WO2014061669A1 - 硬化シート、それを有する積層体、及びその積層体の製造方法 - Google Patents
硬化シート、それを有する積層体、及びその積層体の製造方法 Download PDFInfo
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- WO2014061669A1 WO2014061669A1 PCT/JP2013/077996 JP2013077996W WO2014061669A1 WO 2014061669 A1 WO2014061669 A1 WO 2014061669A1 JP 2013077996 W JP2013077996 W JP 2013077996W WO 2014061669 A1 WO2014061669 A1 WO 2014061669A1
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- WIPO (PCT)
- Prior art keywords
- laminate
- eva
- ethylene
- sheet
- polyethylene
- Prior art date
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- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229920006163 vinyl copolymer Polymers 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
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- 239000008096 xylene Substances 0.000 description 1
Images
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Definitions
- the present invention has a cured sheet obtained by curing a laminate-forming sheet (such as a solar cell sealing film or a laminated glass interlayer film) for bonding and integrating them in a laminated body such as a solar battery or laminated glass. It relates to a laminate.
- a laminate-forming sheet such as a solar cell sealing film or a laminated glass interlayer film
- a sheet (EVA sheet) made of a composition containing an ethylene-vinyl acetate copolymer (hereinafter also referred to as EVA) as a main component is inexpensive and has high transparency.
- EVA ethylene-vinyl acetate copolymer
- the interlayer film for laminated glass is sandwiched between glass plates 11A and 11B and exhibits functions such as penetration resistance and prevention of scattering of broken glass.
- the solar cell sealing film is formed between the solar cell 24 and the front surface side transparent protective member 21 made of a glass substrate or the like, and the solar cell 24 and the back surface side protective member (back). It is arranged between the cover) 22 and exhibits functions such as ensuring insulation and ensuring mechanical durability.
- Patent Documents 1 and 2 A composition or a sealing sheet has been developed (Patent Documents 1 and 2).
- a laminate such as a sealing film for solar cells and an intermediate film for laminated glass made of a composition obtained by mixing EVA and polyethylene as described in Patent Document 1 or 2 Sheet, especially laminated sheets such as solar cells and laminated glass using a laminate-forming sheet with a high content of polyethylene, adhesion of cured sheets cured by a thermocompression bonding process or the like It has been found that durability and flexibility are lowered, and durability of the laminate may be insufficient.
- an object of the present invention is a cured sheet obtained by curing a sheet for forming a laminate including an ethylene-vinyl acetate copolymer and polyethylene, and has excellent adhesion durability and sufficient flexibility even when the polyethylene content is large. It is in providing the cured sheet which has property, the laminated body which has it, and the manufacturing method of the laminated body.
- the above object is a cured sheet constituting the laminate, and is a cured sheet obtained by crosslinking and curing a laminate-forming sheet composed of an ethylene-vinyl acetate copolymer, polyethylene and an organic peroxide.
- the mass ratio (EVA: PE) of the ethylene-vinyl acetate copolymer (EVA) to the polyethylene (PE) is in the range of 3: 7 to 8: 2, and the ethylene-vinyl acetate copolymer is
- the cured sheet is characterized in that it has a sea-island structure in which the polyethylene is an island phase.
- the laminate-forming sheet in which ethylene-vinyl acetate copolymer (EVA) and polyethylene (PE) are mixed maintains a sea-island structure in which the EVA component is the sea phase (continuous phase) and the PE component is the island phase.
- EVA ethylene-vinyl acetate copolymer
- PE polyethylene
- the cured sheet cured and crosslinked in the state is EVA cured compared to the case where the EVA and PE are cured in a co-continuous structure, or when the PE component is cured in the sea phase and the EVA component is cured in the island phase.
- Adhesive strength and flexibility can be sufficiently exhibited, and a cured sheet having excellent adhesion durability and sufficient hardness can be obtained.
- Preferred embodiments of the cured sheet of the present invention are as follows. (1) The average diameter ((average major axis (l) + average minor axis (d)) / 2) of the island phase made of polyethylene is 40 ⁇ m or less. (2) The average aspect ratio (average major axis (l) / average minor axis (d)) of the island phase made of polyethylene is 40 or less.
- the mass ratio (EVA: PE) of the ethylene-vinyl acetate copolymer (EVA) to the polyethylene (PE) is in the range of 3: 7 to 6: 4.
- the object of the present invention is achieved by a laminate having the cured sheet of the present invention.
- the laminate of the present invention has the cured sheet of the present invention that has improved heat resistance, creep resistance, water vapor permeability resistance, etc. by blending PE with EVA, and has the same adhesion durability as EVA. ing. That is, the laminate of the present invention is bonded and integrated by the cured sheet of the present invention, and is a laminate excellent in weather resistance and durability.
- the laminate of the present invention preferably has a structure in which the cured sheet is sandwiched between at least two substrates.
- a structure is a structure in which the adhesive durability of the cured sheet of the present invention is sufficiently exhibited.
- the laminated body of this invention is a laminated glass or a solar cell.
- an object of the present invention is a process for producing a laminate according to the present invention, comprising a composition comprising an ethylene-vinyl acetate copolymer, polyethylene and an organic peroxide, wherein the ethylene-vinyl acetate copolymer ( EVA) to polyethylene (PE) by mass ratio (EVA: PE) is in the range of 3: 7 to 8: 2, the ethylene-vinyl acetate copolymer is the sea phase, and the polyethylene is the island phase.
- EVA ethylene-vinyl acetate copolymer
- PE polyethylene
- a laminate forming sheet having a certain sea-island structure and another laminate material are laminated to form an uncured laminate, and the uncured laminate is heated to form the laminate
- EVA is formed from a composition containing EVA, PE, and an organic peroxide so that the cured sheet of the present invention is obtained.
- the PE molecules in the laminate-forming sheet are heated at the stage of crosslinking and curing the laminate including the laminate-forming sheet. Diffusion occurs, and PE island phase may be enlarged or PE may become continuous phase. In that case, in the laminate after curing, the cured sheet of the present invention cannot be obtained, and the laminate can be inferior in weather resistance and durability.
- the heating temperature in the crosslinking and curing step is in the above range, and the gel fraction is increased so that the EVA gel fraction 5 minutes after the start of heating is in the above range. It is adjusted.
- the temperature of the PE in the laminate forming sheet rises to a temperature at which it is likely to occur, the fluidity of EVA is moderately reduced, so that the enlargement of the PE island phase can be suppressed.
- a laminate having the cured sheet of the present invention can be produced while maintaining the sea-island structure of the EVA sea phase and the PE island phase.
- the rate of increase in the EVA gel fraction can be adjusted by the type and amount of the organic peroxide.
- Preferred embodiments of the laminate manufacturing method of the present invention are as follows.
- the organic peroxide is tert-butylperoxy-2-ethylhexyl monocarbonate or 2,5-dimethyl-2,5-di (tert-butylperoxy) hexane. These organic peroxides are suitable for setting the gel fraction of EVA in the heating time within the above range within the above heating temperature range.
- the content of the organic peroxide is 0.2 to 4.0 parts by mass with respect to 100 parts by mass of the ethylene-vinyl acetate copolymer.
- the present invention by adding PE to EVA, heat resistance and the like are improved, and the cured product of the intermediate film for laminated glass having excellent adhesion durability and sufficient flexibility, and the sealing film for solar cell A cured sheet such as a cured product is obtained. Therefore, it can be said that laminated bodies, such as a laminated glass and a solar cell, having the cured sheet of the present invention are extremely excellent in weather resistance and durability.
- FIG. 1 is a schematic cross-sectional view for explaining the sea-island structure of the cured sheet of the present invention.
- FIG. 1 (a) shows a state where EVA and PE are co-continuous structures
- FIG. 1 (b) shows EVA. Is the sea phase (continuous phase)
- PE is an island-island state
- FIG. 1 (c) is a sea-island structure in which the PE component is the sea phase and the EVA component is the island phase. Indicates.
- a cured sheet obtained by crosslinking and curing a laminate-forming sheet composed of a resin composition containing EVA and PE with a crosslinking agent such as an organic peroxide the EVA component and the PE component as shown in FIG. A state having a continuous structure, a state where the EVA component as shown in FIG. 1B is a sea phase, a state where the PE component is an island phase, and a PE component as shown in FIG. It is a sea phase, and the EVA component may be cured in a state having a sea-island structure that is an island phase.
- these are the composition ratio of EVA and PE in the resin composition when producing the laminate-forming sheet, the mixed state thereof, the type and amount of organic peroxide, and the crosslinking curing temperature condition, etc. May vary.
- the mass ratio of EVA to PE (EVA: PE) is in the range of 3: 7 to 8: 2, and EVA and PE have an EVA component as shown in FIG. It is characterized in that it is cured in a sea-island structure in which the PE component is an island phase.
- the states shown in FIGS. 1 (a) to 1 (c) can be formed according to the production conditions and the cross-linking curing conditions of the laminate-forming sheet.
- the cured sheet that has been crosslinked and cured in the state of the present invention (FIG. 1B) is a cured sheet in which EVA and PE in FIG.
- the adhesive strength and flexibility due to the crosslinking and curing of EVA are sufficiently exhibited, so it has excellent adhesion durability and sufficient It can be set as the cured sheet which has a softness
- the form (shape, size, etc.) of the island phase made of PE constituting the sea-island structure there is no particular limitation on the form (shape, size, etc.) of the island phase made of PE constituting the sea-island structure.
- the shape of the island phase include a cross-sectional shape such as a circle, an ellipse, a polygon such as a rectangle, a rounded polygon such as a rounded rectangle, or a combination of these.
- the size of the island phase for example, in FIG.
- the cross-sectional shape is shown as a circle or an ellipse, but the average value of the average major axis (l) and the average minor axis (d) of the island phase is In the case of the average diameter, it is preferable that the average diameter ((average major axis (l) + average minor axis (d)) / 2) of the island phase made of PE is 40 ⁇ m or less. As a result, it is possible to further exert an adhesive force or the like due to the crosslinking and curing of EVA. Moreover, by making the island phase dense, a cured product having a higher blending ratio of PE can be obtained.
- the average diameter of the island phase is more preferably 30 ⁇ m or less, and particularly preferably 20 ⁇ m or less. Further, the lower limit is preferably 1 ⁇ m or more, more preferably 3 ⁇ m or more. If the size of the island phase is too large, properties close to a co-continuous structure may occur, which may reduce the adhesion durability of the cured product, and if it is too small, the viscosity of the sheet before curing may increase and workability may decrease. There is.
- the average diameter of the island phase is the average major axis (l) where the longest maximum distance in the longitudinal direction is the major axis and the maximum distance in the width direction is the minor axis when the island phase has a polygonal shape or a rounded polygon. And the average minor axis (d) is calculated.
- the average aspect ratio (average major axis (l) / average minor axis (d)) of the island phase made of PE is preferably 40 or less. Thereby, it can be set as the hardened
- the average aspect ratio of the island phase is more preferably 1 to 20, further preferably 1 to 10, and particularly preferably 1 to 5.
- the mass ratio of EVA to PE is from 3: 7 to 8: 2, but the heat resistance, creep resistance, and water vapor transmission resistance are improved by blending PE. It is preferable that the blending ratio of PE is high because the effects such as the above can be sufficiently obtained and the effects such as excellent adhesion durability due to the sea-island structure can be obtained. Therefore, EVA: PE is preferably 3: 7 to 4: 6, particularly preferably 3: 7 to 5: 5.
- the cured sheet of the present invention may be used for any purpose as long as it is a cured sheet that is used for forming a laminate and is integrally bonded to the laminate. What is used especially the outdoors which requires a weather resistance and durability is preferable, and it is preferable that it is a hardened
- the cured sheet of the present invention is a cured product that constitutes a laminate and is cured as a part of the laminate. Therefore, this invention exists also in the laminated body which has the cured sheet of this invention.
- the laminate according to the present invention may have any structure as long as it has the cured sheet according to the present invention, and the laminate materials such as various substrates and coating layers are appropriately combined and bonded and integrated. It is a laminate. Since the adhesive durability of the cured sheet of the present invention is sufficiently exhibited, it is preferable that the cured sheet of the present invention has a structure sandwiched between at least two substrates. Details of these applications will be described later.
- the laminate-forming sheet may occur, and the PE island phase may enlarge or PE may become continuous phase.
- the laminate after curing the cured sheet of the present invention cannot be obtained, and the laminate can be inferior in weather resistance and durability.
- the method for producing a laminate of the present invention comprises a composition comprising an ethylene-vinyl acetate copolymer, polyethylene and an organic peroxide, and the polyethylene (PE) of the ethylene-vinyl acetate copolymer (EVA).
- the mass ratio (EVA: PE) to the range of 3: 7 to 8: 2 preferably in the range of 3: 7 to 4: 6, more preferably in the range of 3: 7 to 5: 5).
- the heating temperature in the cross-linking curing process of the uncured laminate By setting the heating temperature in the cross-linking curing process of the uncured laminate to 130 to 175 ° C., productivity can be improved by shortening the cross-linking process time, and EVA gel 5 minutes after the start of heating
- the rate of increase of the EVA gel fraction so that the fraction is 15 to 70%, the temperature of the laminate-forming sheet is such that the molecular diffusion of PE in the sheet easily occurs (from 100 ° C.
- the temperature rises to 120 ° C. the fluidity of EVA can be reduced moderately.
- EVA electroactive polymer
- the gel fraction 5 minutes after the start of heating is preferably 25 to 60%.
- the EVA gel fraction after crosslinking and curing is preferably 80% or more.
- the heat treatment may be performed under pressure.
- the laminate is pressed while being pressurized at a pressure of 1.0 ⁇ 10 3 Pa to 5.0 ⁇ 10 7 Pa.
- the heating time is not particularly limited, but is preferably 10 minutes to 60 minutes. If the heating time is too short, crosslinking may be insufficient, and if the heating time is too long, there is a risk of deterioration of each laminate material.
- the heating temperature in the crosslinking and curing step is preferably 130 to 170 ° C, and more preferably 140 to 160 ° C. If the heating temperature is too low, the molecular diffusion of PE tends to proceed and the PE island phase may be enlarged. If the heating temperature is too high, foaming may occur due to rapid decomposition of the organic peroxide. In some cases, the cross-linking and curing may occur before the laminate material is laminated, resulting in a decrease in adhesion.
- the rate of increase in the gel fraction of EVA can be adjusted according to the type and blending amount of the organic peroxide, as will be described later.
- polyethylene is a polymer mainly composed of ethylene, and is a homopolymer of ethylene, ethylene and an ⁇ -olefin having 5 or less mol% of 3 or more carbon atoms such as butene. -1, copolymer of hexene-1, 4-methylpentene-1, octene-1, etc., ethylene and 1 mol% or less non-olefin monomer having only functional groups such as carbon, oxygen, and hydrogen Copolymers are included (see JISK6922-1: 1997 annex).
- PE is generally classified by its density, high density polyethylene (HDPE (or PE-HD)), low density polyethylene (LDPE (or PE-LD)), linear low density polyethylene (LLDPE (or PE-LLD)). Any PE may be used, but it is composed of one or more polyethylenes selected from low density polyethylene and / or linear low density polyethylene having a relatively low melting point and low crystallinity. It is preferable.
- HDPE high density polyethylene
- LDPE low density polyethylene
- LLDPE linear low density polyethylene
- LLDPE linear low density polyethylene
- LDPE generally has a long chain branch obtained by polymerizing ethylene in the presence of a radical generator such as an organic peroxide under a high pressure of 100 to 350 MPa, and its density is generally 0.910 g / cm 3 or more and less than 0.930 g / cm 3 .
- LLDPE is generally obtained by copolymerizing ethylene and an ⁇ -olefin in the presence of a transition metal catalyst such as a Ziegler type catalyst, a Phillips catalyst, or a metallocene type catalyst, and its density (according to JIS K 7112). Is generally 0.910 to 0.940 g / cm 3 , preferably 0.910 to 0.930 g / cm 3 . These can use a commercially available thing suitably.
- the content of vinyl acetate in the ethylene-vinyl acetate copolymer (EVA) is usually 20 to 45% by mass with respect to the mass of EVA.
- EVA ethylene-vinyl acetate copolymer
- the cured sheet obtained may become hard, so that content of the vinyl acetate unit of EVA is low.
- the cured sheet of the present invention may not have sufficient transparency and flexibility.
- carboxylic acid, alcohol, amine, etc. will generate
- the content of vinyl acetate in EVA is preferably 20 to 40% by mass, more preferably 22 to 35% by mass.
- the EVA melt flow rate (according to JIS-K7210) is preferably 1.0 g / 10 min or more.
- the MFR is more preferably 1.0 to 50.0 g / 10 minutes, and particularly preferably 4.0 to 30.0 g / 10 minutes.
- MFR is measured on condition of 190 degreeC and load 21.18N.
- an ethylene-acrylic acid copolymer in addition to EVA, an ethylene-acrylic acid copolymer, an ethylene-unsaturated carboxylic acid copolymer such as an ethylene-methacrylic acid copolymer, a carboxyl of the ethylene-unsaturated carboxylic acid copolymer, Ionomer partially or completely neutralized with the above metal, ethylene-methyl acrylate copolymer, ethylene-ethyl acrylate copolymer, ethylene-methyl methacrylate copolymer, ethylene-isobutyl acrylate copolymer Polymers, ethylene-unsaturated carboxylic acid ester copolymers such as ethylene-n-butyl acrylate copolymer, ethylene-isobutyl acrylate-methacrylic acid copolymer, ethylene-n-butyl acrylate-methacrylic acid copolymer Ethylene-unsaturated carboxylic acid ester-unsaturated
- Organic peroxide can form a crosslinked structure of EVA or PE as a crosslinking agent, and can improve the strength, adhesiveness and durability of the cured sheet of the present invention.
- Any organic peroxide may be used as long as it decomposes at a temperature of 100 ° C. or higher to generate radicals.
- those having a decomposition temperature of 70 hours or more with a half-life of 10 hours are preferred.
- organic peroxide examples include tert-butylperoxy-2-ethylhexyl monocarbonate, 2,5-dimethyl-2,5-, from the viewpoint of heating temperature and storage stability in the method for producing a laminate of the present invention.
- organic peroxide tert-butylperoxy-2-ethylhexyl monocarbonate and 2,5-dimethyl-2,5-di (tert-butylperoxy) hexane are particularly preferable. These organic peroxides are suitable for setting the gel fraction of EVA in the heating temperature range and the heating time within a predetermined range in the method for producing a laminate of the present invention, and have higher adhesion durability. A cured sheet can be obtained.
- the content of the organic peroxide is not particularly limited, but is preferably 0.2 to 4.0 parts by mass, more preferably 0.2 to 3.0 parts by mass with respect to 100 parts by mass of the EVA and PE mixture. Part.
- 0.2 to 2.0 parts by mass is preferable with respect to 100 parts by mass of a mixture of EVA and PE, and 2,5-dimethyl-2,5-
- di (tert-butylperoxy) hexane 0.5 to 4.0 parts by mass is preferable with respect to 100 parts by mass of the mixture of EVA and PE.
- the composition of the laminate-forming sheet may contain a crosslinking aid, an adhesion improver, a plasticizer, etc., if necessary, in addition to EVA, PE and organic peroxide.
- Crosslinking aid can improve the gel fraction of EVA and can improve the adhesiveness and durability of the cured sheet of the present invention.
- the content of the crosslinking aid is generally 10 parts by mass or less, preferably 0.1 to 5 parts by mass, more preferably 0.1 to 2.5 parts by mass with respect to 100 parts by mass of the mixture of EVA and PE. used. Thereby, the cured sheet which is further excellent in adhesiveness is obtained.
- crosslinking aid compound having a radical polymerizable group as a functional group
- examples of the crosslinking aid include trifunctional crosslinking aids such as triallyl cyanurate and triallyl isocyanurate, and (meth) acrylic esters (eg, NK ester) ) Monofunctional or bifunctional crosslinking aids.
- trifunctional crosslinking aids such as triallyl cyanurate and triallyl isocyanurate, and (meth) acrylic esters (eg, NK ester) ) Monofunctional or bifunctional crosslinking aids.
- triallyl cyanurate and triallyl isocyanurate are preferable, and triallyl isocyanurate is particularly preferable.
- adhesion improver As the adhesion improver, a silane coupling agent can be used. Thereby, the adhesive force of the cured sheet of the present invention can be further improved.
- the silane coupling agent include ⁇ -chloropropyltrimethoxysilane, vinyltriethoxysilane, vinyltris ( ⁇ -methoxyethoxy) silane, ⁇ -methacryloxypropyltrimethoxysilane, vinyltriacetoxysilane, and ⁇ -glycidoxypropyl.
- the content of the silane coupling agent is preferably 0.1 to 0.7 parts by mass, particularly 0.3 to 0.65 parts by mass with respect to 100 parts by mass of the mixture of EVA and PE.
- plasticizers include phosphites such as trisisodecyl phosphite and trisnonylphenyl phosphite, and phosphorus-containing compounds such as phosphate esters, adipic acid ether esters, trimellitate n-octyl, dioctyl phthalate, dihexyl adipate, sebacic acid Esters of polybasic acids such as dibutyl, 2,2,4-trimethyl-1,3-pentanediol disobutyrate, triethylene glycol-di-2-ethylbutyrate, tetraethylene glycol diheptanoate, triethylene glycol Polyesters such as dipelargonate, epoxidized fatty acid alkyl esters and the like can be used.
- phosphites such as trisisodecyl phosphite and trisnonylphenyl phosphite
- phosphorus-containing compounds such
- various physical properties such as mechanical properties, optical properties such as adhesion, transparency, heat resistance, light resistance, crosslinking speed, etc.
- various additives such as an acryloxy group-containing compound, a methacryloxy group-containing compound, an epoxy group-containing compound, an ultraviolet absorber, a light stabilizer, and / or an anti-aging agent may be added as necessary for adjustment. .
- the same sea island is usually used for the laminate-forming sheet (uncured). It is manufactured to have a structure.
- the production method of the laminate-forming sheet is not particularly limited, but particularly when the blending ratio of PE is high, the above-mentioned sea-island structure is difficult to form, so the conditions for the kneading step of the composition of the laminate-forming sheet are the same. It is preferable to control.
- EVA and PE when kneading EVA and PE, it is obtained by kneading under conditions where the PE viscosity V PE [Pa ⁇ s] is 0.1 to 20 times the EVA viscosity V EVA [Pa ⁇ s]. It is preferred that When EVA and PE are kneaded under these conditions, a composition having a sea-island structure with a higher blending ratio of PE can be obtained.
- the viscosity V PE [Pa ⁇ s] of PE with respect to the viscosity V EVA [Pa ⁇ s] of EVA is further larger than 1 time under the above kneading conditions. It is preferably 20 times or less, more preferably 2 to 15 times, and particularly preferably 4 to 13 times.
- the EVA component flows better than the PE component, so that even with a small amount of EVA blended, the EVA component flows easily, and only EVA makes it easy to form a continuous phase. Thereby, it can be set as the composition which has a sea island structure where the compounding ratio of PE is still higher.
- the EVA viscosity V EVA is preferably 1000 to 50000 Pa ⁇ s, more preferably 2000 to 20000 Pa ⁇ s.
- the viscosity V PE of PE is preferably 20000 to 120,000 Pa ⁇ s, more preferably 30000 to 50000 Pa ⁇ s.
- the viscosity of these resins can be measured using, for example, a capillary rheometer, a shear rate of 6.1 s ⁇ 1 , and a temperature at an actual processing temperature. The viscosity ratio can be calculated from this viscosity.
- the shear rate when kneading EVA and PE is preferably 10 to 1500 s ⁇ 1 .
- the island phase of PE can be formed more densely, and it can be set as the composition which has a sea island structure with the further high compounding ratio of PE.
- the shear rate is more preferably 100 ⁇ 1000 s -1, particularly preferably 200 ⁇ 800s -1.
- the average diameter of PE island phases ((average major axis (l) + average minor axis)
- the diameter (d)) / 2) is preferably 40 ⁇ m or less, more preferably 5 to 30 ⁇ m, and particularly preferably 10 to 20 ⁇ m
- the average aspect ratio of the PE island phase (average major axis (l) / average minor axis (d)) Is preferably 40 or less, more preferably 1 to 30, and particularly preferably 1 to 10.
- the kneading process may be performed with any apparatus.
- EVA, PE and organic peroxide and if necessary, the above materials are put into a super mixer (high-speed fluid mixer), a twin-screw kneader, a planetary gear kneader, a single-screw extruder, etc. Kneading is preferably performed under the above conditions.
- the laminate-forming sheet can be obtained by forming the laminate-forming sheet composition obtained in the above-described kneading step into a sheet.
- the above composition is produced by a method of obtaining a sheet-like material by performing secondary kneading such as roll kneading as necessary, and then molding by ordinary extrusion molding or calendar molding (calendering). Can do.
- the heating temperature during film formation is preferably set to a temperature at which the organic peroxide does not react or hardly reacts.
- the temperature is preferably 50 to 120 ° C, particularly 40 to 100 ° C.
- the thickness of the laminate forming sheet is not particularly limited and can be appropriately set depending on the application. Generally, it is in the range of 50 ⁇ m to 2 mm.
- the cured sheet of the present invention may be used for any purpose as long as it is a cured sheet constituting the laminate as described above.
- heat resistance and the like are imparted by including PE, and the adhesive durability is excellent. Therefore, what is used outdoors where weather resistance and durability are required is preferable, and a cured product of an interlayer film for laminated glass or a sealing film for solar cell is particularly preferable.
- the cured product of the interlayer film for laminated glass is usually a cured product sandwiched between two transparent substrates and bonded and integrated with the laminated glass.
- the laminated glass is produced, for example, by sandwiching the intermediate film 12 (the laminate forming sheet (uncured)) between the two transparent substrates 11A and 11B, as shown in FIG. After deaeration of the laminated body, a method of pressing under heating is used. These processes are performed using, for example, a vacuum bag method, a nip roll method, or the like. Thereby, the intermediate film 12 is cured, and the intermediate film 12 and the transparent substrates 11A and 11B can be bonded and integrated. In order to use the cured product of the intermediate film 12 as the cured sheet of the present invention and the laminated glass as the laminated body of the present invention, it is preferable to carry out in accordance with the conditions of the production method of the laminated body described above.
- the laminate is pre-pressed at a temperature of 80 to 120 ° C., heat-treated at 130 to 175 ° C. for 10 to 60 minutes, and the EVA gel content in the laminate-forming sheet 5 minutes after the start of heating. Heat to a rate of 15-70%. Further, the heat treatment may be performed under pressure. At this time, it is preferable that the laminate is pressed while being pressurized at a pressure of 1.0 ⁇ 10 3 Pa to 5.0 ⁇ 10 7 Pa. Cooling after crosslinking is generally performed at room temperature, and in particular, the faster the cooling, the better.
- the transparent substrate may be a glass film such as a silicate glass, an inorganic glass plate, an uncolored transparent glass plate, or a plastic film.
- the plastic film include a polyethylene terephthalate (PET) film, a polyethylene naphthalate (PEN) film, and a polyethylene butyrate film, and a PET film is preferred.
- PET polyethylene terephthalate
- PEN polyethylene naphthalate
- PET film polyethylene butyrate film
- the thickness of the transparent substrate is generally about 0.05 to 20 mm.
- a cured product of the solar cell sealing film usually, a cured product in which the solar cell is sealed and the solar cell is bonded and integrated between the front-side transparent protective member and the back-side protective member. It is.
- the side (light-receiving surface side) where the light of the solar cell is irradiated is referred to as “front surface side”, and the surface opposite to the light-receiving surface of the solar cell is referred to as “back surface side”.
- the solar cell is manufactured by laminating the front surface side transparent protective member 21, the front surface side sealing film 23 ⁇ / b> A, the solar cell 24, the back surface side sealing film 23 ⁇ / b> B, and the back surface side protective member 22.
- a method of crosslinking and curing the sealing films 23A and 23B according to a conventional method such as heat and pressure is used.
- the laminate forming sheet (uncured) is used as the front surface side sealing film 23A and / or the back surface side sealing film 23B.
- the front side sealing film 23A and the back side sealing film 23B are cross-linked so that the front side transparent protective member 21, the back side through the front side sealing film 23A and the back side sealing film 23B.
- the solar cell 24 can be sealed by integrating the side protection member 22 and the solar cell 24.
- the above-described method for manufacturing the laminated body is used. It is preferable to carry out according to this.
- the laminate is heated with a vacuum laminator at a temperature of 135 to 175 ° C., further 140 to 175 ° C., particularly 155 to 175 ° C., a degassing time of 0.1 to 5 minutes, and a press pressure of 0.1 to 1.5 kg / cm 2. Heating and pressing with a pressing time of 10 to 60 minutes, and heating so that the gel fraction of the ethylene-vinyl acetate copolymer in the laminate-forming sheet 5 minutes after the start of heating is 15 to 70% .
- the cured sheet (cured product of the sealing film for solar cell) of the present invention is a sealing film in a solar cell using a single crystal or polycrystalline silicon crystal cell for solar cells as shown in FIG.
- a cured product of a sealing film in a thin film solar cell such as a thin film silicon-based, thin-film amorphous silicon-based solar cell, or a copper indium selenide (CIS) -based solar cell may be used.
- the back side sealing is performed on the thin film solar cell element layer formed by chemical vapor deposition on the surface of the front side transparent protective member such as a glass substrate, a polyimide substrate, or a fluororesin transparent substrate.
- a structure in which a film and a back surface side protective member are laminated and bonded and integrated, a surface side sealing film and a surface side transparent protective member are laminated and bonded on a solar cell element formed on the surface of the back surface side protective member An integrated structure, or a structure in which a surface-side transparent protective member, a surface-side sealing film, a thin-film solar cell element, a back-side sealing film, and a back-side protective member are laminated in this order and bonded and integrated. Can be mentioned.
- the surface-side transparent protective member 21 used in the present invention is usually a glass substrate such as silicate glass.
- the thickness of the glass substrate is generally from 0.1 to 10 mm, and preferably from 0.3 to 5 mm.
- the glass substrate may be chemically or thermally strengthened.
- the back side protective member 22 used in the present invention is preferably a plastic film such as polyethylene terephthalate (PET). Further, a film obtained by laminating a fluorinated polyethylene film, particularly a fluorinated polyethylene film / Al / fluorinated polyethylene film in this order in consideration of heat resistance and wet heat resistance may be used.
- PET polyethylene terephthalate
- Examples 1 to 17, Comparative Examples 1 to 5 (1) Preparation of laminate-formed sheet sample and cured sheet sample EVA, PE and organic peroxide were kneaded in the respective compounding amounts shown in Table 1 (kneading temperature: 120 ° C), EVA was the sea phase, PE An EVA and PE mixed composition having an island-island sea-island structure was prepared. Subsequently, each laminate sample sheet (thickness: 0.5 mm and 2.0 mm) was prepared by calendering (molding temperature; 85 ° C.) of the composition.
- each laminate-formed sheet sample prepared above (100 mm ⁇ 100 mm ⁇ 2.0 mm thickness) is sandwiched between two release PETs (thickness: 0.75 ⁇ m), pre-pressed at 100 ° C., and in an oven And heated at the temperatures shown in Table 1.
- Two samples were prepared under the same conditions. One sample was taken out after 5 minutes of heating and used as a gel fraction measurement sample, and the other sample was heated for the time shown in Table 1 to prepare each cured sheet sample.
- Adhesive durability (adhesive strength after durability test) About the sample similar to the sample for initial adhesive strength evaluation produced above, after performing a durability test (left for 1500 hours on 85 degreeC and 85% RH conditions), adhesive strength was evaluated similarly to the above. Regarding the adhesion durability, the case where the adhesive strength after the durability test was 9.8 N / cm or more was evaluated as “ ⁇ ”, and the case where it was less than 9.8 N / cm was evaluated as “X”.
- the cured sheets of Examples 1 to 17 having a sea-island structure in which EVA is a sea phase and PE is an island phase are cured sheets having an elastic modulus and adhesion durability only (comparison). It was close to Example 5), and it was recognized that it had excellent initial adhesive strength, adhesion durability and flexibility as compared with the cured sheets of Comparative Examples 1 to 4 comprising EVA and PE mixtures having no sea-island structure.
- a laminated glass and a solar cell excellent in weather resistance and durability can be provided.
Abstract
Description
(1)前記ポリエチレンからなる島相の平均径((平均長径(l)+平均短径(d))/2)が、40μm以下である。
(2)前記ポリエチレンからなる島相の平均アスペクト比(平均長径(l)/平均短径(d))が、40以下である。
以下に本発明の硬化シートについて、図面を参照しながら説明する。
本発明の硬化シートは、積層体を構成し、積層体の一部として硬化された硬化物である。従って、本発明は、本発明の硬化シートを有する積層体にもある。
本発明の積層体は、本発明の硬化シートを有するので、本発明の積層体を製造する場合、本発明の硬化シートが得られるような製造方法を行う必要がある。EVA成分が海相であり、PE成分が島相である海島構造を有する本発明の硬化シートを得るため、通常、EVA、PE、有機過酸化物を含む組成物からなる積層体形成用シート(未硬化)においても、同様な海島構造を有するように製造する。しかしながら、EVAが海相であり、PEが島相である海島構造を有する積層体形成用シートを用いた場合であっても、その積層体形成用シートを含む積層体を加熱して架橋硬化する段階で、積層体形成用シート中のPEの分子拡散が生じ、PEの島相が肥大化したり、PEが連続相化したりする場合がある。その場合、硬化後の積層体において、本発明の硬化シートが得られず、耐候性、耐久性に劣る積層体になり得る。
本発明において、ポリエチレン(PE)は、JISに規定される通り、エチレンを主体とする重合体であり、エチレンの単独重合体、エチレンと5モル%以下の炭素数3以上のα-オレフィン例えばブテン-1、ヘキセン-1、4―メチルペンテン-1、オクテン-1等との共重合体、エチレンと官能基に炭素、酸素、および水素だけを有する1モル%以下の非オレフィン単量体との共重合体を含む(JISK6922-1:1997附属書参照)。PEは一般に、その密度によって分類され、高密度ポリエチレン(HDPE(又はPE-HD))、低密度ポリエチレン(LDPE(又はPE-LD))、直鎖状低密度ポリエチレン(LLDPE(又はPE-LLD)等が挙げられる。PEとしてはどのようなものでも良いが、比較的融点が低く、結晶化度が低い低密度ポリエチレン及び/又は直鎖状低密度ポリエチレンから選択される1種以上のポリエチレンからなることが好ましい。
本発明において、エチレン-酢酸ビニル共重合体(EVA)における酢酸ビニルの含有率は、通常、EVAの質量に対して20~45質量%である。EVAの酢酸ビニル単位の含有量が低い程、得られる硬化シートが硬くなる傾向がある。酢酸ビニルの含有量が20質量%未満では、本発明の硬化シートの透明性、柔軟性が充分でない恐れがある。また、45質量%を超えると、カルボン酸、アルコール、アミン等が発生し積層体における他の部材等との界面で発泡が生じ易くなるおそれがある。
有機過酸化物は、架橋剤として、EVAやPEの架橋構造を形成することができ、本発明の硬化シートの強度、接着性及び耐久性を向上することができるものである。
架橋助剤は、EVAのゲル分率を向上させ、本発明の硬化シートの接着性及び耐久性を向上させることができる。
接着向上剤としては、シランカップリング剤を用いることができる。これにより、本発明の硬化シートの接着力を、更に向上させることができる。前記シランカップリング剤としては、γ-クロロプロピルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリス(β-メトキシエトキシ)シラン、γ-メタクリロキシプロピルトリメトキシシラン、ビニルトリアセトキシシラン、γ-グリシドキシプロピルトリメトキシシラン、γ-グリシドキシプロピルトリエトキシシラン、β-(3,4-エポキシシクロヘキシル)エチルトリメトキシシラン、ビニルトリクロロシラン、γ-メルカプトプロピルトリメトキシシラン、γ-アミノプロピルトリエトキシシラン、N-β-(アミノエチル)-γ-アミノプロピルトリメトキシシランを挙げることができる。これらシランカップリング剤は、単独で使用しても、又は2種以上組み合わせて使用しても良い。なかでも、γ-メタクリロキシプロピルトリメトキシシランが特に好ましく挙げられる。
可塑剤としては、トリスイソデシルホスファイト、トリスノニルフェニルホスファイト等のホスファイトやリン酸エステル等のリン含有化合物、アジピン酸エーテルエステル、トリメリテートn-オクチル、フタル酸ジオクチル、アジピン酸ジヘキシル、セバシン酸ジブチル等の多塩基酸のエステル、2,2,4-トリメチル-1,3-ペンタンジオールジソブチレート、トリエチレングリコール-ジ-2-エチルブチレート、テトラエチレングリコールジヘプタノエート、トリエチレングリコールジペラルゴネート等の多価アルコールのエステル、エポキシ化脂肪酸アルキルエステル等が使用できる。
また、本発明において、積層体形成用シートの用途により、上記の材料の他の添加剤を使用しても良い。例えば、合わせガラス用中間膜や太陽電池用封止膜として使用する場合、種々の物性(機械的強度、接着性、透明性等の光学的特性、耐熱性、耐光性、架橋速度等)の改良あるいは調整のため、必要に応じて、アクリロキシ基含有化合物、メタクリロキシ基含有化合物、エポキシ基含有化合物、紫外線吸収剤、光安定剤、及び/又は老化防止剤などの各種添加剤を添加してもよい。
上述のように、EVA成分が海相であり、PE成分が島相である海島構造を有する本発明の硬化シートを得るために、通常、積層体形成用シート(未硬化)についても同様な海島構造を有するように製造する。積層体形成用シートの製造方法は、特に制限はないが、特にPEの配合比が高い場合は、上述の海島構造が形成され難いので、積層体形成用シートの組成物の混練工程の条件を制御することが好ましい。
本発明の硬化シートは、上述のように積層体を構成する硬化シートであれば、どのような用途でも良いが、PEを含むことで耐熱性等が付与され、且つ接着耐久性に優れているので、耐候性、耐久性が要求される屋外で使用されるものが好ましく、特に合わせガラス用中間膜又は太陽電池用封止膜の硬化物であることが好ましい。
(1)積層体形成用シートサンプル及び硬化シートサンプルの調製
EVA、PE及び有機過酸化物を表1に示す各配合量で混練し(混練温度;120℃)、EVAが海相であり、PEが島相の海島構造を有するEVA及びPE混合組成物を調製した。次いで、その組成物をカレンダ成形(成形温度;85℃)により、各積層体形成用シートサンプル(厚さ;0.5mm及び2.0mm)を調製した。
(i)ゲル分率
各ゲル分率測定用サンプルを200メッシュ金網袋に1g秤量し、ソックスレー抽出器を用い、溶剤(キシレン)で145℃、6時間抽出し、残留物を乾燥し秤量した。初期質量と抽出残留物の乾燥質量からEVAのゲル分率(%)((抽出残留物の乾燥質量/初期質量)×100)を算出した。
各硬化シートサンプルについて、ミクロトーム(leica社製)を用いて断面出しを行い、その断面をAFM(原子間力顕微鏡)(東陽テクニカ社製)にて弾性率マッピングし、EVA及びPEの海島構造を観察した。EVAが海相(連続相)となり、PEが島相となっている場合を○とし、PEが連続相化している場合(共連続相の場合を含む)を×とした。
上記硬化シートサンプルの内PEの島相が認められたものについて、二値化画像処理(解像度の観点から、長径が1.2μm以下となる島相はノイズと判断し、除外して算出)を行い、AFM(原子間力顕微鏡)画像の場合は2500μm2、光学顕微鏡画像の場合は4900μm2中に存在する島相の長径及び短径を測定し、その平均値から平均径((平均長径(l)+平均短径(d))/2)、及び平均アスペクト比(平均長径(l)/平均短径(d))を求めた。
2mm厚の各硬化シートサンプルを直径6mmの円形に打ち抜き、貯蔵弾性率評価用サンプルとした。得られたサンプルをARES(TAインスツルメント社製)にて、30℃、10Hz、0.1%歪の条件で測定し、各サンプルの貯蔵弾性率を求めた。貯蔵弾性率が10MPa以下の場合を○、10MPaを超える場合を×とした。
上記で作製した各積層体形成用シートサンプル(100mm×100mm×0.5mm厚)の片面を離型PETフィルム(厚さ;0.75μm)、もう一方の面を板ガラス(厚さ;3.2mm)で挟み、100℃で仮圧着し、オーブン中で表1に示した温度で加熱することにより初期接着力評価用サンプルを作製した。得られたサンプルを、ガラス板と積層体形成用シートとの間の一部を剥離し、引張試験機(インストロン社製)を用いて、180°ピール試験(JIS K 6584:1994準拠、30℃、引っ張り速度;100mm/分)により初期接着力を評価した。初期接着力が20N/cm以上の場合を◎、20N/cm未満、15N/cm以上の場合を○、15N/cm未満の場合を×とした。
上記で作製した初期接着力評価用サンプルと同様なサンプルについて、耐久性試験(85℃、85%RHの条件で1500時間放置)を行った後、上記と同様に接着力を評価した。接着耐久性は、耐久試験後接着力が9.8N/cm以上の場合を○、9.8N/cm未満の場合を×とした。
評価結果を表1に示す。
12 中間膜
21 表面側透明保護部材
22 裏面側保護部材
23A 表面側封止膜
23B 裏面側封止膜
24 太陽電池用セル
Claims (11)
- 積層体を構成する硬化シートであり、
エチレン-酢酸ビニル共重合体、ポリエチレン及び有機過酸化物を含む組成物からなる積層体形成用シートを架橋硬化してなる硬化シートであって、
前記エチレン-酢酸ビニル共重合体(EVA)の前記ポリエチレン(PE)に対する質量比(EVA:PE)が、3:7~8:2の範囲であり、
前記エチレン-酢酸ビニル共重合体が海相であり、前記ポリエチレンが島相である海島構造を有することを特徴とする硬化シート。 - 前記ポリエチレンからなる島相の平均径((平均長径(l)+平均短径(d))/2)が、40μm以下である請求項1に記載の硬化シート。
- 前記ポリエチレンからなる島相の平均アスペクト比(平均長径(l)/平均短径(d))が、40以下である請求項1又は2に記載の硬化シート。
- 前記エチレン-酢酸ビニル共重合体(EVA)の前記ポリエチレン(PE)に対する質量比(EVA:PE)が、3:7~6:4の範囲である請求項1~3のいずれか1項に記載の硬化シート。
- 合わせガラス用中間膜又は太陽電池用封止膜の硬化物である請求項1~4のいずれか1項に記載の硬化シート。
- 請求項1~5のいずれか1項の硬化シートを有する積層体。
- 前記硬化シートが、少なくとも2枚の基板の間に挟持された構造を有する請求項6に記載の積層体。
- 合わせガラス又は太陽電池である請求項6又は7に記載の積層体。
- 請求項6~8のいずれか1項に記載の積層体の製造方法であって、
エチレン-酢酸ビニル共重合体、ポリエチレン及び有機過酸化物を含む組成物からなり、前記エチレン-酢酸ビニル共重合体(EVA)の前記ポリエチレン(PE)に対する質量比(EVA:PE)が、3:7~8:2の範囲であり、前記エチレン-酢酸ビニル共重合体が海相であり、前記ポリエチレンが島相である海島構造を有する積層体形成用シートと、他の積層体用材料とを積層し、未硬化の積層体を形成する工程、及び
前記未硬化の積層体を加熱して、前記積層体形成用シートを架橋硬化する工程を含み、
前記加熱を130~175℃の温度条件で、加熱開始5分後の前記積層体形成用シート中のエチレン-酢酸ビニル共重合体のゲル分率が、15~70%となるように行うことを特徴とする積層体の製造方法。 - 前記有機過酸化物が、t-ブチルパーオキシ-2-エチルヘキシルモノカーボネート又は2,5-ジメチル-2,5-ジ(tert-ブチルパーオキシ)ヘキサンである請求項9に記載の積層体の製造方法。
- 前記有機過酸化物の含有量が、前記エチレン-酢酸ビニル共重合体及び前記ポリエチレンの混合物100質量部に対して、0.2~4.0質量部である請求項9又は10に記載の積層体の製造方法。
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JPWO2016052670A1 (ja) * | 2014-09-30 | 2017-07-13 | 積水化学工業株式会社 | 合わせガラス用中間膜及び合わせガラス |
JP2018154701A (ja) * | 2017-03-16 | 2018-10-04 | 東ソー株式会社 | 樹脂組成物及びこれよりなる積層体 |
US10538063B2 (en) | 2016-05-09 | 2020-01-21 | Kuraray America, Inc. | Multilayer interlayer and glass laminate |
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