CN113322013B - Co-extrusion synergistic transparent adhesive film and preparation method thereof - Google Patents

Co-extrusion synergistic transparent adhesive film and preparation method thereof Download PDF

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CN113322013B
CN113322013B CN202110495796.2A CN202110495796A CN113322013B CN 113322013 B CN113322013 B CN 113322013B CN 202110495796 A CN202110495796 A CN 202110495796A CN 113322013 B CN113322013 B CN 113322013B
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synergistic
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CN113322013A (en
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邵佳俊
苏丹
何儒琴
黄元旦
魏晓勇
周志英
辛灵敏
张德华
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Zhejiang Xiangbang Technology Co ltd
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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
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • 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
    • 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
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • 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
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
    • 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
    • C09J2301/20—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself
    • C09J2301/208—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive itself the adhesive layer being constituted by at least two or more adjacent or superposed adhesive layers, e.g. multilayer adhesive

Abstract

The invention discloses a synergistic co-extruded transparent adhesive film which consists of three large layers, wherein the outer layer is a special EVA layer, and the middle layer is a composite POE synergistic layer. The composite POE synergistic layer can be divided into a POE bonding filling layer and a super-refraction synergistic layer. The whole glue film is in a grid shape and can be divided into a synergistic area and a functional area. The synergistic area covers the area of the photovoltaic module cell, and the functional area covers the cell gap area of the photovoltaic module. The bonding filling layer in the synergistic layer plays a role in bonding, filling and special effect protection; the super-refraction layer can be in a spherical shape, a hemispherical shape, a cuboid shape, a pyramid shape and the like according to needs. When sunlight obliquely irradiates into the super-refraction layer of the synergistic adhesive film, due to the high refractivity of the super-refraction layer, part of sunlight originally irradiating the cell gap can be refracted to change the path and irradiate the cell area, so that the arrangement utilization rate of the sunlight is further increased, and the power generation efficiency of the packaging assembly is increased.

Description

Co-extrusion synergistic transparent adhesive film and preparation method thereof
Technical Field
The invention relates to a transparent adhesive film, in particular to a co-extrusion synergistic transparent adhesive film and a preparation method thereof.
Background
With the continuous development of science and technology, the global resource consumption is serious, the energy war has become the focus of attention of all countries around the world, solar energy is more and more concerned internationally as a renewable energy source, and the technology of the photovoltaic industry is changed day by day. The photovoltaic packaging adhesive film is an essential part of the photovoltaic module, and the module bears the most important protection function, so that a solid rear shield is provided for the normal operation of the photovoltaic module. With the continuous development of the technology, the whole photovoltaic packaging adhesive film is developed towards synergy and high aging resistance.
With the emergence of the PERC double-sided technology, the photovoltaic industry has entered a completely new field. The double-sided battery realizes the double-sided power generation function through a special passivation technology, and the actual power generation power of the assembly is greatly improved. But the accompanying anti-aging capability becomes a great problem restricting the development of the anti-aging coating. The characteristic requires that the packaging adhesive film needs stronger ageing resistance, and the traditional EVA can not meet the requirement. The POE adhesive film is used as a packaging adhesive film with high aging resistance, and although the high aging resistance can meet the packaging requirement of the double-sided component, the high price and poor compatibility of the POE adhesive film make the POE adhesive film difficult to perfectly adapt to the packaging of the photovoltaic component. Moreover, the white packaging adhesive film is used as the only synergistic adhesive film used in large batch at present, and the synergistic point of the white packaging adhesive film is contrary to the double-sided technical scheme, so that the white packaging adhesive film cannot be adapted to the double-sided battery technology.
The double-sided technology is used as a breakthrough synergistic technology, the power generation efficiency is greatly improved under the condition that the cost is not increased, and the characteristic is that the double-sided technology becomes the mainstream at the present stage. The photovoltaic packaging adhesive film is an indispensable part, so that how to ensure effective protection of the double-sided battery and improve the power generation efficiency of the assembly becomes an important development direction in the field.
Disclosure of Invention
The invention mainly solves the defects in the prior art, and provides a co-extrusion type synergistic transparent adhesive film which sequentially comprises a special EVA layer, a composite POE synergistic layer and a special EVA layer.
The technical problem of the invention is mainly solved by the following technical scheme:
a co-extruded synergistic transparent adhesive film is composed of three main layers, the outer layer is a special EVA layer, the middle layer is a composite POE synergistic layer, and the composite POE synergistic layer can be divided into a POE bonding filling layer and a super-refraction synergistic layer.
The whole glue film is in a grid shape and can be divided into a synergistic area and a functional area. The synergistic area covers the photovoltaic module cell area, and the functional area covers the photovoltaic module cell gap area. The functional area can play the role of area demarcation and functionalization by changing color. In the composite POE synergistic layer, the bonding filling layer plays a role in bonding, filling and special effect protection; the super-refraction synergistic layer can be in the shape of sphere, hemisphere, cuboid, pyramid and the like according to the requirement, and plays a role in refraction synergistic effect.
Preferably, the specification of the special EVA layer is as follows: the melt index of the selected EVA resin substrate is 10-40 g/10min, and the volume resistivity is more than or equal to 1.0 multiplied by 10 15 ；
The special EVA layer is prepared from the following components in parts by mass: 100 portions of ethylene-vinyl acetate copolymer resin, 0.2 to 1.5 portions of assistant crosslinking agent, 0.05 to 1 portion of light stabilizer, 0.2 to 2 portions of initiator and 0.1 to 2 portions of silane coupling agent; wherein the proportion of the EVA reinforced master batch is 5-20%.
Preferably, the composite POE synergistic layer consists of a bonding filling layer and a super-refraction synergistic layer;
the specification of the bonding filling layer is that the melt index of the base material polyolefin elastomer is 3-20 g/min, and the volume resistivity is more than 1.0 multiplied by 10 16 The light transmittance is more than 90 percent;
the bonding filling layer group is prepared from the following components in parts by mass: 100 portions of polyolefin elastomer, 0.5 to 1.5 portions of assistant crosslinking agent, 0.05 to 1 portion of light stabilizer, 0.5 to 2 portions of initiator and 0.1 to 2 portions of silane coupling agent; wherein, the proportion of the POE reinforced master batch is 5 to 20 percent;
the specification of the super-refraction synergistic layer is as follows: the light transmittance is more than 90 percent, and the refractive index is more than 2.0;
the super-refraction synergistic layer is prepared from the following components in parts by mass: 100 portions of matrix material, 0.2 to 0.8 portion of initiator, 0.6 to 1.5 portions of auxiliary crosslinking agent, 0.01 to 0.5 portion of light stabilizer, 0.1 to 5 portions of silane coupling agent and 0.1 to 10 portions of refraction reinforcing agent.
Preferably, the EVA reinforced master batch is prepared from the following components in parts by mass: 100 parts of ethylene-vinyl acetate copolymer resin, 0.1-5 parts of silane coupling agent, 0-0.5 part of peroxide initiator, 0.5-10 parts of material toughening agent and 0-5 parts of material reinforcing agent;
the EVA reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 110-180 ℃, melting, extruding, cutting into granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400-600 r/min.
Preferably, the POE reinforced master batch is prepared from the following components in parts by mass: 100 parts of polyolefin elastomer, 0.1-2 parts of silane coupling agent, 0-0.5 part of peroxide initiator and 0.5-10 parts of material toughening agent;
the POE reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 180-220 ℃, melting, extruding, cutting into granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 300-500 r/min.
Preferably, the silane coupling agent is one or more of vinyltrichlorosilane, n-butylaminopropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) hexyltrimethoxysilane, 1,3, 5-heptamethyltrisiloxane, dicyclopentyldimethylchlorosilane, bistriethoxypropylamine, triisopropenylmethacrylate, vinyltrimethoxysilane, ethyl orthosilicate Si-40, 3-methacryloxypropyltris (trimethylsiloxyalkyl) silane;
the initiator is one or more of tert-amyl peroxy-2-ethylhexyl ester, tert-butyl peroxyisopropyl carbonate, tert-butyl peroxycarbonate-2-ethylhexyl ester, 1-bis (tert-butylperoxy) cyclohexane, 2-bis (tert-butylperoxy) butane, tert-butyl peroxy-3, 5-trimethylhexanoate, 1' -bis (tert-butylperoxy) -3, 5-trimethylcyclohexane benzene and ethyl 3, 3-di (tert-butylperoxy) butyrate;
the auxiliary crosslinking agent is one or a combination of more of triallyl isocyanurate, triallyl cyanurate, triisopropyl isocyanurate, ethylene glycol dimethacrylate, 1,3, 5-tri-2-propenyl-1, 3, 5-triazine-2, 4,6 (1H, 3H, 5H) -trione, trimethylolpropane trimethacrylate, diethylene glycol dimethacrylate and triallyl isocyanate;
the light stabilizer is 3, 5-di-tert-butyl-4-hydroxy-benzoic acid hexadecyl ester, N, bis (2, 6-tetramethyl-4-piperidyl) -1, 6-hexanediamine, bis-2, 6-tetramethylpiperidinol sebacate, and mixtures thereof one or more of dihydroxy-tetra-N-octyl hydroxy benzophenone and bis (2, 6-tetramethyl piperidyl) sebacate;
the toughening agent is one or more of propoxylated glycerol triacrylate, trimethylolpropane trimethacrylate, ditrimethylolpropane tetraacrylate, dipentaerythritol hexaacrylate, aliphatic urethane acrylate, polyether polyol-aliphatic polyurethane acrylate, aromatic urethane acrylate, epoxy acrylate, modified bisphenol A epoxy acrylate, epoxy methacrylate and fatty acid modified polyester hexaacrylate;
the reinforcing agent is one or more of nano hydrotalcite, nano calcium chloride and nano zinc oxide; the average grain diameter of the reinforcing agent is less than 10nm.
Preferably, the base material of the super-refraction synergistic layer is one or more of dipropylene glycol dicarbonate, high-permeability high-molecular-weight bisphenol A epoxy resin, high-permeability high-molecular-weight bisphenol A type epoxy resin, novolac epoxy-episulfide resin and bisphenol F type epoxy resin;
the refraction enhancer is nano-polymeric carbon nitride.
Preferably, the thickness of the special EVA layer is 0.05-0.5 mm; the thickness of the composite POE synergistic layer is 0.2-5 mm.
A preparation method of a co-extrusion synergistic transparent adhesive film is characterized in that a composite POE synergistic layer is compounded in a die head internal compounding mode; the special EVA layer is distributed to two sides in the die head through a distributor, and then is subjected to co-extrusion compounding with the POE synergistic layer in a compounding mode in the die head.
The curtain coating equipment that chooses for use is the reinforced curtain coating equipment of three-phase, and the membrane head that chooses for use is compound membrane head in the three-layer mould, and compound membrane head intermediate level contains inside discharge gate and coating mouth in the three-layer mould, and accessible PLC controls discharge pressure and time, and control refraction layer shape and thickness form increase district, the functional area of coating simultaneously.
The functional zones may play different roles when coated in different colors: when the functional area is white, the function of reflection enhancement and boundary can be realized; when the functional area is black or other, the function of component color integration, boundary function and the like can be realized.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention solves the problem of compatibility of the material selected by the super-refraction layer and the refraction reinforcing agent with the whole adhesive film system by a multilayer coextrusion casting technology. The problems of fogging, bonding force reduction and the like in the mixing process of the super-refraction layer and the adhesive film system are avoided.
2. According to the invention, a specific formula is adopted to carry out grafting reaction on the selected silane coupling agent, the material toughening agent and the material reinforcing agent, so that the water penetration resistance and the anti-adhesion attenuation capability of the EVA layer and the POE layer are improved. So that a strong interlayer bonding force is maintained between the whole layers of the adhesive film, and the delamination phenomenon between the layers of the adhesive film is prevented. Meanwhile, the material reinforcing agent can effectively improve the PID (potential induced degradation) resistance of the adhesive film and improve the potential-induced attenuation resistance of the assembly.
3. The super-refraction layer adopted by the invention has very high refractive index, and can change the direction of sunlight passing through. The matched grid structure can refract sunlight originally irradiating the cell gap area to the cell area, and the sunlight utilization rate is increased. The more the sunlight deviates from the vertical angle, the higher the sunlight refraction utilization ratio is, and the higher the power generation efficiency is improved. The double-sided battery is more obviously used.
Drawings
FIG. 1 is a schematic cross-sectional view of a co-extruded synergistic transparent adhesive film according to a preferred embodiment of the present invention;
in fig. 1: 1 is a special EVA layer; 2. 3 and 4 are respectively a POE super-refraction layer, a POE filling layer and a functional area coating layer, and the three layers are combined into a composite POE synergistic layer. 5 is a placed cell area, 6 is a schematic diagram of incident light;
as can be seen from the light ray diagram of fig. 1, when sunlight passes through the refraction layer, a part of sunlight which originally directly irradiates the cell gap area will be refracted to change the trajectory, so as to irradiate the cell area. The effective utilization rate of sunlight is increased.
Detailed Description
The technical scheme of the invention is further specifically described by the embodiments and the attached drawings.
Example 1: the co-extruded synergistic transparent adhesive film is produced with special EVA layer, composite POE synergistic layer and special EVA layer successively. The selected super-refractive layer is hemispherical.
The special EVA layer comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 0.6 part of triallyl isocyanurate, 0.1 part of 3, 5-di-tert-butyl-4-hydroxy-benzoic acid hexadecyl ester, 0.8 part of peroxy-2-ethylhexyl tert-amyl ester and 0.6 part of vinyl trichlorosilane. The proportion of the EVA reinforced master batch is 10 percent.
The adhesive filling layer of the composite POE synergistic layer comprises, by mass, 100 parts of a polyolefin elastomer, 0.7 part of triallyl isocyanurate, 0.1 part of 3, 5-di-tert-butyl-4-hydroxy-benzoic acid hexadecyl ester, 0.4 part of peroxy-2-ethylhexyl tert-amyl ester and 0.8 part of a silane coupling agent. The proportion of the POE reinforced master batch is 10 percent.
The super-refraction layer of the composite POE synergistic layer comprises, by mass, 100 parts of high-permeability high-molecular-weight bisphenol A epoxy resin, 0.2 part of peroxide 2-ethylhexyl tert-amyl ester, 0.6 part of triallyl isocyanurate, 0.1 part of 3, 5-di-tert-butyl-4-hydroxy-benzoic hexadecyl ester, 0.6 part of vinyl trichlorosilane and 5 parts of nano polymeric carbon nitride.
The EVA reinforced master batch comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 2 parts of vinyl trichlorosilane, 0.1 part of peroxide 2-ethylhexyl tert-amyl ester, 4 parts of propoxylated glycerol triacrylate and 2 parts of nano hydrotalcite. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 180 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 600r/min.
The POE reinforced master batch comprises, by mass, 100 parts of a polyolefin elastomer, 2 parts of a silane coupling agent vinyl trichlorosilane, 0.1 part of peroxide 2-ethylhexyl tert-amyl ester and 4 parts of propoxylated glycerol triacrylate. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 200 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 500r/min.
The single-layer thickness of the special EVA layer of the co-extrusion synergistic transparent adhesive film is 0.1mm; the thickness of the composite POE synergistic layer is 0.4mm.
Example 2:
a co-extrusion synergistic transparent adhesive film comprises a special EVA layer, a composite POE synergistic layer and a special EVA layer in sequence. The selected super-refractive layer is hemispherical.
The special EVA layer comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 0.7 part of triallyl cyanurate, 0.1 part of N, N, -bis (2, 6-tetramethyl-4-piperidyl) -1, 6-hexanediamine, 0.8 part of isopropyl tert-butyl peroxycarbonate and 0.4 part of N-butylaminopropyltrimethoxysilane. The proportion of the EVA reinforced master batch is 10 percent.
The adhesive filling layer of the composite POE synergistic layer comprises, by mass, 100 parts of polyolefin elastomer, 0.8 part of triallyl cyanurate, 0.1 part of N, N, -bis (2, 6-tetramethyl-4-piperidyl) -1, 6-hexanediamine, 0.5 part of tert-butyl isopropyl peroxycarbonate and 0.6 part of N-butylaminopropyl trimethoxy silane. The proportion of the POE reinforced master batch is 10 percent.
The super-refraction layer of the composite POE synergistic layer comprises, by mass, 100 parts of novolac epoxy-episulfide resin, 0.4 part of tert-butyl peroxyisopropyl carbonate, 0.4 part of triallyl cyanurate, 0.1 part of N, N-bis (2, 6-tetramethyl-4-piperidyl) -1, 6-hexanediamine, 0.6 part of N-butylaminopropyl trimethoxy silane and 5 parts of nano polymeric carbon nitride.
The EVA reinforced master batch comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 4 parts of n-butylaminopropyl trimethoxy silane, 0.2 part of tert-butyl isopropyl peroxycarbonate, 5 parts of trimethylolpropane trimethacrylate and 4 parts of nano calcium chloride. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 180 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 600r/min.
The POE reinforced master batch comprises, by mass, 100 parts of a polyolefin elastomer, 3 parts of n-butylaminopropyl trimethoxy silane, 0.2 part of tert-butyl peroxyisopropyl carbonate and 3 parts of trimethylolpropane trimethacrylate. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 200 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 500r/min.
The single-layer thickness of the special EVA layer of the co-extrusion synergistic transparent adhesive film is 0.1mm; the thickness of the composite POE synergistic layer is 0.5mm.
Example 3:
a co-extrusion synergistic transparent adhesive film comprises a special EVA layer, a composite POE synergistic layer and a special EVA layer in sequence. The selected super-refractive layer is hemispherical.
The special EVA layer comprises 100 parts of ethylene-vinyl acetate copolymer resin, 0.6 part of triisopropylisocyanurate, 0.1 part of bis-2, 6-tetramethylpiperidinol sebacate, 0.6 part of 2, 2-bis (t-butylperoxy) butane and 0.7 part of 1,3, 5-heptamethyltrisiloxane. The proportion of the EVA reinforced master batch is 12 percent.
The adhesive filling layer of the composite POE synergistic layer comprises 100 parts by mass of polyolefin elastomer and 0.8 part by mass of triisopropyl isocyanurate, 0.1 part of bis-2, 6-tetramethylpiperidinol sebacate, 0.6 part of 2, 2-bis (t-butylperoxy) butane and 0.7 part of 1,3, 5-heptamethyltrisiloxane. The proportion of the POE reinforced master batch is 12 percent.
The super-refraction layer is a composite POE synergistic layer, and comprises 100 parts of bisphenol F type episulfide-epoxy resin and 0.5 part of 2, 2-bis (tert-butylperoxy) butane by mass, 0.7 part of triisopropylisocyanurate, 0.1 part of bis-2, 6-tetramethylpiperidinol sebacate, 0.7 part of 1,3, 5-heptamethyltrisiloxane and 5 parts of nano-polymeric carbon nitride.
The EVA reinforced master batch comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 5 parts of 1,3, 5-heptamethyltrisiloxane, 0.1 part of 2, 2-bis (tert-butylperoxy) butane, 5 parts of modified bisphenol A epoxy acrylate and 3 parts of nano calcium chloride. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 150 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 500r/min.
The POE reinforced master batch comprises 100 parts of polyolefin elastomer, 2 parts of 1,3, 5-heptamethyltrisiloxane, 0.1 part of 2, 2-bis (tert-butylperoxy) butane and 3 parts of modified bisphenol A epoxy acrylate by mass fraction. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 200 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400r/min.
The single-layer thickness of the special EVA layer of the co-extrusion synergistic transparent adhesive film is 0.1mm; the thickness of the composite POE synergistic layer is 0.5mm.
Example 4:
a co-extrusion synergistic transparent adhesive film comprises a special EVA layer, a composite POE synergistic layer and a special EVA layer in sequence. The selected super-refractive layer is in a cuboid shape.
The special EVA layer comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 0.6 part of 1,3, 5-tri-2-propenyl-1, 3, 5-triazine-2, 4,6 (1H, 3H, 5H) -trione, 0.1 part of dihydroxy-tetra-n-octyl hydroxy benzophenone, 0.5 part of 1,1' -bis (tert-butylperoxy) -3, 5-trimethylcyclohexane benzene and 0.7 part of vinyl trimethoxy silane. The proportion of the EVA reinforced master batch is 12 percent.
The adhesive filling layer is composed of 100 parts by mass of a polyolefin elastomer, 0.8 part by mass of 1,3, 5-tri-2-propenyl-1, 3, 5-triazine-2, 4,6 (1H, 3H, 5H) -trione, 0.1 part by mass of dihydroxy-tetra-n-octyl hydroxybenzophenone, 0.5 part by mass of 1,1' -bis (t-butylperoxy) -3, 5-trimethylcyclohexane benzene, 0.6 part by mass of vinyltrimethoxysilane and 12 parts by mass of POE reinforced master batch.
The super-refraction layer of the composite POE synergistic layer comprises, by mass, 50 parts of diethylene glycol dipropylene dicarbonate, 50 parts of bisphenol F type sulfur-epoxy resin, 0.4 part of 1,1' -bis (tert-butylperoxy) -3, 5-trimethylcyclohexane benzene, 0.5 part of 1,3, 5-tri-2-propenyl-1, 3, 5-triazine-2, 4,6 (1H, 3H, 5H) -trione, 0.1 part of dihydroxy-tetra-n-octyl hydroxy benzophenone, 0.6 part of vinyl trimethoxy silane and 3 parts of nano-polymerized carbon nitride.
The EVA reinforced master batch comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 4 parts of vinyl trimethoxy silane, 0.2 part of 1,1' -bis (tert-butylperoxy) -3, 5-trimethylcyclohexane benzene, 6 parts of polyether polyol-aliphatic polyurethane acrylate, and 2 parts of a mixture of nano hydrotalcite and nano calcium chloride in equal amount. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 180 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 600r/min.
The POE reinforced master batch comprises, by mass, 100 parts of polyolefin elastomer, 2 parts of vinyl trimethoxy silane, 0.2 part of 1,1' -bis (tert-butylperoxy) -3, 5-trimethylcyclohexane benzene and 3 parts of polyether polyol-aliphatic polyurethane acrylate. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 200 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400r/min.
The single-layer thickness of the special EVA layer of the co-extrusion synergistic transparent adhesive film is 0.1mm; the thickness of the composite POE synergistic layer is 0.4mm.
Example 5:
the co-extruded synergistic transparent adhesive film is produced with special EVA layer, composite POE synergistic layer and special EVA layer successively. The selected super-refractive layer is in a cuboid shape.
The special EVA layer comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 0.6 part of triallyl isocyanate, 0.2 part of bis (2, 6-tetramethylpiperidyl) sebacate, 0.5 part of ethyl 3, 3-di (tert-butylperoxy) butyrate and 400.7 parts of ethyl orthosilicate Si. The proportion of the EVA reinforced master batch is 12 percent.
The adhesive filling layer of the composite POE synergistic layer comprises, by mass, 100 parts of a polyolefin elastomer, 0.5 part of triallyl isocyanate, 0.2 part of bis (2, 6-tetramethylpiperidyl) sebacate, 0.7 part of ethyl 3, 3-di (tert-butylperoxy) butyrate, si-400.6 parts of ethyl orthosilicate and 12% of POE reinforced master batch.
The super-refraction layer of the composite POE synergistic layer comprises, by mass, 100 parts of bisphenol F type ring sulfur-epoxy resin, 0.5 part of ethyl 3, 3-di (tert-butylperoxy) butyrate, 0.5 part of triallyl isocyanate, 0.2 part of bis (2, 6-tetramethylpiperidyl) sebacate, 400.5 parts of ethyl orthosilicate Si and 6 parts of nano-polymeric carbon nitride.
The EVA reinforced master batch comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 405 parts of ethyl orthosilicate Si-405, 0.1 part of ethyl 3, 3-di (tert-butylperoxy) butyrate, 6 parts of epoxy methacrylate and 4 parts of nano hydrotalcite. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 180 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 500r/min.
The POE reinforced master batch comprises, by mass, 100 parts of a polyolefin elastomer, si-402 parts of ethyl orthosilicate, 0.1 part of ethyl 3, 3-di (tert-butylperoxy) butyrate and 3 parts of epoxy methacrylate. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating to 220 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400r/min.
The single-layer thickness of the special EVA layer of the root co-extrusion synergistic transparent adhesive film is 0.2mm; the thickness of the composite POE synergistic layer is 0.6mm.
Example 6:
a co-extrusion synergistic transparent adhesive film comprises a special EVA layer, a composite POE synergistic layer and a special EVA layer in sequence. The selected super-refractive layer is in a cuboid shape.
The special EVA layer comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 0.5 part of triisopropylisocyanurate, 0.1 part of 3, 5-di-tert-butyl-4-hydroxy-benzoic acid hexadecyl ester, 0.5 part of tert-butyl peroxy 3, 5-trimethylhexanoate and 0.5 part of triisopropylene methacrylate. The proportion of the POE reinforced master batch is 15 percent.
The adhesive filling layer of the composite POE synergistic layer comprises, by mass, 100 parts of a polyolefin elastomer, 0.7 part of triisopropylisocyanurate, 0.1 part of 3, 5-di-tert-butyl-4-hydroxy-benzoic acid hexadecyl ester, 0.6 part of tert-butyl peroxy 3, 5-trimethylhexanoate and 0.5 part of triisopropylene methyl acrylate. The proportion of the POE reinforced master batch is 15 percent.
The super-refraction layer of the composite POE synergistic layer comprises, by mass, 100 parts of high-permeability high-molecular-weight bisphenol A epoxy resin, 0.5 part of tert-butyl peroxy 3, 5-trimethylhexanoate, 0.5 part of triisopropyl isocyanurate, 0.1 part of 3, 5-di-tert-butyl-4-hydroxy-hexadecylbenzoate, 0.6 part of triisopropylene methyl acrylate silicone grease and 5 parts of nano polymeric carbon nitride.
The EVA reinforced master batch comprises, by mass, 100 parts of ethylene-vinyl acetate copolymer resin, 4 parts of triisopropylene methyl acrylate silicone grease, 0.1 part of tert-butyl peroxy 3,5 trimethyl hexanoate, 5 parts of dipentaerythritol hexaacrylate and 2 parts of nano calcium chloride. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 140 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400r/min.
The POE reinforced master batch comprises 100 parts of polyolefin elastomer, 3 parts of triisopropylene silicon methacrylate, 0.1 part of tert-butyl peroxy 3,5 trimethyl hexanoate and 2 parts of dipentaerythritol hexaacrylate by mass fraction. The reinforced master batch is prepared by the following method: the preparation method comprises the steps of uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 180 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400r/min.
The single-layer thickness of the special EVA layer of the co-extrusion synergistic transparent adhesive film is 0.1mm; the thickness of the composite POE synergistic layer is 0.5mm.
Comparative example 1:
a photovoltaic module packaging adhesive film is the same as embodiment 1 except that a filling layer is used for replacing a refraction layer, and the description is omitted here.
Comparative example 2:
the packaging adhesive film of the comparative example is the first EPE type multilayer co-extrusion packaging adhesive film sold on the market.
Comparative example 3:
the packaging adhesive film of the comparative example is a common high-transmittance EVA packaging adhesive film with the first three sales volumes in the market.
Comparative example 4:
the packaging adhesive film of the comparative example is a common high-transmittance POE packaging adhesive film of the first three on the market.
Test example
The adhesive packaging films of examples 1 to 6 and comparative examples 1 to 4 were subjected to performance tests, and the test results are shown in table 1. Wherein: the light transmittance test adopts a UV-2600 ultraviolet spectrophotometer to test;
the volume resistivity is tested by adopting a ZC-90E volume resistivity tester;
testing the yellow edge index by adopting ColorQuest XE;
and in the power generation efficiency test, 80 modules are manufactured for each product to form a power station, the power station is respectively connected with inverters, each module uses battery pieces with the same type, and the module is a double-sided 72-piece module. The installation positions are uniformly fixed to be the same shelterless section. The time of electricity generation was recorded as 90 days.
TABLE 1 Performance test Table for packaging adhesive film
Figure BDA0003054355230000141
As can be seen from the comparative data in Table 1, the actual power generation efficiency of the component is improved by improving the actual effective utilization rate of sunlight by using the component prepared by the product provided by the invention, and the improvement efficiency is about 2%. Moreover, the added new agent does not affect the basic performance and the aging performance of the product.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the scope of the present invention claimed in the present invention.

Claims (4)

1. A co-extrusion type synergistic transparent adhesive film is characterized in that: the composite POE synergistic layer can be divided into a POE bonding filling layer and a super-refraction synergistic layer;
the specification of the special EVA layer is as follows: the melt index of the selected EVA resin substrate is 10-40 g/10min, and the volume resistivity is more than or equal to 1.0 multiplied by 10 15 Ω·cm；
The special EVA layer is prepared from the following components in parts by mass: 100 portions of ethylene-vinyl acetate copolymer resin, 0.2 to 1.5 portions of assistant crosslinking agent, 0.05 to 1 portion of light stabilizer, 0.2 to 2 portions of initiator and 0.1 to 2 portions of silane coupling agent; wherein the proportion of the EVA reinforced master batch is 5-20%;
the composite POE synergistic layer consists of a bonding filling layer and a super-refraction synergistic layer;
the specifications of the bonding filling layer are that the melt index of the base material polyolefin elastomer is 3-20 g/min, and the volume resistivity is more than 1.0 multiplied by 10 16 Omega cm, light transmittance is more than 90%;
the bonding filling layer group is prepared from the following components in parts by mass: 100 parts of polyolefin elastomer, 0.5-1.5 parts of auxiliary crosslinking agent, 0.05-1 part of light stabilizer, 0.5-2 parts of initiator and 0.1-2 parts of silane coupling agent; wherein, the proportion of the POE reinforced master batch is 5 to 20 percent;
the specification of the super-refraction synergistic layer is as follows: the light transmittance is more than 90 percent, and the refractive index is more than 2.0;
the super-refraction synergistic layer is prepared from the following components in parts by mass: 100 parts of matrix material, 0.2-0.8 part of initiator, 0.6-1.5 parts of assistant crosslinking agent, 0.01-0.5 part of light stabilizer, 0.1-5 parts of silane coupling agent and 0.1-10 parts of refraction reinforcing agent;
the EVA reinforced master batch is prepared from the following components in parts by mass: 100 parts of ethylene-vinyl acetate copolymer resin, 0.1-5 parts of silane coupling agent, 0-0.5 part of peroxide initiator, 0.5-10 parts of material toughening agent and 0-5 parts of material reinforcing agent;
the EVA reinforced master batch is prepared by the following method: mixing various resins uniformly, putting the mixture into a double-screw extrusion granulator, heating the mixture at 110-180 ℃, melting and extruding the mixture, and cutting the mixture to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 400-600 r/min;
the POE reinforced master batch is prepared from the following components in parts by mass: 100 parts of polyolefin elastomer, 0.1-2 parts of silane coupling agent, 0-0.5 part of peroxide initiator and 0.5-10 parts of material toughening agent;
the POE reinforced master batch is prepared by the following method: uniformly mixing various resins, putting the resins into a double-screw extrusion granulator, heating at 180-220 ℃, melting, extruding, and cutting to form granules, wherein the rotating speed of a screw in the double-screw extrusion granulator is 300-500 r/min;
the base material of the super-refraction synergistic layer is one or more of dipropylene glycol dicarbonate, high-permeability high-molecular-weight bisphenol A type epoxy resin, high-permeability high-molecular-weight bisphenol A type episulfide resin, novolac epoxy-episulfide resin and bisphenol F type episulfide-epoxy resin;
the refraction enhancer is nano-polymeric carbon nitride.
2. The co-extruded synergistic transparent adhesive film as claimed in claim 1, wherein: the silane coupling agent is one or more of vinyltrichlorosilane, n-butylaminopropyltrimethoxysilane, 2- (3, 4-epoxycyclohexyl) hexyltrimethoxysilane, 1,3, 5-heptamethyltrisiloxane, dicyclopentyldimethylchlorosilane, bistriethoxysilylpropylamine, triisopropenylmethacrylate, vinyltrimethoxysilane, tetraethoxysilane Si-40 and 3-methacryloxypropyltri (trimethylsiloxyalkyl) silane;
the initiator is one or more of tert-amyl peroxy-2-ethylhexyl ester, tert-butyl peroxyisopropyl carbonate, tert-butyl peroxy2-ethylhexyl carbonate, 1-bis (tert-butylperoxy) cyclohexane, 2-bis (tert-butylperoxy) butane, tert-butyl peroxy-3, 5-trimethylhexanoate, 1' -bis (tert-butylperoxy) -3, 5-trimethylcyclohexane benzene and ethyl 3, 3-di (tert-butylperoxy) butyrate;
the auxiliary crosslinking agent is one or a combination of more of triallyl isocyanurate, triallyl cyanurate, triisopropyl isocyanurate, ethylene glycol dimethacrylate, 1,3, 5-tri-2-propenyl-1, 3, 5-triazine-2, 4,6 (1H, 3H, 5H) -trione, trimethylolpropane trimethacrylate, diethylene glycol dimethacrylate and triallyl isocyanate;
the light stabilizer is 3, 5-di-tert-butyl-4-hydroxy-benzoic acid hexadecyl ester, N, bis (2, 6-tetramethyl-4-piperidyl) -1, 6-hexanediamine, bis-2, 6-tetramethylpiperidinol sebacate, and mixtures thereof one or more of dihydroxy-tetra-N-octyl hydroxybenzophenone and bis (2, 6-tetramethyl piperidyl) sebacate;
the toughening agent is one or more of propoxylated glycerol triacrylate, trimethylolpropane trimethacrylate, ditrimethylolpropane tetraacrylate, dipentaerythritol hexaacrylate, aliphatic urethane acrylate, polyether polyol-aliphatic polyurethane acrylate, aromatic urethane acrylate, epoxy acrylate, modified bisphenol A epoxy acrylate, epoxy methacrylate and fatty acid modified polyester hexaacrylate;
the reinforcing agent is one or more of nano hydrotalcite, nano calcium chloride and nano zinc oxide; the average grain diameter of the reinforcing agent is less than 10nm.
3. The co-extruded synergistic transparent adhesive film as claimed in claim 1, wherein: the thickness of the special EVA layer is 0.05-0.5 mm; the thickness of the composite POE synergistic layer is 0.2-5 mm.
4. The method for preparing a co-extruded synergistic transparent adhesive film as claimed in claim 1, wherein: the composite POE synergistic layer is compounded in a compounding mode inside the die head; the special EVA layer is distributed to two sides in the die head through a distributor, and then is subjected to co-extrusion compounding with the POE synergistic layer in a compounding mode in the die head.
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