CN106356474A - Aluminum plastic compound film with excellent heat sealing property and low-temperature flexibility - Google Patents

Aluminum plastic compound film with excellent heat sealing property and low-temperature flexibility Download PDF

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Publication number
CN106356474A
CN106356474A CN201610944914.2A CN201610944914A CN106356474A CN 106356474 A CN106356474 A CN 106356474A CN 201610944914 A CN201610944914 A CN 201610944914A CN 106356474 A CN106356474 A CN 106356474A
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layer
aluminium foil
polypropylene
aluminum
stearic acid
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王丹旭
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GUANGDONG ANDELI NEW MATERIALS Co Ltd
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GUANGDONG ANDELI NEW MATERIALS Co 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
    • B32B15/085—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 comprising polyolefins
    • 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
    • B32B15/088—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 comprising polyamides
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
    • 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
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention provides an aluminum plastic compound film with excellent heat sealing property and low-temperature flexibility. The aluminum plastic compound film is characterized by comprising a heat sealing layer, a first glue sticking layer, an aluminum foil layer, a second glue sticking layer and an outer protecting layer in turn from inside to outside, wherein the heat sealing layer is made from a casting polypropylene film; the beta crystal in the casting polypropylene film is 30-99% of total crystalline portion of polypropylene; the outer protecting layer is arranged as a bidirectional stretching polyethylene terephthalate (bidirectional stretching PET layer) or a bidirectional stretching polyamide layer (bidirectional stretching PA layer). The aluminum plastic compound film provided by the invention has higher heat sealing temperature, lower heat sealing lower-limit temperature and more excellent flexibility, especially, flexibility under low-temperature environment.

Description

A kind of aluminum-plastic composite membrane with excellent heat sealability and low-temperature flexibility
Technical field
The present invention relates to packaging material for battery case is and in particular to a kind of have excellent heat sealability and low-temperature flexibility Aluminum-plastic composite membrane.
Background technology
Lithium ion battery is because of its running voltage height, small volume, light weight, specific energy is high, self discharge is little, temperature limit Wide, have extended cycle life and pollution-free, the advantage such as have a safety feature, be described as " the most promising chemical energy source ", be widely used in The electronic equipments such as mobile phone, portable computer, video camera, photographing unit and the power supply of power vehicle.Lithium ion battery can be adopted With aluminum-plastic composite membrane as packaging material, carry out heat sealed package, form shell defendance battery body.Whole in order to intact parcel Individual battery body, and through being heated, the impact of electrolyte and mechanical force is it is desirable to the internal layer (i.e. hot sealing layer) of aluminum-plastic composite membrane provides Relatively low initial heat-sealing temperature, wider heat-sealing temperature scope are so as to can quickly sealing and obtaining higher heat seal strength； Especially, lithium ion battery needs to use under various environment or even low temperature environment, and under these circumstances, lithium battery aluminum-plastic film has There is higher toughness, be particularly important.
The packing timber of integration will be bonded in order by drawing polyamide layer, aluminium foil layer, polypropylene layer at present Material, wherein polypropylene layer are hot sealing layer.The acrylic resin that polypropylene layer is adopted is generally alpha-crystal form, and its melt temperature is higher, Required heat-sealing temperature is also higher.If heat-sealing temperature is not high enough or the heat-sealing time falls short of, heat seal strength all can be led to poor, It is difficult to meet use requirement.And, polypropylene layer toughness is poor, and especially low-temperature flexibility is poor, in the deep forming process of punching or one-tenth During assembled battery uses after type, such as run into low temperature environment, tend to embrittlement, toughness is not enough, is easily destroyed.
In brief, existing aluminum-plastic composite membrane heat sealability is poor (heat-sealing temperature is too high, heat-sealing window is narrow etc.), and Toughness particularly low-temperature flexibility is not enough it is impossible to meet its application requirement in lithium ion battery packaging well.
Content of the invention
The technical problem to be solved be provide a kind of aluminum-plastic composite membrane, this aluminum-plastic composite membrane can as lithium from The packaging material of sub- battery, have excellent heat sealability, and have excellent toughness especially low-temperature flexibility.Using technology Scheme is as follows:
A kind of aluminum-plastic composite membrane with excellent heat sealability and low-temperature flexibility is it is characterised in that include successively from the inside to the outside Hot sealing layer, the first adhesive layer, aluminium foil layer, the second adhesive layer and external protection；Described hot sealing layer is made up of cast polypropylene film, stream Prolong beta crystal in polypropylene screen account for the total crystalline portion of polypropylene relative percentage be 30-99%；Described external protection is two-way drawing Stretch polyethylene terephthalate layer (biaxial tension pet layer) or two-way stretching polyamide layer (biaxial tension pa layer).
The relative percentage that in preferably above-mentioned cast polypropylene film, beta crystal accounts for the total crystalline portion of polypropylene is 40-70%.
The preparation method of preferably above-mentioned cast polypropylene film comprises the steps:
(1) by mass, it is equipped with following raw materials: beta crystal-type nucleater 0.01-10%, nano silicon 0.1-10%, remaining Measure as polypropylene；
Described polypropylene is one of polypropylene homopolymer and polypropylene copolymer or both mixture；
The mean isotactic regularity of described polypropylene homopolymer and polypropylene copolymer is all located at the scope of 55-99% Interior (by [carbon] NMR (Nuclear Magnetic Resonance) spectrum (13C nuclear magnetic resonance spectroscopy, referred to as13c- Nmr) measure)；The fusing point of described polypropylene homopolymer and polypropylene copolymer is 130-170 DEG C (by means of differential scanning calorimetry Instrument (dsc) measures)；The melt flow index of described polypropylene homopolymer and polypropylene copolymer is 0.1-25g/10min and (adopts With meeting the Melt Flow Rate Measurer of din53735 standard, measure under 230 DEG C and 2.16kg load)；Described polypropylene homo The solvable sex ratio of normal heptane of thing and polypropylene copolymer is below 20wt%；
(2) polypropylene is added together with beta crystal-type nucleater extruder carry out kneading, extrude, and through being cast chill roll stream Prolong film forming, the temperature of extruder barrel is 180-260 DEG C, and the temperature of extrusion die is 200-280 DEG C, the temperature of curtain coating chill roll For 30-80 DEG C, obtain described cast polypropylene film.
In preferred steps (1), the mass percent of provisioned raw material is: beta crystal-type nucleater 0.02-5%, nano-silica SiClx 1-5%, balance of polypropylene.
In preferred steps (2), the temperature of curtain coating chill roll is 40-70 DEG C.
The melt flow index of preferably above-mentioned polypropylene homopolymer and polypropylene copolymer is 0.5-10g/10min.
Preferably above-mentioned beta crystal-type nucleater is calcium pimelate, calcium suberate, n, n- dicyclohexyl -2,6,-naphthalene dicarboxamide, One of n, n- dicyclohexyl terephthalamide, gamma-quinacridinelone, dihydro quinacridine and calcium phthalate or wherein many The mixture planted.
The material of above-mentioned aluminium foil layer can be aluminum or aluminum alloy.
In above-mentioned cast polypropylene film, beta crystal is accounted for the relative percentage of the total crystalline portion of polypropylene and is spread out by wide angle X-ray Penetrate instrument (waxd) to measure and calculate (formula: k according to turner-jones formulaβ=h (β)/(h (β)+h (α)) × 100%, its Middle kβFor the relative amount of beta crystal, h (β) represents the height of beta crystal diffraction maximum in waxd collection of illustrative plates, in h (α) expression waxd collection of illustrative plates The height sum of each alpha-crystal form diffraction maximum).The β crystalline substance ratio of above-mentioned cast polypropylene film is mainly together decided on by following factors: (1) The addition (addition generally, increasing beta crystal-type nucleater can improve β crystalline substance ratio) of beta crystal-type nucleater in raw material, with And the species of selected beta crystal-type nucleater；(2) pp material mean isotactic regularity (pp material averagely complete Higher with steric regularity, then β crystalline substance ratio is higher)；(3) it is cast the temperature (i.e. crystallization temperature) of chill roll, this temperature is higher, then β crystalline substance ratio is higher.
In order to strengthen the acid corrosion-resistant performance of above-mentioned aluminum-plastic composite membrane, the inner surface of preferably above-mentioned aluminium foil layer has Monostearate film layer, the first stearic acid film layer is connected with described hot sealing layer by the first adhesive layer, on the outer surface of aluminium foil layer There is the second stearic acid film layer, the second stearic acid film layer is connected with described external protection by the second adhesive layer.
In preferred version, the first stearic acid film layer, the second stearic acid are formed on the inner surface, outer surface of aluminium foil layer The method of film layer comprises the steps: successively
(1 ') immerses aluminium foil in hydrochloric acid-oxalic acid mixed solution that temperature is 20-30 DEG C, soaks 0.5-2min；
Every liter of hydrochloric acid-oxalic acid mixed solution is formed by the preparation of raw material of following ratios: 5-20 gram of oxalic acid, concentrated hydrochloric acid 5-100 Gram, balance of water；
Aluminium foil is taken out from hydrochloric acid-oxalic acid mixed solution and immerses the potassium permanganate solution that temperature is 20-30 DEG C by (2 ') In, soak 1-2min；
Every liter of potassium permanganate solution contains: 5-32 gram of potassium permanganate, balance of water；
Aluminium foil is taken out from potassium permanganate solution by (3 '), after being cleaned aluminium foil with water, then aluminium foil drying (is preferably existed Dry at 70-80 DEG C)；
(4 ') immerse aluminium foil in the stearic acid ethanol solution that mass percent concentration is 0.1-1%, soak 1-10 minute； Then aluminium foil is taken out from stearic acid ethanol solution and is dried (preferably using 50-70 DEG C of hot air drying), in the inner side table of aluminium foil First stearic acid film layer, the second stearic acid film layer are formed on face, outer surface, described aluminium foil constitutes the aluminum of aluminum-plastic composite membrane respectively Layers of foil.
In preferred steps (1 '), aluminium foil used is the alloy foil that thickness is 30-50 μm.
In above-mentioned steps (1 '), hydrochloric acid-oxalic acid mixed solution impregnates acid etch to aluminium foil, forms micron order in aluminium foil surface Loose structure.Hydrochloric acid-oxalic acid mixed liquor acts on to aluminium foil surface: aluminium foil is immersed in hydrochloric acid-oxalic acid mixed solution, aluminium foil surface Oxide-film dissolved first；Then (pit corrosion), when running into hydrochloric acid, preferentially can be corroded in the high-energy point area of aluminium foil surface, Subsequently etch pit interior metal is made to dissolve in the presence of hydrogen and acid, uneven due to metal inside lattice defect Property, makes metal etch speed inconsistent, also results in that surface corrosion degree is different, and occur in that many sizes differ is concavo-convex micro- Fine texture, thus form micron-sized random loose structure in aluminium foil surface.Oxalic acid belongs to weak acid, to aluminum and oxide-film dissolving Property is little, plays the effect of acid restrainer.
Above-mentioned concentrated hydrochloric acid refers to the hydrochloric acid that containing hydrogen chloride mass percent is 37%.
In step (2 '), potassium permanganate solution impregnates to aluminium foil, and potassium permanganate, can used as a kind of strong oxidizer, passivator So that one layer more tiny of (nanoscale), finer and close oxide layer to be re-formed on the aluminium surface of micrometer level porous structure, thus Aluminium foil surface forms granular layer (about 1-5 μm of the hole depth of this loose structure granular layer, the aperture of loose structure micro-, that nanometer is alternate About 1-2 μm, about 5-20 μm of pitch of holes), make aluminium foil layer rough surface.
In above-mentioned steps (4 '), when the aluminium foil through rough surface is immersed in stearic acid ethanol solution, stearic acid second Alcoholic solution can penetrate in the hole of aluminium foil surface, and wraps the granular layer of loose structure, so, the first stearic acid of formation Granular layer is wrapped by film layer, the second stearic acid film layer, and combines closely with aluminium foil layer surface.Stearic acid is low-surface-energy thing Matter, is interweaved with um porous structure particles layer, forms fine and close coating layer (i.e. the first stearic acid film layer, the second stearic acid Film layer), there is superhydrophobic characteristic, excellent acid-resistant corrosion；Meanwhile, stearic acid is a kind of fatty acid of saturation, molecule long-chain In be all connected with methylene singly-bound, internal carbon atom bonding two hydrogen atoms, and stearic acid molecule can pass through ionic bond and aluminum The porous structure layer on paper tinsel surface combines and makes coating layer adhesiveness strong, and surface property is stable, thus the first stearic acid film layer, second Stearic acid film layer is big with aluminium foil surface adhesion, can form good bonding with the first adhesive layer and the second adhesive layer further, It is easy to and plastic resin layers and external protection bonding.
Above-mentioned first stearic acid film layer, the second stearic acid film layer are stable super-hydrophobic layer.Generally, above-mentioned first stearic acid The contact angle of film layer, the second stearic acid film layer and water is all higher than 150 °, and water droplet roll angle is respectively less than 10 °.Preferably above-mentioned first is hard The contact angle of fat acid film layer, the second stearic acid film layer and water is all higher than 160 °, and water droplet roll angle is respectively less than 7 °.Preferably above-mentioned first Stearic acid film layer, the thickness of the second stearic acid film layer are 3-10 μm.
The superhydrophobic aluminum foil (being made up of the first stearic acid film layer, aluminium foil layer and the second stearic acid film layer) being formed is common All there is in air ambient and slightly acidic water solution environmental good super-hydrophobic stability.
The contact angle of above-mentioned first stearic acid film layer, the second stearic acid film layer and water can pass through screen optical contact angular measurement Instrument measures, and using the measurement of drop method of testing, during measurement, water droplet used is 7 μ l-9 μ l.Water droplet roll angle can adopt following methods Test: the Super-hydrophobic aluminium foil sample that need are tested is fixed on the sample stage with protractor, then carefully tilts from 0 ° of beginning Sample platform, then with microsyringe, 5 μ l-9 μ l water droplets are dropped on sample stage, when water droplet tumbles foil samples surface, sample stage tilts Angle is just the water droplet roll angle on this superhydrophobic aluminum foil surface.
It is a discovery of the invention that the β crystalline substance of acrylic resin has the characteristic than α low 10-20 DEG C of fusing point of crystalline substance, and its toughness is especially Low-temperature flexibility is significantly better than α crystalline substance, therefore using the high casting polypropylene film layer of beta crystal content as hot sealing layer.Due to the fusing point ratio that β is brilliant α is brilliant low 10-20 DEG C, and therefore, hot sealing layer has lower melt temperature and heat-sealing temperature；On the other hand, β crystalline substance have more excellent Tensile toughness, toughness especially at low temperature.Therefore, the aluminum-plastic composite membrane of the present invention has broader heat-sealing temperature, more Toughness under low heat-sealing lower limit temperature, more excellent toughness especially low temperature environment.
The aluminum-plastic composite membrane of the present invention can be used as the packaging material of lithium ion battery, and its initial heat-sealing temperature is relatively low, heat-sealing Temperature range width, can quickly seal and obtain higher heat seal strength, have excellent heat sealability, and have excellent Toughness especially low-temperature flexibility.
Brief description
Fig. 1 is the structural representation of preferred embodiment of the present invention 1-4 aluminum-plastic composite membrane；
Fig. 2 is the structural representation of preferred embodiment of the present invention 5-7 aluminum-plastic composite membrane.
Specific embodiment
Embodiment 1
With reference to Fig. 1, the present embodiment there is the aluminum-plastic composite membrane of excellent heat sealability and low-temperature flexibility from the inside to the outside successively Including hot sealing layer 1, the first adhesive layer 4, aluminium foil layer 2, the second adhesive layer 5 and external protection 3；Described hot sealing layer 1 is by curtain coating poly- third Alkene film is constituted, and the relative percentage that in cast polypropylene film, beta crystal accounts for the total crystalline portion of polypropylene is 57.8%；External protection 3 It is biaxial tension polyethylene terephthalate layer.
The preparation method of cast polypropylene film comprises the steps:
(1) by mass, it is equipped with following raw materials: beta crystal-type nucleater 0.02% (being calcium pimelate), nano silicon 3%, balance of polypropylene (wherein 80% is polypropylene homopolymer, and 16.98% is polypropylene copolymer)；
The mean isotactic regularity of described polypropylene homopolymer is 85.3% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 151 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 5g/10min (using meeting The Melt Flow Rate Measurer of din53735 standard, measures under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 7.1wt%；
The mean isotactic regularity of described polypropylene copolymer is 63.4% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 132 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 7g/10min (using meeting The Melt Flow Rate Measurer of din53735 standard, measures under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 13.8wt%；
(2) polypropylene is added together with beta crystal-type nucleater extruder carry out kneading, extrude, and through being cast chill roll stream Prolong film forming, the temperature of extruder barrel is 180-200 DEG C, and the temperature of extrusion die is 230 DEG C, the temperature of curtain coating chill roll is 65 DEG C, obtain described cast polypropylene film.
Measured by wide-angle x-ray diffraction instrument (waxd) and (formula: k is calculated according to turner-jones formulaβ=h (β)/(h (β)+h (α)) × 100%, wherein kβFor the relative amount of beta crystal, beta crystal diffraction maximum in h (β) expression waxd collection of illustrative plates Height, h (α) represent waxd collection of illustrative plates in each alpha-crystal form diffraction maximum height sum), in above-mentioned cast polypropylene film beta crystal account for poly- The relative percentage of the total crystalline portion of propylene is 57.8%.
Embodiment 2
With reference to Fig. 1, the present embodiment there is the aluminum-plastic composite membrane of excellent heat sealability and low-temperature flexibility from the inside to the outside successively Including hot sealing layer 1, the first adhesive layer 4, aluminium foil layer 2, the second adhesive layer 5 and external protection 3；Described hot sealing layer 1 is by curtain coating poly- third Alkene film is constituted, and the relative percentage that in cast polypropylene film, beta crystal accounts for the total crystalline portion of polypropylene is 65.7%；External protection 3 It is two-way stretching polyamide layer.
The preparation method of cast polypropylene film comprises the steps:
(1) by mass, it is equipped with following raw materials: beta crystal-type nucleater 0.3% (it is n, n- dicyclohexyl -2,6,-naphthalene two Carboxylic acid amides), nano silicon 3%, (wherein 90% is polypropylene homopolymer to balance of polypropylene, and 6.7% is Polypropylene copolymer Thing)；
The mean isotactic regularity of described polypropylene homopolymer is 94.3% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 153 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 3.5g/10min (using symbol Close the Melt Flow Rate Measurer of din53735 standard, measure under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 5.1wt%；
The mean isotactic regularity of described polypropylene copolymer is 70.6% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 137 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 10g/10min (using meeting The Melt Flow Rate Measurer of din53735 standard, measures under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 11.8wt%；
(2) polypropylene is added together with beta crystal-type nucleater extruder carry out kneading, extrude, and through being cast chill roll stream Prolong film forming, the temperature of extruder barrel is 240-260 DEG C, and the temperature of extrusion die is 280 DEG C, the temperature of curtain coating chill roll is 60 DEG C, obtain described cast polypropylene film.
Measured by wide-angle x-ray diffraction instrument (waxd) and (formula: k is calculated according to turner-jones formulaβ=h (β)/(h (β)+h (α)) × 100%, wherein kβFor the relative amount of beta crystal, beta crystal diffraction maximum in h (β) expression waxd collection of illustrative plates Height, h (α) represent waxd collection of illustrative plates in each alpha-crystal form diffraction maximum height sum), in above-mentioned cast polypropylene film beta crystal account for poly- The relative percentage of the total crystalline portion of propylene is 65.7%.
Embodiment 3
With reference to Fig. 1, the present embodiment there is the aluminum-plastic composite membrane of excellent heat sealability and low-temperature flexibility from the inside to the outside successively Including hot sealing layer 1, the first adhesive layer 4, aluminium foil layer 2, the second adhesive layer 5 and external protection 3；Described hot sealing layer 1 is by curtain coating poly- third Alkene film is constituted, and the relative percentage that in cast polypropylene film, beta crystal accounts for the total crystalline portion of polypropylene is 40.7%；External protection 3 It is biaxial tension polyethylene terephthalate layer.
The preparation method of cast polypropylene film comprises the steps:
(1) by mass, it is equipped with following raw materials: beta crystal-type nucleater 0.5% (wherein 0.3% is gamma-quinacridinelone, 0.2% is dihydro quinacridine), nano silicon 3%, balance of polypropylene (wherein 70% is polypropylene homopolymer, 26.5% For polypropylene copolymer)；
The mean isotactic regularity of described polypropylene homopolymer is 80.7% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 145 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 7g/10min (using meeting The Melt Flow Rate Measurer of din53735 standard, measures under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 10.1wt%；
The mean isotactic regularity of described polypropylene copolymer is 55.6% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 132 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 18g/10min (using meeting The Melt Flow Rate Measurer of din53735 standard, measures under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 17.8wt%；
(2) polypropylene is added together with beta crystal-type nucleater extruder carry out kneading, extrude, and through being cast chill roll stream Prolong film forming, the temperature of extruder barrel is 220-240 DEG C, and the temperature of extrusion die is 250 DEG C, the temperature of curtain coating chill roll is 40 DEG C, obtain described cast polypropylene film.
Measured by wide-angle x-ray diffraction instrument (waxd) and (formula: k is calculated according to turner-jones formulaβ=h (β)/(h (β)+h (α)) × 100%, wherein kβFor the relative amount of beta crystal, beta crystal diffraction maximum in h (β) expression waxd collection of illustrative plates Height, h (α) represent waxd collection of illustrative plates in each alpha-crystal form diffraction maximum height sum), in above-mentioned cast polypropylene film beta crystal account for poly- The relative percentage of the total crystalline portion of propylene is 40.7%.
Embodiment 4
With reference to Fig. 1, the present embodiment there is the aluminum-plastic composite membrane of excellent heat sealability and low-temperature flexibility from the inside to the outside successively Including hot sealing layer 1, the first adhesive layer 4, aluminium foil layer 2, the second adhesive layer 5 and external protection 3；Described hot sealing layer 1 is by curtain coating poly- third Alkene film is constituted, and the relative percentage that in cast polypropylene film, beta crystal accounts for the total crystalline portion of polypropylene is 72.9%；External protection 3 It is two-way stretching polyamide layer.
The preparation method of cast polypropylene film comprises the steps:
(1) by mass, it is equipped with following raw materials: beta crystal-type nucleater 2% (being calcium phthalate), nanometer titanium dioxide Silicon 3%, balance of polypropylene (wherein 90% is polypropylene homopolymer, and 5% is polypropylene copolymer)；
The mean isotactic regularity of described polypropylene homopolymer is 98% (being measured by [carbon] NMR (Nuclear Magnetic Resonance) spectrum), Fusing point is 160 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 4.0g/10min (using meeting The Melt Flow Rate Measurer of din53735 standard, measures under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 2.1wt%；
The mean isotactic regularity of described polypropylene copolymer is 77.5% (by the survey of [carbon] NMR (Nuclear Magnetic Resonance) spectrum Fixed), fusing point is 140 DEG C (being measured by differential scanning calorimeter (dsc)), and melt flow index is 7.0g/10min (using symbol Close the Melt Flow Rate Measurer of din53735 standard, measure under 230 DEG C and 2.16kg load), the solvable sex ratio of normal heptane is 9.8wt%；
(2) polypropylene is added together with beta crystal-type nucleater extruder carry out kneading, extrude, and through being cast chill roll stream Prolong film forming, the temperature of extruder barrel is 230-250 DEG C, and the temperature of extrusion die is 260 DEG C, the temperature of curtain coating chill roll is 70 DEG C, obtain described cast polypropylene film.
Measured by wide-angle x-ray diffraction instrument (waxd) and (formula: k is calculated according to turner-jones formulaβ=h (β)/(h (β)+h (α)) × 100%, wherein kβFor the relative amount of beta crystal, beta crystal diffraction maximum in h (β) expression waxd collection of illustrative plates Height, h (α) represent waxd collection of illustrative plates in each alpha-crystal form diffraction maximum height sum), in above-mentioned cast polypropylene film beta crystal account for poly- The relative percentage of the total crystalline portion of propylene is 72.9%.
Embodiment 5
With reference to Fig. 2, in the present embodiment, the inner surface of aluminium foil layer 2 has the first stearic acid film layer 6, the first stearic acid Film layer 6 is connected with hot sealing layer 1 by the first adhesive layer 4, and the outer surface of aluminium foil layer 2 has the second stearic acid film layer 7, and second Stearic acid film layer 7 is connected with external protection 3 by the second adhesive layer 5.
First stearic acid film layer 6, the side of the second stearic acid film layer 7 are formed on the inner surface, outer surface of aluminium foil layer 2 Method comprises the steps: successively
Hydrochloric acid-oxalic acid that aluminium foil (aluminium foil used is the alloy foil that thickness is 35 μm) immersion temperature is 25 DEG C is mixed by (1 ') Close in solution, soak 1min；
Every liter of hydrochloric acid-oxalic acid mixed solution is formed by the preparation of raw material of following ratios: 7.2 grams of oxalic acid, and 5 grams of concentrated hydrochloric acid is remaining Measure as water；
Aluminium foil is taken out from hydrochloric acid-oxalic acid mixed solution and immerses in the potassium permanganate solution that temperature is 25 DEG C by (2 '), Soak 1min；
Every liter of potassium permanganate solution contains: 15.8 grams of potassium permanganate, balance of water；
Aluminium foil is taken out from potassium permanganate solution by (3 '), after being cleaned aluminium foil with water, then aluminium foil is dried (at 75 DEG C Dry)；
Form the granular layer of loose structure micro-, that nanometer is alternate in aluminium foil surface, the hole depth of this loose structure granular layer is about 1-2 μm, about 1 μm of aperture, about 15-20 μm of pitch of holes；
Aluminium foil immersion mass percent concentration is in 0.5% stearic acid ethanol solution by (4 '), soaks 5 minutes；Then Aluminium foil is taken out from stearic acid ethanol solution and (with 60 DEG C hot air dryings) is dried, in inner surface, the outer surface of aluminium foil Upper form the first stearic acid film layer 6, the second stearic acid film layer 7 respectively, described aluminium foil constitutes the aluminium foil layer 2 of aluminum-plastic composite membrane；
First stearic acid film layer 6, aluminium foil layer 2 and the second stearic acid film layer 7 composition superhydrophobic aluminum foil.After tested, first is hard Fat acid film layer 6, the second stearic acid film layer 7 and the contact angle of water are 153 ± 2.0 °, and water droplet roll angle is 9 °；First Hard Fat Sorrel layer 6, the thickness of the second stearic acid film layer 7 are each about 5 μm.
Remaining feature of the present embodiment is same as Example 1.
Embodiment 6
With reference to Fig. 2, in the present embodiment, the inner surface of aluminium foil layer 2 has the first stearic acid film layer 6, the first stearic acid Film layer 6 is connected with hot sealing layer 1 by the first adhesive layer 4, and the outer surface of aluminium foil layer 2 has the second stearic acid film layer 7, and second Stearic acid film layer 7 is connected with external protection 3 by the second adhesive layer 5.
First stearic acid film layer 6, the side of the second stearic acid film layer 7 are formed on the inner surface, outer surface of aluminium foil layer 2 Method comprises the steps: successively
In the present embodiment, the preparation method of aluminum-plastic composite membrane comprises the steps:
Hydrochloric acid-oxalic acid that aluminium foil (aluminium foil used is the alloy foil that thickness is 45 μm) immersion temperature is 20 DEG C is mixed by (1 ') Close in solution, soak 0.8min；
Every liter of hydrochloric acid-oxalic acid mixed solution is formed by the preparation of raw material of following ratios: 7.2 grams of oxalic acid, and 20 grams of concentrated hydrochloric acid is remaining Measure as water；
Aluminium foil is taken out from hydrochloric acid-oxalic acid mixed solution and immerses in the potassium permanganate solution that temperature is 20 DEG C by (2 '), Soak 1.5min；
Every liter of potassium permanganate solution contains: 31.6 grams of potassium permanganate, balance of water；
Aluminium foil is taken out from potassium permanganate solution by (3 '), after being cleaned aluminium foil with water, then aluminium foil is dried (at 70 DEG C Dry)；
Form the granular layer of loose structure micro-, that nanometer is alternate in aluminium foil surface, the hole depth of this loose structure granular layer is about 2-5 μm, about 2 μm of aperture, about 5-10 μm of pitch of holes；
Aluminium foil immersion mass percent concentration is in 1% stearic acid ethanol solution by (4 '), soaks 5 minutes；Then will Aluminium foil takes out from stearic acid ethanol solution and (with 50 DEG C hot air dryings) is dried, on the inner surface, outer surface of aluminium foil Form the first stearic acid film layer, the second stearic acid film layer respectively, described aluminium foil constitutes the aluminium foil layer of aluminum-plastic composite membrane；
First stearic acid film layer, aluminium foil layer and the second stearic acid film layer composition superhydrophobic aluminum foil.After tested, the first stearic acid The contact angle of film layer, the second stearic acid film layer and water is 167 ± 1.8 °, and water droplet roll angle is 6 °；First stearic acid film layer, The thickness of the second stearic acid film layer is each about 8 μm.
Remaining feature of the present embodiment is same as Example 2.
Embodiment 7
With reference to Fig. 2, in the present embodiment, the inner surface of aluminium foil layer 2 has the first stearic acid film layer 6, the first stearic acid Film layer 6 is connected with hot sealing layer 1 by the first adhesive layer 4, and the outer surface of aluminium foil layer 2 has the second stearic acid film layer 7, and second Stearic acid film layer 7 is connected with external protection 3 by the second adhesive layer 5.
First stearic acid film layer 6, the side of the second stearic acid film layer 7 are formed on the inner surface, outer surface of aluminium foil layer 2 Method comprises the steps: successively
In the present embodiment, the preparation method of aluminum-plastic composite membrane comprises the steps:
Hydrochloric acid-oxalic acid that aluminium foil (aluminium foil used is the alloy foil that thickness is 50 μm) immersion temperature is 30 DEG C is mixed by (1 ') Close in solution, soak 0.5min；
Every liter of hydrochloric acid-oxalic acid mixed solution is formed by the preparation of raw material of following ratios: 20 grams of oxalic acid, and 100 grams of concentrated hydrochloric acid is remaining Measure as water；
Aluminium foil is taken out from hydrochloric acid-oxalic acid mixed solution and immerses in the potassium permanganate solution that temperature is 30 DEG C by (2 '), Soak 2min；
Every liter of potassium permanganate solution contains: 7.9 grams of potassium permanganate, balance of water；
Aluminium foil is taken out from potassium permanganate solution by (3 '), after being cleaned aluminium foil with water, then aluminium foil is dried (at 80 DEG C Dry)；
(hole depth of this loose structure granular layer is about to form the granular layer of loose structure micro-, that nanometer is alternate in aluminium foil surface 4-5 μm, about 1-2 μm of aperture, about 15-20 μm of pitch of holes)；
Aluminium foil immersion mass percent concentration is in 0.1% stearic acid ethanol solution by (4 '), soaks 10 minutes；Then Aluminium foil is taken out from stearic acid ethanol solution and (with 70 DEG C hot air dryings) is dried, in inner surface, the outer surface of aluminium foil Upper form the first stearic acid film layer, the second stearic acid film layer respectively, described aluminium foil constitutes the aluminium foil layer of aluminum-plastic composite membrane；
First stearic acid film layer, aluminium foil layer and the second stearic acid film layer composition superhydrophobic aluminum foil.After tested, the first stearic acid The contact angle of film layer, the second stearic acid film layer and water is 161 ± 1.8 °, and water droplet roll angle is 8 °；First stearic acid film layer, The thickness of the second stearic acid film layer is each about 7 μm.
Remaining feature of the present embodiment is same as Example 3.
The performance of the aluminum-plastic composite membrane of embodiment 1-4 is tested, test result is as shown in table 1 below.
Table 1: the aluminum-plastic composite membrane the performance test results of embodiment 1-4
The performance of the aluminum-plastic composite membrane of embodiment 5-7 is tested, test result is as shown in table 2 below.
Table 2: the aluminum-plastic composite membrane the performance test results of embodiment 5-7

Claims (10)

1. a kind of aluminum-plastic composite membrane with excellent heat sealability and low-temperature flexibility is it is characterised in that include heat from the inside to the outside successively Sealing, the first adhesive layer, aluminium foil layer, the second adhesive layer and external protection；Described hot sealing layer is made up of cast polypropylene film, curtain coating The relative percentage that in polypropylene screen, beta crystal accounts for the total crystalline portion of polypropylene is 30-99%；Described external protection is biaxial tension Polyethylene terephthalate layer or two-way stretching polyamide layer.
2. aluminum-plastic composite membrane according to claim 1, is characterized in that: in described cast polypropylene film, beta crystal accounts for polypropylene The relative percentage of total crystalline portion is 40-70%.
3. aluminum-plastic composite membrane according to claim 1 and 2 is it is characterised in that the preparation method bag of described cast polypropylene film Include following step:
(1) by mass, it is equipped with following raw materials: beta crystal-type nucleater 0.01-10%, nano silicon 0.1-10%, balance of poly- Propylene；
Described polypropylene is one of polypropylene homopolymer and polypropylene copolymer or both mixture；
The mean isotactic regularity of described polypropylene homopolymer and polypropylene copolymer is all located in the range of 55-99%；Institute State polypropylene homopolymer and the fusing point of polypropylene copolymer is 130-170 DEG C；Described polypropylene homopolymer and Polypropylene copolymer The melt flow index of thing is 0.1-25g/10min；The normal heptane of described polypropylene homopolymer and polypropylene copolymer is solvable Sex ratio is below 20wt%；
(2) polypropylene is added together with beta crystal-type nucleater extruder carry out kneading, extrude, and be cast into through curtain coating chill roll Film, the temperature of extruder barrel is 180-260 DEG C, and the temperature of extrusion die is 200-280 DEG C, and the temperature of curtain coating chill roll is 30-80 DEG C, obtain described cast polypropylene film.
4. aluminum-plastic composite membrane according to claim 3, is characterized in that: in step (1), the percent mass of provisioned raw material Than for beta crystal-type nucleater 0.02-5%, nano silicon 1-5%, balance of polypropylene.
5. aluminum-plastic composite membrane according to claim 3, is characterized in that: in step (2), the temperature of curtain coating chill roll is 40- 70℃.
6. aluminum-plastic composite membrane according to claim 3, is characterized in that: described polypropylene homopolymer and polypropylene copolymer Melt flow index is 0.5-10g/10min.
7. aluminum-plastic composite membrane according to claim 3, is characterized in that: described beta crystal-type nucleater is calcium pimelate, suberic acid Calcium, n, n- dicyclohexyl -2,6,-naphthalene dicarboxamide, n, n- dicyclohexyl terephthalamide, gamma-quinacridinelone, dihydro quinoline a word used for translation One of pyridine and calcium phthalate or many of mixture.
8. aluminum-plastic composite membrane according to claim 1 and 2, is characterized in that: has on the inner surface of described aluminium foil layer Monostearate film layer, the first stearic acid film layer is connected with described hot sealing layer by the first adhesive layer, on the outer surface of aluminium foil layer There is the second stearic acid film layer, the second stearic acid film layer is connected with described external protection by the second adhesive layer.
9. aluminum-plastic composite membrane according to claim 8, is characterized in that: shape on the inner surface, outer surface of aluminium foil layer The first stearic acid film layer, the method for the second stearic acid film layer is become to comprise the steps: successively
(1 ') immerses aluminium foil in hydrochloric acid-oxalic acid mixed solution that temperature is 20-30 DEG C, soaks 0.5-2min；
Every liter of hydrochloric acid-oxalic acid mixed solution is formed by the preparation of raw material of following ratios: 5-20 gram of oxalic acid, and 5-100 gram of concentrated hydrochloric acid is remaining Measure as water；
Aluminium foil is taken out from hydrochloric acid-oxalic acid mixed solution and immerses in the potassium permanganate solution that temperature is 20-30 DEG C by (2 '), leaching Bubble 1-2min；
Every liter of potassium permanganate solution contains: 5-32 gram of potassium permanganate, balance of water；
Aluminium foil is taken out from potassium permanganate solution by (3 '), after being cleaned aluminium foil with water, then aluminium foil is dried；
(4 ') immerse aluminium foil in the stearic acid ethanol solution that mass percent concentration is 0.1-1%, soak 1-10 minute；Then Aluminium foil is taken out from stearic acid ethanol solution and is dried, the inner surface, outer surface of aluminium foil form first respectively hard Fat acid film layer, the second stearic acid film layer, described aluminium foil constitutes the aluminium foil layer of aluminum-plastic composite membrane.
10. aluminum-plastic composite membrane according to claim 9, is characterized in that: in step (1 '), aluminium foil used is thickness is 30- 50 μm of alloy foil.
CN201610944914.2A 2016-11-02 2016-11-02 Aluminum plastic compound film with excellent heat sealing property and low-temperature flexibility Pending CN106356474A (en)

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CN108656491A (en) * 2018-04-24 2018-10-16 苏州融达信新材料科技有限公司 A kind of preparation process and its equipment of novel aluminum-plastic composite membrane
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CN111244335A (en) * 2020-01-20 2020-06-05 江西明冠锂膜技术有限公司 Method for reducing surface friction of aluminum-plastic film and aluminum-plastic film prepared by method
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CN106784434A (en) * 2017-03-27 2017-05-31 贺万军 A kind of aluminum plastic film
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CN108656491A (en) * 2018-04-24 2018-10-16 苏州融达信新材料科技有限公司 A kind of preparation process and its equipment of novel aluminum-plastic composite membrane
CN109228575A (en) * 2018-10-30 2019-01-18 上海恩捷新材料科技有限公司 A kind of plastic-aluminum membrane structure
CN109897565A (en) * 2018-12-19 2019-06-18 上海奥威科技开发有限公司 The anti-battery aluminum plastic film for crossing envelope
CN111244335A (en) * 2020-01-20 2020-06-05 江西明冠锂膜技术有限公司 Method for reducing surface friction of aluminum-plastic film and aluminum-plastic film prepared by method
CN111244335B (en) * 2020-01-20 2021-12-10 江西明冠锂膜技术有限公司 Method for reducing surface friction of aluminum-plastic film and aluminum-plastic film prepared by method
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