CN108822750A - A kind of polyolefin packaging adhesive film with self-repair function - Google Patents
A kind of polyolefin packaging adhesive film with self-repair function Download PDFInfo
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- CN108822750A CN108822750A CN201810329859.5A CN201810329859A CN108822750A CN 108822750 A CN108822750 A CN 108822750A CN 201810329859 A CN201810329859 A CN 201810329859A CN 108822750 A CN108822750 A CN 108822750A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C09J123/0815—Copolymers of ethene with aliphatic 1-olefins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/04—Homopolymers or copolymers of ethene
- C09J123/08—Copolymers of ethene
- C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C09J123/0853—Vinylacetate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/322—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of solar panels
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
-
- 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
- C09J2423/00—Presence of polyolefin
- C09J2423/04—Presence of homo or copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2483/00—Presence of polysiloxane
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
A kind of disclosed polyolefin packaging adhesive film with self-repair function, including following components in terms of mass fraction, 80-100 parts of packaging adhesive film substrate POE, 8-15 parts of supermolecule self-healing function compound, 0.5-2.0 parts of crosslinking agent, 0.2-2.0 parts of antioxidant, 0.02-1.0 parts of UV light stabilizing agent, 0.5-2.0 parts of tackifier, wherein supermolecule self-healing function compound is formed by the polysiloxanes or polysilsesquioxane monomer autohemagglutination of olefin-containing amide, has crosslinking net macromolecular structure.Hydrogen bond with reversible nature is introduced into glue film resin material by the present invention, has the supermolecule cross-linked network of three-dimensional body structure by hydrogen bond building, assigns the repeatable processing of material, can the properties such as active self-healing.
Description
Technical field
The invention belongs to packaging adhesive film for solar cell fields, and in particular to a kind of polyolefin envelope with self-repair function
Fill glue film.
Background technique
Packaging adhesive film for solar cell is largely EVA adhesive film at present, and light-heat aging easily occurs when in use and decomposes by EVA,
Xanthochromia occurs for appearance, causes encapsulation performance to decline, has seriously affected the light transmittance of glue film and the service life of solar battery, phase
Be compared to ethylene-vinyl acetate copolymer (EVA) encapsulating material, polyolefin POE packaging adhesive film material have it is good it is weather-proof,
Anti-ultraviolet ageing performance and excellent heat-resisting, resistance to low temperature, use temperature range is wide, and since its good light penetrates
Rate, excellent electrical insulation capability have a good application prospect in terms of photovoltaic industry encapsulating material.
Polyolefine material often increases the bonding energy of itself and material to be bonded body (such as glass) by grafting of polar monomers group
Power.103289582 B of Chinese invention patent CN discloses a kind of POE solar photovoltaic assembly packaging adhesive film of cross-linking type, this
The main ingredient of kind packaging adhesive film is the POE resin of Silane Grafted, while also containing crosslinking agent, cross-linking aid, age resister etc.
Auxiliary agent, preparation method are the POE resin for first preparing Silane Grafted, then the POE of grafting are passed through with auxiliary agent after evenly mixing crowded
Machine is cast to obtain glue film of the invention out, is implemented to test the cohesive force of the glue film and backboard or glass in 40N/cm or more.
5281670 A of U.S. patent Nos US discloses through grafted maleic anhydride the adhesive property for improving polyolefin.Chinese invention
105860174 B of patent CN discloses a kind of XNBR vulcanization of rubber glue and preparation method thereof with self-healing properties, utilizes cream
Liquid is blended, and after PVA solution is blended with XNBR latex, aminated compounds, vulcanizing agent and promotor is added, and passes through vulcanization processing system
It is standby go out the XNBR vulcanization of rubber glue containing PVA, while using the fracture of the hydrogen bond formed between PVA and aminated compounds be bonded again
Process improves the mechanical strength and self-reparing capability of XNBR.
Mostly to improve glue film with the cohesive force of backboard or glass as final purpose in current existing technical solution, but work as
When phenomena such as glue film itself damaged such as slight crack occurs or is broken, the very fast decline of bonding peeling force, another party on the one hand will cause
Face to increase a possibility that it is damaged, so that final encapsulation component utilization rate and making in material to be encapsulated exposure external environment
With efficiency sharp fall.And using existing recovery technique come online repair breakage or the slight crack of packaging adhesive film the defects of, one
Aspect operation sequence complexity is cumbersome, and another aspect rehabilitation cost is higher, greatly reduces the service efficiency of package assembling.
Summary of the invention
The problem to be solved in the present invention is to provide a kind of polyolefin packaging adhesive film with self-repair function, will have reversible
The hydrogen bond of property is introduced into glue film resin material, has the supermolecule cross-linked network of three-dimensional body structure by hydrogen bond building,
Assign the repeatable processing of material, can the properties such as active self-healing.
To achieve the above object, the technical solution adopted by the present invention is as follows:A kind of polyolefin envelope with self-repair function
Glue film is filled, including following components, 80-100 parts of packaging adhesive film substrate POE, supermolecule self-healing function in terms of mass fraction
Object 8-15 parts of conjunction, 0.5-2.0 parts of crosslinking agent, 0.2-2.0 parts of antioxidant, 0.02-1.0 parts of UV light stabilizing agent, tackifier
0.5-2.0 parts, wherein supermolecule self-healing function compound by olefin-containing amide polysiloxanes or polysilsesquioxane list
Body autohemagglutination forms, and has crosslinking net macromolecular structure, wherein the polysiloxanes of olefin-containing amide or polysilsesquioxane monomer
Structural unit be expressed as:
Wherein-R1For one of following structural formula,
Wherein-R- is one of following structural formula,
The packaging adhesive film substrate POE is ethylene-propylene copolymer, ethylene-butene-1 copolymer, ethylene -1- octene are total
Polymers, ethylene-isobutylene copolymers, ethylene -1- hexene copolymer, ethylene -1- heptene copolymer, ethylene -1- nonene copolymer,
One or more mixtures of ethylene -1- decene copolymer, wherein the melt flow index of packaging adhesive film POE is 0.5-
40g/10min, light transmittance >=80%.
The preparation method of the supermolecule self-healing function compound is:
Under the conditions of being stirred at room temperature, the polysiloxanes for having active amino structure or polysilsesquioxane are dissolved in methylene chloride
In solution, alkene acyl chlorides base class compound, activator are sequentially added, at room temperature 24~48h of synthetic reaction, wherein amino structure
The molar ratio of polysiloxanes or polysilsesquioxane and alkene acyl chlorides base class compound is 1: 2-10, activator and alkene acid chloride group
The mass ratio of class compound is 1: 15-25, and after synthetic reaction, alkali in 0.1-1mol/L sodium hydroxide solution is added in material
It washes, adds in 0.5-1mol/L dilute hydrochloric acid solution that salt is washed in pickling and 0.5-1mol/L magnesium chloride solution, then layering, organic
Mutually supermolecule self-healing function compound is obtained after drying, removal solvent.
The alkene acyl chlorides base class compound is the monomer containing olefin group and acid chloride group, specially acryloyl simultaneously
Chlorine, methacrylic chloride, 2- methyl -3- phenyl -2- acryloyl chloride, beta-phenyl acryloyl chloride, 2- crotonyl chloride, 3- methyl -2-
Crotonyl chloride, 3- crotonyl chloride, 4- prenyl chloride or 2,2- dimethyl -3- (2- methyl-1-propylene base)-cyclopropanecarbonyl chloride.
The activator is one of carbodiimide, n,N-diisopropylethylamine, pentamethyl-diethylenetriamine.
The polysiloxanes or polysilsesquioxane with active amino structure is at least two Amino End Group structures
Siloxanes or silesquioxane compound, bis- (3- aminopropyl) tetramethyl disiloxanes of specially 1,3-, bis- (the 4- ammonia of 1,3-
Base butyl) tetramethyl disiloxane, Amino End Group dimethyl silicone polymer, amino cage modle polysilsesquioxane (POSS- (R2')nN=
2,3 ... 12), and structural formula is respectively:
The amino cage modle polysilsesquioxane (POSS- (R2')nN=2,3 ... 12) in, POSS be pentahedron, six faces
One of body, heptahedron, octahedra silsesquioxane ,-R2' structure is such as one of flowering structure:
The crosslinking agent is organic peroxide class compound, preferably benzylhydroperoxide tert-pentyl ester, tert-butyl hydroperoxide benzene
Formic acid esters, tert-butyl hydroperoxide -2 ethyl hexanoic acid ester, tert-butyl hydroperoxide-butylperoxyisopropyl carbonate, tert-butyl hydroperoxide -3,5,
5- tri-methyl hexanoic acid ester, peroxide acid tert-amyl acetate, normal-butyl -4,4- bis- (tert-butyl hydroperoxide) valerate, ethyl -3,3-
The one or more of two (tert-butyl hydroperoxide) butyrates, tert-butyl hydroperoxide -2- ethylhexyl carbonate.
The antioxidant be benzophenone class, triazines, organophosphorus ester or phosphite ester compound, preferably three (2,
4- di-tert-butyl-phenyl) phosphite ester, β-(4- hydroxyl -3,5- di-tert-butyl-phenyl) propionic acid n-octadecyl alcohol ester, three (nonyl benzenes
Base) phosphite ester, three (2,4- di-tert-butyl-phenyl) phosphite esters, four-(4- hydroxyl -3,5- butyl phenyl propionic acid) pentaerythrites
Ester, distearyl pentaerythrityl diphosphite, three (1,2,2,6,6- pentamethyl -4- piperidyl) phosphite esters, decanedioic acid be double -
2,2,6,6- tetramethyl piperidine alcohol esters, bis- (1,2,2,6,6- pentamethyl -4- piperidyl) sebacates, 2,6- di-t-butyl are to first
Base phenol, pentaerythritol bis-phosphite two (octadecyl alcolol) ester, 3,5- di-t-butyl -4- hydroxy-benzoic acid cetyl ester.
The UV light stabilizing agent is dihydroxy -4- methoxy benzophenone, 2- (2 '--5 '-aminomethyl phenyl of hydroxyl) benzo
Triazole, 2-hydroxy-4-n-octoxybenzophenone, 4-HBA -2,4- 6- di-tert-butyl phenyl ester, 2- hydroxyl -4- methoxyl group -
2 '-carboxyl benzophenones, 2- (2 '--4 '-hydroxy phenyl of methyl) benzotriazole, 2- hydroxyl -5- chlorobenzophenone, 2,2 '-four Asias
Methyl bis- (3,1- benzoxazine -4- ketone), 2- hydroxyl -4- benzoyl oxygroup benzophenone, 2- (bis- uncle penta of 2- hydroxyl -3,5-
Base phenyl) benzotriazole, 2, one or more kinds of mixtures of 2 ', 4,4 '-tetrahydroxybenzophenones.
The tackifier are silane coupling agent, preferably 3- aminopropyl trimethoxysilane, three ethoxy of 3- aminopropyl
Base silane, 4- ammobutyltriethoxysilane, N- aminoethyl -3- aminopropyl triethoxysilane, aminophenyl triethoxy
Silane, N- (normal-butyl)-aminopropyl trimethoxysilane, 4- amino -3,3- dimethylbutyl trimethoxy silane, anilinomethyl
Triethoxysilane, methacryloxypropyl trimethoxy silane, the vinyltrimethoxysilane, (β-first of vinyl three
Oxygroup ethyoxyl) silane, one of vinyltriethoxysilane.
There is the polyolefin packaging adhesive film of active self-repair function the present invention provides a kind of excellent in mechanical performance and simultaneously
Material, using reactive extrusion copolymerization by the way of by self-healing function material introduce POE polymer molecular chain on, on the one hand by
In the effect of polysiloxanes or POSS structure, enhance the cohesive force and stretching-fracture property of adhesive film material, on the other hand due to
The polysiloxanes or polysilsesquioxane monomer autohemagglutination of olefin amide act on, and hydrogen bond crosslinks net has been formd in POE polymer
Network, by the fracture and healing of hydrogen bond, assigning material has good self-reparing capability, when the glue film as encapsulating material by
It is cracked under varying environment and alternate stress effect, slight crack and when being broken, adhesive film material break surface exists largely not
The hydrogen-bond donor (C=O) and receptor (- N-H) of association, when break surface contacts and keep certain time, multiple hydrogen bonding donor (C
=O) and receptor (- N-H) can actively re-form hydrogen bond and recombinate constitute polymer macromolecule cross-linked network.
Beneficial effect:A kind of disclosed polyolefin packaging adhesive film with self-repair function, have has as follows
Beneficial effect:Hydrogen bond with reversible nature is introduced into glue film resin material, there is three-dimensional body structure by hydrogen bond building
Supermolecule cross-linked network, assign the repeatable processing of material, can the properties such as active self-healing, to reduce online reparation
The triviality of operation, and rehabilitation cost is reduced, improve the service life and efficiency of package assembling.
Detailed description of the invention
Fig. 1 is the intrinsic structural schematic diagram of polyolefin packaging adhesive film with self-repair function of the invention.
Specific embodiment
Below in conjunction with particular content of the invention, to the technical solution of the embodiment of the present invention carry out it is clear, completely retouch
It states.
The hydrogen bond for having reversible nature will be introduced into glue film resin material by the way of reactive extrursion copolymerization by the present invention
In, the supermolecule cross-linked network with three-dimensional body structure is constructed, while using the fracture of hydrogen bond and bonding process again, preparing
Polyolefin packaging adhesive film with good self-reparing capability (process is as shown in Figure 1).
A kind of polyolefin packaging adhesive film with self-repair function, including following components, packaging adhesive film in terms of mass fraction
80-100 parts of substrate POE, 8-15 parts of supermolecule self-healing function compound, 0.5-2.0 parts of crosslinking agent, antioxidant 0.2-
2.0 parts, 0.02-1.0 parts of UV light stabilizing agent, 0.5-2.0 parts of tackifier, wherein supermolecule self-healing function compound is by containing
The polysiloxanes or polysilsesquioxane monomer autohemagglutination of olefin amide form, and have crosslinking net macromolecular structure, wherein containing alkene
The polysiloxanes of hydrocarbon amide or the structural unit of polysilsesquioxane monomer are expressed as:
Wherein-R1For one of following structural formula,
Wherein-R- is one of following structural formula,
The packaging adhesive film substrate POE is ethylene-propylene copolymer, ethylene-butene-1 copolymer, ethylene -1- octene are total
Polymers, ethylene-isobutylene copolymers, ethylene -1- hexene copolymer, ethylene -1- heptene copolymer, ethylene -1- nonene copolymer,
One or more mixtures of ethylene -1- decene copolymer, wherein the melt flow index of packaging adhesive film POE is 0.5-
40g/10min, light transmittance >=80%.
Wherein the preparation method of the supermolecule self-healing function compound is:
Under the conditions of being stirred at room temperature, the polysiloxanes for having active amino structure or polysilsesquioxane are dissolved in methylene chloride
In solution, alkene acyl chlorides base class compound, activator are sequentially added, at room temperature 24~48h of synthetic reaction, wherein amino structure
The molar ratio of polysiloxanes or polysilsesquioxane and alkene acyl chlorides base class compound is 1: 2-10, activator and alkene acid chloride group
The mass ratio of class compound is 1: 15-25, and after synthetic reaction, alkali in 0.1-1mol/L sodium hydroxide solution is added in material
It washes, adds in 0.5-1mol/L dilute hydrochloric acid solution that salt is washed in pickling and 0.5-1mol/L magnesium chloride solution, then layering, organic
Mutually supermolecule self-healing function compound is obtained after drying, removal solvent.
The alkene acyl chlorides base class compound is the monomer containing olefin group and acid chloride group, specially acryloyl simultaneously
Chlorine, methacrylic chloride, 2- methyl -3- phenyl -2- acryloyl chloride, beta-phenyl acryloyl chloride, 2- crotonyl chloride, 3- methyl -2-
Crotonyl chloride, 3- crotonyl chloride, 4- prenyl chloride or 2,2- dimethyl -3- (2- methyl-1-propylene base)-cyclopropanecarbonyl chloride.
The activator is one of carbodiimide, n,N-diisopropylethylamine, pentamethyl-diethylenetriamine.
The polysiloxanes or polysilsesquioxane with active amino structure is at least two Amino End Group structures
Siloxanes or silesquioxane compound, bis- (3- aminopropyl) tetramethyl disiloxanes of specially 1,3-, bis- (the 4- ammonia of 1,3-
Base butyl) tetramethyl disiloxane, Amino End Group dimethyl silicone polymer, amino cage modle polysilsesquioxane (POSS- (R2 ')n n
=2,3 ... 12), and structural formula is respectively:
The amino cage modle polysilsesquioxane (POSS- (R2′)nN=2,3 ... 12) in, POSS be pentahedron, six faces
One of body, heptahedron, octahedra silsesquioxane ,-R2' structure is such as one of flowering structure:
The crosslinking agent is organic peroxide class compound, preferably benzylhydroperoxide tert-pentyl ester, tert-butyl hydroperoxide benzene
Formic acid esters, tert-butyl hydroperoxide -2 ethyl hexanoic acid ester, tert-butyl hydroperoxide-butylperoxyisopropyl carbonate, tert-butyl hydroperoxide -3,5,
5- tri-methyl hexanoic acid ester, peroxide acid tert-amyl acetate, normal-butyl -4,4- bis- (tert-butyl hydroperoxide) valerate, ethyl -3,3-
The one or more of two (tert-butyl hydroperoxide) butyrates, tert-butyl hydroperoxide -2- ethylhexyl carbonate.
The antioxidant be benzophenone class, triazines, organophosphorus ester or phosphite ester compound, preferably three (2,
4- di-tert-butyl-phenyl) phosphite ester, β-(4- hydroxyl -3,5- di-tert-butyl-phenyl) propionic acid n-octadecyl alcohol ester, three (nonyl benzenes
Base) phosphite ester, three (2,4- di-tert-butyl-phenyl) phosphite esters, four-(4- hydroxyl -3,5- butyl phenyl propionic acid) pentaerythrites
Ester, distearyl pentaerythrityl diphosphite, three (1,2,2,6,6- pentamethyl -4- piperidyl) phosphite esters, decanedioic acid be double -
2,2,6,6- tetramethyl piperidine alcohol esters, bis- (1,2,2,6,6- pentamethyl -4- piperidyl) sebacates, 2,6- di-t-butyl are to first
Base phenol, pentaerythritol bis-phosphite two (octadecyl alcolol) ester, 3,5- di-t-butyl -4- hydroxy-benzoic acid cetyl ester.
The UV light stabilizing agent is dihydroxy -4- methoxy benzophenone, 2- (2 '--5 '-aminomethyl phenyl of hydroxyl) benzo
Triazole, 2-hydroxy-4-n-octoxybenzophenone, 4-HBA -2,4- 6- di-tert-butyl phenyl ester, 2- hydroxyl -4- methoxyl group -
2 '-carboxyl benzophenones, 2- (2 '--4 '-hydroxy phenyl of methyl) benzotriazole, 2- hydroxyl -5- chlorobenzophenone, 2,2 '-four Asias
Methyl bis- (3,1- benzoxazine -4- ketone), 2- hydroxyl -4- benzoyl oxygroup benzophenone, 2- (bis- uncle penta of 2- hydroxyl -3,5-
Base phenyl) benzotriazole, 2, one or more kinds of mixtures of 2 ', 4,4 '-tetrahydroxybenzophenones.
The tackifier are silane coupling agent, preferably 3- aminopropyl trimethoxysilane, three ethoxy of 3- aminopropyl
Base silane, 4- ammobutyltriethoxysilane, N- aminoethyl -3- aminopropyl triethoxysilane, aminophenyl triethoxy
Silane, N- (normal-butyl)-aminopropyl trimethoxysilane, 4- amino -3,3- dimethylbutyl trimethoxy silane, anilinomethyl
Triethoxysilane, methacryloxypropyl trimethoxy silane, the vinyltrimethoxysilane, (β-first of vinyl three
Oxygroup ethyoxyl) silane, one of vinyltriethoxysilane.
The contents of the present invention are described in detail with several specific embodiments below:
Embodiment 1
(1) preparation of supermolecule self-healing function compound
Under the conditions of being stirred at room temperature, by 5mol 1, bis- (3- aminopropyl) tetramethyl disiloxanes of 3- are dissolved in 250ml dichloromethane
In alkane solution, 10mol acryloyl chloride, 2/3mol carbodiimide are sequentially added, for 24 hours, synthetic reaction terminates synthetic reaction at room temperature
Afterwards, alkali cleaning in 50ml 0.1mol/L sodium hydroxide solution is added in material, added in 50ml 0.5mol/L dilute hydrochloric acid solution
Salt is washed in pickling and 50ml 0.5mol/L magnesium chloride solution, and then layering, organic phase obtain oversubscription after drying, removal solvent
Sub- self-healing function compound.
(2) preparation of polyolefin packaging adhesive film
8 parts of supermolecule self-healing function compound, 0.5 part of friendship are added in 80 parts of packaging adhesive film ethylene-propylene copolymers
Connection agent tert-butyl hydroperoxide -2 ethyl hexanoic acid ester, 0.2 part of antioxidant three (2,4- di-tert-butyl-phenyl) phosphite ester, 0.02
Part UV light stabilizing agent 4-HBA -2,4- 6- di-tert-butyl phenyl ester, 0.5 part of three second of tackifier N- aminoethyl -3- aminopropyl
Oxysilane imports packaging adhesive film after evenly mixing and produces unit, by extrusion, the processes such as curtain coating, winds, cuts and can be obtained
Polyolefin packaging adhesive film.
Embodiment 2
(1) preparation of supermolecule self-healing function compound
Under the conditions of being stirred at room temperature, it is molten that tri- aminopropyl cage type octahedral polysilsesquioxane of 5mol is dissolved in 250ml methylene chloride
In liquid, 50mol 3- crotonyl chloride, 2mol n,N-diisopropylethylamine (DIPEA) are sequentially added, at room temperature synthetic reaction 48h,
After synthetic reaction, alkali cleaning in 50ml 1mol/L sodium hydroxide solution is added in material, adds the dilute salt of 50ml 1mol/L
Salt is washed in pickling and 50ml 1mol/L magnesium chloride solution in acid solution, and then layering, organic phase are after drying, removal solvent
To supermolecule self-healing function compound.
(2) preparation of polyolefin packaging adhesive film
15 parts, 2 parts of supermolecule self-healing function compound are added in 100 parts of packaging adhesive film ethylene -1- hexene copolymers
Crosslinking agent normal-butyl -4,4- bis- (tert-butyl hydroperoxide) valerate, double -2,2,6, the 6- tetramethyl piperazines of 2 parts of antioxidant decanedioic acid
Pyridine alcohol ester, 1 part of UV light stabilizing agent 2- hydroxyl -4- benzoyl oxygroup benzophenone, 2 parts of tackifier methacryloxies third
Base trimethoxy silane imports packaging adhesive film after evenly mixing and produces unit, by extrusion, the processes such as curtain coating, winds, cuts i.e.
Polyolefin packaging adhesive film can be obtained.
Embodiment 3
(1) preparation of supermolecule self-healing function compound
Under the conditions of being stirred at room temperature, by 5mol 1, bis- (4- aminobutyl) tetramethyl disiloxanes of 3- are dissolved in 250ml dichloromethane
In alkane solution, 25mol 4- prenyl chloride, 2mol pentamethyl-diethylenetriamine are sequentially added, at room temperature synthetic reaction 30h, synthesized
After reaction, alkali cleaning in 50ml 0.5mol/L sodium hydroxide solution is added in material, adds the dilute salt of 50ml 0.8mol/L
Salt is washed in pickling and 50ml 0.6mol/L magnesium chloride solution in acid solution, and then layering, organic phase are after drying, removal solvent
Obtain supermolecule self-healing function compound.
(2) preparation of polyolefin packaging adhesive film
10 parts of supermolecule self-healing function compound, 1 part of friendship are added in 95 parts of packaging adhesive film ethylene -1- decene copolymers
Join agent tert-butyl hydroperoxide -2- ethylhexyl carbonate, 1 part of antioxidant bis- (1,2,2,6,6- pentamethyl -4- piperidyl) last of the ten Heavenly stems
Two acid esters, 0.5 part of 2,2 '-tetramethylene of UV light stabilizing agent is bis- (3,1- benzoxazine -4- ketone), 1 part of tackifier 3- aminopropan
Ethyl triethoxy silicane alkane imports packaging adhesive film after evenly mixing and produces unit, by extrusion, the processes such as curtain coating, winds, cuts i.e.
Polyolefin packaging adhesive film can be obtained.
Embodiment 4
(1) preparation of supermolecule self-healing function compound
Under the conditions of being stirred at room temperature, by 2mol Amino End Group dimethyl silicone polymer, 3mol 1, bis- (4- aminobutyl) tetramethyls of 3-
Base disiloxane is dissolved in 250ml dichloromethane solution, and it is sub- to sequentially add 30mol 3- methyl-2-butene acyl chlorides, 2mol carbon two
After synthetic reaction, alkali in 50ml 0.5mol/L sodium hydroxide solution is added in material by amine, at room temperature synthetic reaction 48h
It washes, adds in 50ml 0.8mol/L dilute hydrochloric acid solution that salt is washed in pickling and 50ml 0.6mol/L magnesium chloride solution, then divide
Layer, organic phase obtain supermolecule self-healing function compound after drying, removal solvent.
(2) preparation of polyolefin packaging adhesive film
It is added in 40 parts of packaging adhesive film ethylene-propylene copolymers, 40 parts of packaging adhesive film ethylene-butene-1 copolymer mixtures
15 parts of supermolecule self-healing function compound, 0.1 part of crosslinking agent tert-butyl hydroperoxide-butylperoxyisopropyl carbonate, 0.3 part of tert-butyl
Peroxidating -3,5,5- tri-methyl hexanoic acid ester, 0.1 part of peroxide acid tert-amyl acetate, 1.5 parts of (2,4- bis- tertiary fourths of antioxidant three
Base phenyl) phosphite ester, 0.5 part of β-(4- hydroxyl -3,5- di-tert-butyl-phenyl) propionic acid n-octadecyl alcohol ester, 0.25 part of ultraviolet light
Stabilizer 2- (2 '--4 '-hydroxy phenyl of methyl) benzotriazole, 0.25 part of 2- hydroxyl -5- chlorobenzophenone, 0.25 part 2,2 '-four
Di-2-ethylhexylphosphine oxide (3,1- benzoxazine -4- ketone), 0.25 part of 2- hydroxyl -4- benzoyl oxygroup benzophenone, 0.5 part of tackifier N-
Aminoethyl -3- aminopropyl triethoxysilane, 0.5 part of aminophenyl triethoxysilane, 0.5 part of N- (normal-butyl)-aminopropyl
Trimethoxy silane imports packaging adhesive film after evenly mixing and produces unit, by extrusion, the processes such as curtain coating, winds, cuts
Obtain polyolefin packaging adhesive film.
Comparative example 1
The preparation method of implementation 1 is repeated according to specified each component number, but is not added using supermolecule self-healing function
Property compound.
Comparative example 2
The preparation method of implementation 2 is repeated according to specified each component number, but is not added using supermolecule self-healing function
Property compound.
Comparative example 3
The preparation method of implementation 3 is repeated according to specified each component number, but is not added using supermolecule self-healing function
Property compound.
Comparative example 4
The preparation method of implementation 4 is repeated according to specified each component number, but is not added using supermolecule self-healing function
Property compound.
The performance of polyolefin packaging adhesive film such as table 1 in embodiment,
Table 1:
Self-reparing capability=glue film is broken tensile strength/glue film initial tensile strength × 100% after selfreparing
The embodiment of the invention is described in detail above, but the content is only the preferable of the invention
Embodiment should not be considered as limiting the invention the practical range of creation.It is all according to made by the invention application range
Deng variation and improvement etc., belong within the patent covering scope of the invention.
Claims (10)
1. a kind of polyolefin packaging adhesive film with self-repair function, it is characterised in that:Including following components in terms of mass fraction,
80-100 parts of packaging adhesive film substrate POE, 8-15 parts of supermolecule self-healing function compound, 0.5-2.0 parts of crosslinking agent, antioxygen
0.2-2.0 parts of agent, 0.02-1.0 parts of UV light stabilizing agent, 0.5-2.0 parts of tackifier, wherein supermolecule self-healing function
It closes object to be formed by the polysiloxanes or polysilsesquioxane monomer autohemagglutination of olefin-containing amide, there is crosslinking net macromolecular structure,
Wherein the structural unit of the polysiloxanes of olefin-containing amide or polysilsesquioxane monomer is expressed as:
Wherein-R1For one of following structural formula,
Wherein-R- is one of following structural formula,
2. a kind of polyolefin packaging adhesive film with self-repair function according to claim 1, it is characterised in that:The envelope
Dress glue film substrate POE is ethylene-propylene copolymer, ethylene-butene-1 copolymer, ethylene-l-octane copolymer, ethylene-isobutyl
Alkene copolymer, ethylene -1- hexene copolymer, ethylene -1- heptene copolymer, ethylene -1- nonene copolymer, ethylene -1- decene are total
One or more mixtures of polymers, wherein the melt flow index of packaging adhesive film POE is 0.5-40g/10min, thoroughly
Light rate >=80%.
3. a kind of polyolefin packaging adhesive film with self-repair function according to claim 1, it is characterised in that:It is described super
The preparation method of molecule self-healing function compound is:
Under the conditions of being stirred at room temperature, the polysiloxanes for having active amino structure or polysilsesquioxane are dissolved in dichloromethane solution
In, alkene acyl chlorides base class compound, activator are sequentially added, at room temperature 24~48h of synthetic reaction, wherein the poly- silicon of amino structure
The molar ratio of oxygen alkane or polysilsesquioxane and alkene acyl chlorides base class compound is 1: 2-10, activator and alkene acyl chlorides base class
The mass ratio for closing object is 1: 15-25, and after synthetic reaction, alkali cleaning in 0.1-1mol/L sodium hydroxide solution is added in material,
Add in 0.5-1mol/L dilute hydrochloric acid solution that salt is washed in pickling and 0.5-1mol/L magnesium chloride solution, then layering, organic phase
Supermolecule self-healing function compound is obtained after drying, removal solvent.
4. a kind of polyolefin packaging adhesive film with self-repair function according to claim 3, it is characterised in that:The alkene
Hydrocarbon acyl chlorides base class compound is the monomer containing olefin group and acid chloride group simultaneously, specially acryloyl chloride, methacrylic chloride,
2- methyl -3- phenyl -2- acryloyl chloride, beta-phenyl acryloyl chloride, 2- crotonyl chloride, 3- methyl-2-butene acyl chlorides, 3- crotonoyl
Chlorine, 4- prenyl chloride or 2,2- dimethyl -3- (2- methyl-1-propylene base)-cyclopropanecarbonyl chloride.
5. a kind of polyolefin packaging adhesive film with self-repair function according to claim 3, it is characterised in that:The work
Agent is one of carbodiimide, n,N-diisopropylethylamine, pentamethyl-diethylenetriamine.
6. a kind of polyolefin packaging adhesive film with self-repair function according to claim 3, it is characterised in that:The band
The polysiloxanes or polysilsesquioxane of active amino structure are siloxanes or sesquialter at least two Amino End Group structures
Bis- (3- aminopropyl) tetramethyl disiloxanes of silicone compounds, specially 1,3-, bis- (4- aminobutyl) tetramethyls of 1,3-
Disiloxane, Amino End Group dimethyl silicone polymer, amino cage modle polysilsesquioxane (POSS- (R2')nN=2,3 ... 12),
Structural formula is respectively:
The amino cage modle polysilsesquioxane (POSS- (R2′)nN=2,3 ... 12) in, POSS be pentahedron, hexahedron,
One of heptahedron, octahedra silsesquioxane ,-R2' structure is such as one of flowering structure:
7. a kind of polyolefin packaging adhesive film with self-repair function according to claim 1, it is characterised in that:The friendship
Connection agent is organic peroxide class compound.
8. a kind of polyolefin packaging adhesive film with self-repair function according to claim 1, it is characterised in that:It is described anti-
Oxidant is benzophenone class, triazines, organophosphorus ester or phosphite ester compound.
9. a kind of polyolefin packaging adhesive film with self-repair function according to claim 1, it is characterised in that:The purple
Outer light stabilizer is dihydroxy -4- methoxy benzophenone, 2- (2 '--5 '-aminomethyl phenyl of hydroxyl) benzotriazole, 2- hydroxyl -4-
Oxy-octyl benzophenone, 4-HBA -2,4- 6- di-tert-butyl phenyl ester, 2- hydroxyl -4- methoxyl group -2 '-carboxyl hexichol first
Ketone, 2- (2 '--4 '-hydroxy phenyl of methyl) benzotriazole, 2- hydroxyl -5- chlorobenzophenone, bis- (3, the 1- benzene of 2,2 '-tetramethylenes
Bing oxazine -4- ketone), 2- hydroxyl -4- benzoyl oxygroup benzophenone, 2- (2- hydroxyl -3,5- di-tert-pentyl-phenyl) benzo three
Azoles, 2, one or more kinds of mixtures of 2 ', 4,4 '-tetrahydroxybenzophenones.
10. a kind of polyolefin packaging adhesive film with self-repair function according to claim 1, it is characterised in that:It is described
Tackifier be silane coupling agent.
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