, hydrogen-oxygen Change 1.5 parts of sodium, 0.8 part of perbenzoic acid, 0.3 part of 6- tert-butyl-m-cresols, 0.03 part of polyoxyethylene laurate, adjacent benzene two 3 parts of formic acid two (2- ethyl hexyls) ester, 41 parts of methanol, 6 parts of sodium hydroxide, 80 parts of ultra-pure water, 25 parts of acetone, 9 parts of m-xylene diamine, 25 parts of polyethylene glycol, 12 parts of adipic acid, 12 parts of polytetrafluoroethylene (PTFE), carbon fiber reinforced carbon and carborundum double substrate material 7 part, nanometer 6 parts of copper oxide, 0.08 part of sodium bicarbonate.
5. a kind of aluminum-plastic composite membrane for packing lithium ion battery according to claim 1, which is characterized in that described to change Property binder include following parts by weight proportioning raw material：10 parts of hydroxyl telechelic polyester component, 1.5 parts of terminal isocyanate group component, 2.5 parts of bisphenol A type epoxy resin E44,9 parts of ethyl acetate, 3 parts of phenolic resin, 38 parts of absolute ethyl alcohol, 5 parts of ethylenediamine, go from 12 parts of sub- water, 8 parts of phenol, 3 parts of graphite powder, 2.5 parts of silica flour.
6. a kind of preparation method for packing the aluminum-plastic composite membrane of lithium ion battery, which is characterized in that include the following steps：
1) preparation of modified heat-sealing film
(1) vinyl acetate of 10-20 mass parts is added in the t-butanol solvent of 20-30 mass parts, is stirred, then The vinyl monomer of 2-5 mass parts is added, after being uniformly mixed, is subsequently added into sodium hydroxide, the 0.5-1 mass of 1-2 mass parts The polyoxyethylene laural of the perbenzoic acid of part, the 6- tert-butyl-m-cresols of 0.1-0.5 mass parts, 0.01-0.05 mass parts Phthalic acid two (2- ethyl hexyls) ester of acid esters, 2-5 mass parts occurs freely at pressure 4-5MPa, 80-90 DEG C of temperature Vinyl-vinyl acetate copolymer is made in base copolyreaction；
(2) vinyl-vinyl acetate copolymer obtained in step (1) is added in the methanol solvate of 30-40 mass parts, then The sodium hydroxide alkali catalyst of 5-8 mass parts is added, under nitrogen protection, being heated with stirring in system has methanol steam to evaporate Go out, the methanol of 5-8 mass parts is added in reaction process, is uniformly carried out with keeping reacting, react 5-6h, be cooled to room temperature, pass through By the acetyl group alcoholysis in vinyl-vinyl acetate copolymer at hydroxyl, EVOH copolymers are made；
(3) EVOH copolymers made from the milli-Q water step (3) of 50-60 mass parts are used, it is water-soluble miscellaneous to remove sodium acetate etc. Matter removes the oil-soluble impurities such as methyl acetate then with 12-14h is extracted in the acetone of 20-30 mass parts, and EVOH components are made；
(4) m-xylene diamine of 8-10 mass parts is added in reaction kettle, is subsequently added into the ultra-pure water of 15-20 mass parts, then The polyethylene glycol of 20-30 mass parts is added, is uniformly mixed, the adipic acid of 10-15 mass parts is then added, in nitrogen atmosphere Protection under, be stirred, keep reaction temperature at 50 DEG C hereinafter, adding the polytetrafluoroethylene (PTFE) of 10-15 mass parts, 5- The nano cupric oxide of the carbon fiber reinforced carbon and carborundum double substrate material and 5-8 mass parts of 8 mass parts, is uniformly mixed, When reaction temperature no longer changes, the sodium bicarbonate that 0.05-0.1 mass parts are added is added, and is uniformly mixed, and adjusts acid-base value To 7.0-7.5, reaction terminates, and crystallinity nylon resin component is made；
(5) crystallinity nylon resin made from EVOH components made from step (3) and step (4) is added to batch mixer, opened The blender of batch mixer, mixing speed 550-600r/min, mixing time 30-60min obtain mixture；
(6) mixture made from step (5) is put into calender, the calendered film come out from calender bottom roller passes through the successively One group deflect from roller, second group deflect from roller and third group deflects from roller, first group of channel temperature for deflecting from roller is 20-30 DEG C, second group Deflect from roller and third group to deflect from the channel temperature of roller be 140-150 DEG C, calendered film using first group of chill roll, second group it is cold But the temperature of roller and the cooling of third group chill roll, first group of chill roll is 70-75 DEG C, and the temperature of second group of chill roll is 60-65 DEG C, the temperature of third group chill roll is 50-55 DEG C, and trimming and volume area are carried out after cooling, obtains modified heat-sealing film；
2) preparation of modified binder
(1) the terminal isocyanate group component mixed preparing of the hydroxyl telechelic polyester component for taking 9-12 mass parts and 1-2 mass parts obtains Polyurethane adhesive component；Then take the bisphenol A type epoxy resin E44 of 2-3 mass parts spare；
(2) in N2Under protection, the bisphenol A type epoxy resin E44 of 2-3 mass parts is carried out using the ethyl acetate of 8-10 mass parts Dissolving, solution temperature are 50-60 DEG C, and epoxy resin E44 is made；
(3) epoxy resin E44 obtained is added in step (1) prepared polyurethane adhesive after dissolving step (2), fills Divide and be uniformly mixed, binder is made；
(4) phenolic resin for taking 2-5 mass parts is added in the absolute ethyl alcohol of 8-10 mass parts, stirs evenly；
(5) ethylenediamine for taking 3-6 mass parts is added in the deionized water of 10-15 mass parts, stirs evenly, and is made with step (4) The phenolic aldehyde ethanol solution mixing obtained, stirs evenly, and binder made from step (3) is added, and ultrasonic 30-60min distills, and removes Absolute ethyl alcohol obtains adhesive aid；
(6) phenol of 5-10 mass parts is added in the absolute ethyl alcohol of 25-30 mass parts, is uniformly mixed, slowly increased Temperature is 50-60 DEG C, insulated and stirred 50-60min, is subsequently added into the silica flour of the graphite powder and 2-3 mass parts of 2-4 mass parts, Continue insulated and stirred 30-40min, adhesive aid obtained in step (5) is then added, it is 80-90 DEG C to increase temperature, and heat preservation is stirred It mixes 20-30 minutes, is cooled to room temperature, obtains modified binder；
3) surface is modified the preparation of aluminium foil
(1) citric acid of 20-30 mass parts is added in the deionized water of 20-30 mass parts, is being stirred, is being added slowly The sodium hydroxide of 5-8 mass parts, after being stirred, then add the sodium metasilicate of 2-3 mass parts, 10-12 mass parts N, N- is bis- The acid dimethyl sodium of ethoxy coconut oleamide and 8-10 mass parts, is uniformly mixed, and degreaser is made；
(2) soft aluminium foil is immersed in degreaser made from step (1) and impregnates 80-100min, remove the grease on aluminium foil surface Impurity；
(3) aluminium foil after step (2) oil removing is placed in vacuum drying chamber and is dried in vacuo 30-50min in 100-105 DEG C, i.e., Modified aluminium foil is made；
4) modified binder prepared by the coating inside surfaces step 2) of aluminium foil layer, coating thickness 5- are modified on surface Modification heat-sealing film layer prepared by step 1) is then pressed together on the surface of modified binder, through fast press at 80 DEG C by 8um again Under the conditions of, 1-2min is pressed, places into 80-100 DEG C of baking oven and cures for 24 hours, obtain aluminum-plastic composite membrane.
CN201810397895.5A 2018-04-28 2018-04-28 It is a kind of to be used to pack aluminum-plastic composite membrane of lithium ion battery and preparation method thereof Withdrawn CN108630837A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111331984A (en) * 2020-03-19 2020-06-26 昆山金盛达包装制品有限公司 Aluminum-plastic composite film for packaging material
CN113488698A (en) * 2020-07-31 2021-10-08 惠州市合盈科技有限公司 Manufacturing method for producing soft-shell lithium battery
CN114583171A (en) * 2022-01-20 2022-06-03 贵阳学院 Lithium battery electrode adhesive and preparation method thereof
CN115000604A (en) * 2022-06-24 2022-09-02 江西永德立新能源有限公司 Preparation process of aluminum plastic film for lithium battery outer package

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111331984A (en) * 2020-03-19 2020-06-26 昆山金盛达包装制品有限公司 Aluminum-plastic composite film for packaging material
CN113488698A (en) * 2020-07-31 2021-10-08 惠州市合盈科技有限公司 Manufacturing method for producing soft-shell lithium battery
CN114583171A (en) * 2022-01-20 2022-06-03 贵阳学院 Lithium battery electrode adhesive and preparation method thereof
CN115000604A (en) * 2022-06-24 2022-09-02 江西永德立新能源有限公司 Preparation process of aluminum plastic film for lithium battery outer package
CN115000604B (en) * 2022-06-24 2023-09-15 江西永德立新能源有限公司 Preparation process for lithium battery outer package aluminum plastic film

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