WO2015046583A1 - 合わせガラス用中間膜及び合わせガラス - Google Patents
合わせガラス用中間膜及び合わせガラス Download PDFInfo
- Publication number
- WO2015046583A1 WO2015046583A1 PCT/JP2014/076142 JP2014076142W WO2015046583A1 WO 2015046583 A1 WO2015046583 A1 WO 2015046583A1 JP 2014076142 W JP2014076142 W JP 2014076142W WO 2015046583 A1 WO2015046583 A1 WO 2015046583A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- weight
- laminated glass
- polyvinyl acetal
- acetal resin
- interlayer film
- Prior art date
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10018—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising only one glass sheet
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10743—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing acrylate (co)polymers or salts thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/22—Layered products comprising a layer of synthetic resin characterised by the use of special additives using plasticisers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/306—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl acetate or vinyl alcohol (co)polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/03—3 layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2270/00—Resin or rubber layer containing a blend of at least two different polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/10—Properties of the layers or laminate having particular acoustical properties
- B32B2307/102—Insulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/006—Transparent parts other than made from inorganic glass, e.g. polycarbonate glazings
Definitions
- the present invention relates to an interlayer film for laminated glass used for obtaining laminated glass. Moreover, this invention relates to the laminated glass using the said intermediate film for laminated glasses.
- Laminated glass is superior in safety even if it is damaged by an external impact and the amount of glass fragments scattered is small. For this reason, the said laminated glass is widely used for a motor vehicle, a rail vehicle, an aircraft, a ship, a building, etc.
- the laminated glass is manufactured, for example, by sandwiching an interlayer film for laminated glass between a pair of glass plates.
- the coincidence effect means that when a sound wave is incident on the glass plate, the transverse wave propagates on the glass surface due to the rigidity and inertia of the glass plate, and the transverse wave and the incident sound resonate. This is a phenomenon that occurs.
- Patent Document 1 100 parts by weight of a polyvinyl acetal resin having a degree of acetalization of 60 to 85 mol%, and at least one metal salt of an alkali metal salt and an alkaline earth metal salt is 0.001 to 1
- a sound insulation layer comprising 0.0 parts by weight and more than 30 parts by weight of a plasticizer is disclosed. This sound insulation layer can be used as a single layer as an intermediate film or laminated with other layers as a multilayer intermediate film.
- the plasticizer migrates from the layer having a high plasticizer content to the layer having a small plasticizer content, and the plasticizer bleeds on the surface of the interlayer film or the interface between the layers. May be out.
- the elastic modulus of the intermediate film may change, the adhesiveness of the intermediate film may decrease, or the sound insulation of the laminated glass may decrease.
- An object of the present invention is to provide an interlayer film for laminated glass capable of enhancing the sound insulating properties of the laminated glass, and to provide a laminated glass using the interlayer film for laminated glass.
- a polyvinyl acetal resin and a second resin component having a glass transition temperature of ⁇ 15 ° C. or more and 5 ° C. or less, the polyvinyl acetal resin and the second resin component In a total of 100% by weight, the content of the polyvinyl acetal resin is 10% by weight to 50% by weight, the content of the second resin component is 50% by weight to 90% by weight, An interlayer film for laminated glass in which the polyvinyl acetal resin and the second resin component have a sea-island structure is provided.
- the polyvinyl acetal resin and the second resin component as a whole have a sea-island structure in the interlayer film.
- a temperature indicating a maximum value of a loss tangent derived from the polyvinyl acetal resin is 50 ° C. or more
- the temperature showing the maximum value of the loss tangent derived from the second resin component is ⁇ 15 ° C. or more and 5 ° C. or less, and the maximum value of the loss tangent derived from the second resin component is 0.4 or more. is there.
- the interlayer film does not contain a plasticizer, or contains 100% by weight or less of the plasticizer in the interlayer film.
- the intermediate film preferably contains 20% by weight or less, more preferably 10% by weight or less of the plasticizer in 100% by weight of the intermediate film.
- the interlayer film does not contain a plasticizer.
- the interlayer film for laminated glass in a specific aspect of the interlayer film for laminated glass according to the present invention, at least a part of the polyvinyl acetal resin and at least a part of the second resin component are polymerized.
- the second resin component is a (meth) acrylic resin.
- the interlayer film for laminated glass is obtained by polymerizing the monomer having the (meth) acryloyl group in the presence of the polyvinyl acetal resin.
- the first laminated glass member, the second laminated glass member, and the interlayer film for laminated glass described above are provided, and the first laminated glass member and the second laminated glass are provided.
- the interlayer film for laminated glass according to the present invention includes a polyvinyl acetal resin and a second resin component having a glass transition temperature of ⁇ 15 ° C. or more and 5 ° C. or less, and the polyvinyl acetal resin and the second resin component In the total 100% by weight, the content of the polyvinyl acetal resin is 10% by weight or more and 50% by weight or less, and the content of the second resin component is 50% by weight or more and 90% by weight or less, Furthermore, in the said intermediate film, since the said polyvinyl acetal resin and said 2nd resin component have a sea island structure, the sound insulation of the laminated glass using the intermediate film for laminated glasses which concerns on this invention can be improved.
- FIG. 1 is a partially cutaway cross-sectional view showing a laminated glass using an interlayer film for laminated glass according to an embodiment of the present invention.
- FIG. 2 is a partially cutaway cross-sectional view showing a modified example of a laminated glass using an interlayer film for laminated glass according to an embodiment of the present invention.
- the interlayer film for laminated glass according to the present invention includes a polyvinyl acetal resin and a second resin component having a glass transition temperature of ⁇ 15 ° C. or higher and 5 ° C. or lower.
- the interlayer film for laminated glass according to the present invention can be obtained, for example, by forming a polyvinyl acetal resin composition.
- the content of the polyvinyl acetal resin is 10% by weight or more and 50% by weight or less in a total of 100% by weight of the polyvinyl acetal resin and the second resin component.
- the content of the second resin component is 50% by weight or more and 90% by weight or less.
- the polyvinyl acetal resin and the second resin component have a sea-island structure. Since the sound insulation of the laminated glass using the interlayer film for laminated glass according to the present invention can be further enhanced, in the interlayer film for laminated glass according to the present invention, the polyvinyl acetal resin and the second resin component Preferably have a sea-island structure as a whole.
- the polyvinyl acetal resin may be the polyvinyl acetal resin alone, or the polyvinyl acetal resin may be reacted with the second resin component.
- the second resin component may be the second resin component alone or may react with the polyvinyl acetal resin.
- the polyvinyl acetal resin and the second resin component may react at the interface between the sea part and the island part.
- the part derived from the polyvinyl acetal resin is included in the polyvinyl acetal resin, and the part derived from the second resin component is included in the second resin component.
- the polyvinyl acetal resin is a portion derived from the polyvinyl acetal resin in a reaction product of the polyvinyl acetal resin alone and the reaction product of the polyvinyl acetal resin and the second resin component.
- the second resin component is a part derived from the second resin component in the reaction product of the second resin component alone and the polyvinyl acetal resin and the second resin component.
- the sound insulation of the laminated glass can be enhanced.
- the polyvinyl acetal resin and the second resin component have a sea-island structure.
- the content of the polyvinyl acetal resin is 10% by weight or more and 50% by weight in a total of 100% by weight of the polyvinyl acetal resin and the second resin component in the intermediate film.
- the content of the second resin component is limited to 50% by weight or more and 90% by weight or less.
- the content of the second resin component is too high, the content of the polyvinyl acetal resin is too low, the content of the second resin component is too low, or the content of the polyvinyl acetal resin is too high. In such a case, the maximum value of the loss tangent may not show a good value in the dynamic viscoelastic spectrum, and the sound insulation may be lowered.
- the total content of the polyvinyl acetal resin and the second resin component is 100% by weight.
- the content of the polyvinyl acetal resin is preferably 12% by weight or more, more preferably 15% by weight or more, and still more preferably. Is 20% by weight or more, preferably 45% by weight or less, more preferably 40% by weight or less, and still more preferably 35% by weight or less.
- the content of the second resin component is preferably 55% by weight or more, more preferably Is 60% by weight or more, more preferably 65% by weight or more, preferably 88% by weight or less, more preferably 85% by weight or less, and still more preferably 80% by weight or less.
- the islands are substantially spherical and dispersed in the continuous phase (sea), and the average diameter of the individual islands is preferably 0.1 ⁇ m or more, preferably 10 ⁇ m or less. is there.
- the island portion is substantially spherical, the area of the interface between the sea portion and the island portion is further increased, and more vibration energy is absorbed, so that the sound insulation of the intermediate film is further enhanced.
- the sea-island structure constituted by the polyvinyl acetal resin and the second resin component in the intermediate film can be determined by observing the intermediate film. For the observation, an optical microscope, a transmission electron microscope, a scanning electron microscope, a phase contrast microscope, a polarizing microscope, a scanning tunnel microscope, a microscopic Raman, or the like is used.
- a blending method and a two-stage reaction method can be employed.
- the blending method is a method in which the polyvinyl acetal resin and the second resin component are separately prepared, and then both are mixed (blended).
- melt-kneading mixing, solution mixing, or the like can be used.
- the two-stage reaction method is a method of polymerizing a compound constituting the second resin component in the presence of the polyvinyl acetal resin. In the intermediate film obtained through this two-stage reaction method, the island portion of the sea-island structure is smaller than in the blend method.
- the production of the intermediate film is preferably a two-stage reaction method.
- the temperature showing the maximum value of the loss tangent derived from the polyvinyl acetal resin is preferably 50 ° C. or higher, more preferably 60 ° C. or higher, still more preferably. Is 64 ° C. or higher. 100 degreeC or less may be sufficient as the temperature which shows the maximum value of the loss tangent originating in the said polyvinyl acetal resin.
- the polyvinyl acetal resin can be produced, for example, by acetalizing polyvinyl alcohol with an aldehyde.
- the polyvinyl alcohol can be obtained, for example, by saponifying polyvinyl acetate.
- the saponification degree of the polyvinyl alcohol is preferably 70 mol% or more, more preferably 80 mol% or more, still more preferably 85 mol% or more and 100% or less, preferably 99.9 mol% or less, more preferably 99.8. It is less than mol%.
- the average degree of polymerization of the polyvinyl alcohol is preferably 200 or more, more preferably 500 or more, further preferably 800 or more, preferably 5000 or less, more preferably 4500 or less, still more preferably 3500 or less, and particularly preferably 3000 or less. .
- the average degree of polymerization is not less than the above lower limit, the penetration resistance of the laminated glass is further enhanced.
- the average degree of polymerization is not more than the above upper limit, the intermediate film can be easily molded.
- the average degree of polymerization of the polyvinyl alcohol is determined by a method based on JIS K6726 “Testing method for polyvinyl alcohol”.
- the polyvinyl acetal resin is preferably a polyvinyl acetal resin having a saponification degree of 80 mol% or more and an average polymerization degree of 800 or more and 5000 or less. More preferred is a polyvinyl acetal resin having a saponification degree of 85 mol% or more and an average polymerization degree of 1000 or more and 4500 or less.
- the carbon number of the acetal group contained in the polyvinyl acetal resin is not particularly limited.
- the aldehyde used when manufacturing the said polyvinyl acetal resin is not specifically limited.
- the carbon number of the acetal group in the polyvinyl acetal resin is preferably 3 or 4. When the carbon number of the acetal group in the polyvinyl acetal resin is 3 or more, the glass transition temperature of the intermediate film is sufficiently low.
- the aldehyde is not particularly limited. In general, an aldehyde having 1 to 10 carbon atoms is preferably used as the aldehyde.
- Examples of the aldehyde having 1 to 10 carbon atoms include formaldehyde (including paraformaldehyde), acetaldehyde (including paraacetaldehyde), propionaldehyde, n-butyraldehyde, isobutyraldehyde, n-valeraldehyde, and 2-ethylbutyl.
- n-butyraldehyde is more preferable from the viewpoint of further improving the balance between productivity and characteristics of the interlayer film.
- n-butyraldehyde is more preferable.
- the said aldehyde only 1 type may be used and 2 or more types may be used together.
- the hydroxyl group content (hydroxyl content) of the polyvinyl acetal resin is preferably 15 mol% or more, more preferably 18 mol% or more, still more preferably 20 mol% or more, particularly preferably 25 mol% or more, and most preferably 28. It is at least mol%, preferably at most 40 mol%, more preferably at most 35 mol%, further preferably at most 34 mol%, particularly preferably at most 32 mol%.
- the hydroxyl group content is at least the above lower limit, the adhesive strength of the interlayer film is further increased. Further, when the hydroxyl group content is not more than the above upper limit, the flexibility of the interlayer film is increased, and the handling of the interlayer film is facilitated.
- the hydroxyl group content of the polyvinyl acetal resin is a value indicating the mole fraction obtained by dividing the amount of ethylene groups to which the hydroxyl group is bonded by the total amount of ethylene groups in the main chain, as a percentage.
- the amount of ethylene group to which the hydroxyl group is bonded can be determined, for example, by measuring in accordance with JIS K6726 “Testing method for polyvinyl alcohol” or in accordance with ASTM D1396-92.
- the degree of acetylation (acetyl group amount) of the polyvinyl acetal resin is preferably 0.1 mol% or more, more preferably 0.3 mol% or more, still more preferably 0.5 mol% or more, preferably 30 mol% or less. More preferably, it is at most 25 mol%, further preferably at most 20 mol%, particularly preferably at most 15 mol%.
- the acetylation degree is not less than the above lower limit, the compatibility between the polyvinyl acetal resin and the plasticizer is increased.
- the acetylation degree is not more than the above upper limit, the moisture resistance of the interlayer film and the laminated glass is increased.
- the degree of acetylation is obtained by subtracting the amount of ethylene groups to which acetal groups are bonded and the amount of ethylene groups to which hydroxyl groups are bonded from the total amount of ethylene groups of the main chain, It is a value indicating the mole fraction obtained by dividing by the percentage.
- the amount of ethylene group to which the acetal group is bonded can be measured, for example, according to JIS K6728 “Testing method for polyvinyl butyral” or according to ASTM D1396-92.
- the degree of acetalization of the polyvinyl acetal resin is preferably 40 mol% or more, more preferably 60 mol% or more, still more preferably 63 mol% or more, preferably 85 mol%. Below, more preferably 80 mol% or less, still more preferably 75 mol% or less, particularly preferably 70 mol% or less.
- the degree of acetalization is not less than the above lower limit, the compatibility between the polyvinyl acetal resin and the plasticizer increases, and the hydrogen bond between the molecules of the polyvinyl acetal resin does not become too strong, and the flexibility of the interlayer film Is even more expressed.
- the degree of acetalization is less than or equal to the above upper limit, the reaction time required for producing the polyvinyl acetal resin is shortened, and the hydrogen bond between the molecules of the polyvinyl acetal resin is not too weak, and the strength of the interlayer film is reduced. Becomes even higher.
- the above-mentioned degree of acetalization is a value indicating the mole fraction obtained by dividing the amount of ethylene groups to which acetal groups are bonded by the total amount of ethylene groups in the main chain as a percentage.
- the degree of acetalization was determined by measuring the degree of acetylation and the content of hydroxyl groups by a method based on JIS K6728 “Testing methods for polyvinyl butyral” or a method based on ASTM D1396-92. The rate can be calculated and then calculated by subtracting the degree of acetylation and the hydroxyl content from 100 mol%.
- the hydroxyl group content (hydroxyl content), acetalization degree (butyralization degree), and acetylation degree are preferably calculated from results measured by a method in accordance with JIS K6728 “Testing methods for polyvinyl butyral”.
- the polyvinyl acetal resin is a polyvinyl butyral resin
- the hydroxyl group content (hydroxyl content), the degree of acetalization (degree of butyralization) and the degree of acetylation are measured by a method according to JIS K6728 “Testing methods for polyvinyl butyral”. It is preferable to calculate from the obtained results.
- the glass transition temperature of the second resin component is ⁇ 15 ° C. or higher and 5 ° C. or lower. From the viewpoint of further improving the sound insulation, the temperature showing the maximum value of the loss tangent derived from the second resin component in the dynamic viscoelastic spectrum of the interlayer film at a frequency of 1 Hz is preferably ⁇ 15 ° C. or higher.
- the maximum value of the loss tangent derived from the second resin component is preferably 0.35 or more, more preferably 0.4 or more, and further preferably 0.5 or more.
- the maximum value of the loss tangent derived from the second resin component is particularly preferably 1 or more.
- the second resin component is not particularly limited.
- (meth) acrylic such as silicone rubber, polyisoprene, polybutadiene, polyisobutylene, polyethylene, polypropylene, polyvinylidene chloride, polyvinylidene fluoride, and poly (meth) acrylic acid ester.
- examples thereof include resins, polyacetals, polyurethanes, polyoxymethylenes, and polyoxyethylenes.
- a (meth) acrylic resin is preferable, and the (meth) acrylic resin is preferably a poly (meth) acrylic acid ester.
- a polybutadiene elastomer or a styrene butadiene copolymer may be used as the second resin component.
- the glass transition temperature can be more easily controlled, and the temperature at which the loss tangent maximum value derived from the second resin component is controlled to a suitable range.
- the transparency of the intermediate film can be further improved, and the sound insulation in a wide temperature range can be further enhanced.
- Examples of the method for adjusting the refractive index of the second resin component include a method of copolymerizing monomers having different refractive indexes, and a monomer having a refractive index different from that of the monomer constituting the main chain component. A method is mentioned.
- the poly (meth) acrylic acid ester is not particularly limited.
- the temperature at which the maximum value of loss tangent is -15 ° C. or higher and 5 ° C. or lower in the dynamic viscoelastic spectrum at a frequency of 1 Hz when measured alone using poly (meth) acrylate is preferable. .
- poly (meth) acrylic acid ester examples include poly (meth) acrylate methyl, poly (meth) ethyl acrylate, poly (meth) acrylate n-propyl, poly (meth) acrylate i-propyl, poly N-butyl (meth) acrylate, i-butyl poly (meth) acrylate, t-butyl poly (meth) acrylate, 2-ethylhexyl poly (meth) acrylate, octyl poly (meth) acrylate, poly (meta ) Propyl acrylate, poly (meth) acrylate 2-ethyloctyl, poly (meth) acrylate nonyl, poly (meth) acrylate isononyl, poly (meth) acrylate decyl, poly (meth) acrylate isodecyl, poly ( Lauryl (meth) acrylate, isotetradecyl poly (meth) acryl
- polyacrylic acid esters are preferred because the temperature at which the loss tangent maximum value can be easily controlled within the above range in the dynamic viscoelastic spectrum, and polyethyl acrylate, poly (ethyl acrylate), and poly (n-butyl acrylate) are preferred. More preferred is 2-ethylhexyl polyacrylate or octyl polyacrylate.
- poly (meth) acrylic acid ester only 1 type may be used and 2 or more types may be used together.
- a compound having a (meth) acryloyl group may be used as a component constituting the second resin component.
- the second resin component may be obtained by polymerizing a compound having a (meth) acryloyl group.
- the second resin component may have a crosslinked structure.
- the elastic modulus can be controlled, and an intermediate film having both excellent flexibility and high strength can be produced.
- the method for crosslinking the second resin component functional groups that react with each other are introduced into the polymer structure of the resin to form a crosslink, and the functional group present in the polymer structure of the resin reacts. Examples include a method of crosslinking using a crosslinking agent having two or more functional groups, a method of crosslinking a polymer using a radical generator having hydrogen abstraction ability such as peroxide, and a method of crosslinking by electron beam irradiation. It is done.
- the method of forming crosslinks by introducing functional groups that react with each other into the polymer structure of the resin is preferable because the sea-island structure is easily controlled and the productivity of the intermediate film is increased.
- the intermediate film may contain a compatibilizing agent.
- the compatibilizing agent is appropriately selected so that the sea-island structure can be satisfactorily maintained.
- the compatibilizer is not particularly limited.
- a block copolymer or graft copolymer of a polyvinyl acetal resin and a second resin component particularly a block copolymer or graft copolymer of a polyvinyl acetal resin and (meth) acrylate
- ionic Examples include compatibilizers by interaction. Examples of the compatibilizer having an ionic interaction include a compound having a specific functional group, and the compound may be a polymer.
- the content of the compatibilizer is 0 part by weight (unused) or more, more preferably 0. 0 part by weight with respect to 100 parts by weight in total of the polyvinyl acetal resin and the second resin component. 01 parts by weight or more, preferably 20 parts by weight or less.
- the intermediate film preferably does not contain a plasticizer or contains a plasticizer in an amount of 40% by weight or less in 100% by weight of the intermediate film.
- the intermediate film is more preferably 30% by weight or less, further preferably 20% by weight or less, and particularly preferably 10% by weight in 100% by weight of the intermediate film. Included below.
- the interlayer film does not contain a plasticizer. That is, when the intermediate film contains a plasticizer, the smaller the plasticizer content, the better. The smaller the plasticizer content, the more difficult the plasticizer migrates between the resins, and the sound insulation of the intermediate film is more stably exhibited over a long period of time immediately after fabrication. The physical properties are more difficult to change.
- the physical properties of the multi-layered intermediate film may change until the plasticizer migration reaches equilibrium.
- the intermediate film according to the present invention the physical properties can be prevented from changing over time, and the manufacturing process can be shortened.
- an intermediate film can be reduced in weight. For this reason, the fuel consumption of the motor vehicle using the laminated glass provided with an intermediate film can be made still better, for example.
- the plasticizer is preferably a diester plasticizer represented by the following formula (1).
- R1 and R2 each represent an organic group having 2 to 10 carbon atoms
- R3 represents an ethylene group, an isopropylene group or an n-propylene group
- p represents an integer of 3 to 10
- R1 and R2 in the above formula (1) are each preferably an organic group having 5 to 10 carbon atoms, and more preferably an organic group having 6 to 10 carbon atoms.
- the plasticizer is preferably triethylene glycol di-2-ethylhexanoate (3GO), triethylene glycol di-2-ethylbutyrate (3GH) or triethylene glycol di-2-ethylpropanoate. More preferred is triethylene glycol di-2-ethylhexanoate or triethylene glycol di-2-ethylbutyrate, and even more preferred is triethylene glycol di-2-ethylhexanoate.
- 3GO triethylene glycol di-2-ethylhexanoate
- GGH triethylene glycol di-2-ethylbutyrate
- triethylene glycol di-2-ethylpropanoate More preferred is triethylene glycol di-2-ethylhexanoate or triethylene glycol di-2-ethylbutyrate, and even more preferred is triethylene glycol di-2-ethylhexanoate.
- the intermediate film may contain an antioxidant, an ultraviolet shielding agent, a light stabilizer, a flame retardant, an antistatic agent, a pigment, a dye, an adhesion modifier, a moisture-resistant agent, a fluorescent whitening agent, an infrared absorber, and the like as necessary.
- An additive may be included.
- the thickness of the interlayer film for laminated glass according to the present invention is not particularly limited. From the viewpoint of practical use and from the viewpoint of sufficiently increasing the heat shielding property, the thickness of the intermediate film is preferably 0.1 mm or more, more preferably 0.25 mm or more, preferably 3 mm or less, more preferably 1.5 mm or less. It is. When the thickness of the intermediate film is not less than the above lower limit, the penetration resistance of the laminated glass is increased.
- FIG. 1 An example of the laminated glass using the intermediate film for laminated glasses which concerns on one Embodiment of this invention is shown with sectional drawing.
- a laminated glass 1 shown in FIG. 1 includes an intermediate film 2, a first laminated glass member 21, and a second laminated glass member 22.
- the intermediate film 2 is a single-layer intermediate film.
- the intermediate film 2 is used to obtain a laminated glass.
- the interlayer film 2 is an interlayer film for laminated glass.
- the intermediate film 2 is disposed between the first laminated glass member 21 and the second laminated glass member 22 and is sandwiched.
- a first laminated glass member 21 is laminated on the first surface 2 a (one surface) of the intermediate film 2.
- a second laminated glass member 22 is laminated on a second surface 2 b (the other surface) opposite to the first surface 2 a of the intermediate film 2.
- FIG. 2 is a sectional view showing a modified example of the laminated glass using the interlayer film for laminated glass according to one embodiment of the present invention.
- the laminated glass 11 shown in FIG. 2 includes an intermediate film 12, a first laminated glass member 21, and a second laminated glass member 22.
- the intermediate film 12 is a multilayer intermediate film.
- the intermediate film 12 is used to obtain a laminated glass.
- the intermediate film 12 is an intermediate film for laminated glass.
- the intermediate film 12 has a structure in which three intermediate films of a first layer 13 (intermediate film), a second layer 14 (intermediate film), and a third layer 15 (intermediate film) are laminated in this order.
- the second layer 14 is a sound insulation layer.
- an intermediate film according to an embodiment of the present invention is used as the second layer 14, an intermediate film according to an embodiment of the present invention is used.
- the first layer 13 and the third layer 15 are protective layers.
- the first layer 13 and the third layer 15 may also be intermediate films according to embodiments of the present invention.
- the intermediate film 12 is disposed between the first laminated glass member 21 and the second laminated glass member 22 and is sandwiched.
- the second layer 14 (intermediate film) is also disposed between the first laminated glass member 21 and the second laminated glass member 22 via the first layer 13 and the third layer 15.
- a first laminated glass member 21 is laminated on the outer surface 13 a of the first layer 13.
- a second laminated glass member 22 is laminated on the outer surface 15 a of the third layer 15.
- the laminated glass according to the present invention includes the first laminated glass member, the second laminated glass member, and the interlayer film for laminated glass according to the present invention, wherein the interlayer film for laminated glass is These are disposed between the first laminated glass member and the second laminated glass member.
- the laminated glass may include only the intermediate film for laminated glass according to the present invention as an intermediate film, or may include the intermediate film for laminated glass according to the present invention and another intermediate film for laminated glass. .
- the interlayer film for laminated glass according to the present invention may be used by being laminated on another interlayer film for laminated glass.
- the laminated glass includes at least the interlayer film for laminated glass according to the present invention.
- the laminated glass member examples include a glass plate and a PET (polyethylene terephthalate) film.
- the laminated glass includes not only laminated glass in which an intermediate film is disposed between two glass plates, but also laminated glass in which an intermediate film is disposed between a glass plate and a PET film or the like.
- Laminated glass is a laminated body provided with a glass plate, and preferably at least one glass plate is used.
- the glass plate examples include inorganic glass and organic glass.
- the inorganic glass examples include float plate glass, heat ray absorbing plate glass, heat ray reflecting plate glass, polished plate glass, mold plate glass, netted plate glass, and lined plate glass.
- the organic glass is a synthetic resin glass substituted for inorganic glass.
- the organic glass examples include polycarbonate plates and poly (meth) acrylic resin plates.
- the poly (meth) acrylic resin plate examples include a polymethyl (meth) acrylate plate.
- the thickness of the laminated glass member is preferably 1 mm or more, preferably 5 mm or less, more preferably 3 mm or less.
- the thickness of the glass plate is preferably 1 mm or more, preferably 5 mm or less, more preferably 3 mm or less.
- the thickness of the PET film is preferably 0.03 mm or more, and preferably 0.5 mm or less.
- the method for producing the laminated glass is not particularly limited.
- the first laminated glass member is sandwiched between a first laminated glass member and a second laminated glass member, passed through a pressing roll, or placed in a rubber bag and sucked under reduced pressure, to form a first laminated glass. Air remaining between the member and the intermediate film and between the second laminated glass member and the intermediate film is degassed. Thereafter, it is pre-bonded at about 70 to 110 ° C. to obtain a laminate.
- the laminate is put in an autoclave or pressed and pressed at about 120 to 150 ° C. and a pressure of 1 to 1.5 MPa. In this way, a laminated glass can be obtained.
- the interlayer film and the laminated glass can be used for automobiles, railway vehicles, aircraft, ships, buildings, and the like.
- the said intermediate film and the said laminated glass can be used besides these uses.
- the interlayer film and the laminated glass are preferably a vehicle or architectural interlayer film and a laminated glass, and more preferably a vehicle interlayer film and a laminated glass.
- the intermediate film and the laminated glass can be used for an automobile windshield, side glass, rear glass, roof glass, or the like.
- Example 1 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 67.0 mol%, hydroxyl group content 32.0 mol% Acetylation degree 1.0 mol%) 10 parts by weight, 30 parts by weight of ethyl acrylate and 60 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was applied onto a release-treated PET (polyethylene terephthalate) film and dried at 80 ° C. for 1 hour to obtain a film formed of the polyvinyl acetal resin composition.
- the obtained interlayer film was cut into a length of 30 mm and a width of 320 mm. Next, an interlayer film was sandwiched between two transparent float glasses (length 25 mm ⁇ width 305 mm ⁇ thickness 2.0 mm), held in a vacuum laminator at 90 ° C. for 30 minutes, and vacuum pressed to obtain a laminate. . In the laminate, the intermediate film portion protruding from the glass was cut off to obtain a laminated glass used for measurement of the loss factor.
- Example 2 Preparation of a film formed from a polyvinyl acetal resin composition
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% Acetylation degree 1.2 mol% 10 parts by weight, ethyl acrylate 15 parts by weight, 2-ethylhexyl acrylate 7.5 parts by weight, benzyl acrylate 7.5 parts by weight, and acetic acid as a polymerization solvent 60 parts by weight of ethyl was added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 3 Preparation of a film formed from a polyvinyl acetal resin composition
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 67.0 mol%, hydroxyl group content 32.0 mol% , Degree of acetylation 1.0 mol%) 5 parts by weight, 20 parts by weight of ethyl acrylate and 75 parts by weight of ethyl acetate as a polymerization solvent were added, and polyvinyl butyral was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 4 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 3300, butyralization degree 67.0 mol%, hydroxyl group content 30.8 mol% , Degree of acetylation 2.2 mol%) 5 parts by weight, 43 parts by weight of ethyl acrylate, and 100 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 5 Preparation of a film formed from a polyvinyl acetal resin composition
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% , Degree of acetylation 1.2 mol% 20 parts by weight, 25 parts by weight of ethyl acrylate and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 6 Preparation of a film formed from a polyvinyl acetal resin composition
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% , Degree of acetylation 1.2 mol% 10 parts by weight, 20 parts by weight of ethyl acrylate and 70 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 7 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% Acetylation degree 1.2 mol%) 10 parts by weight, 25 parts by weight of ethyl acrylate, and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 8 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 65.0 mol%, hydroxyl group content 34.0 mol% Acetylation degree 1.0 mol%) 10 parts by weight, 6.6 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, and 8.4 butyl acrylate.
- Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 9 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 65.8 mol%, hydroxyl group content 33.0 mol% Acetylation degree 1.2 mol%) 10 parts by weight, 6.6 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, and 8.4 butyl acrylate.
- Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 10 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 2500, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% Acetylation degree 1.2 mol%) 10 parts by weight, 6.6 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, and 8.4 butyl acrylate.
- Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 11 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% Acetylation degree: 1.2 mol%) 10 parts by weight, 15 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 4-hydroxybutyl acrylate, and 65 parts by weight of ethyl acetate as a polymerization solvent The polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 12 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 67.0 mol%, hydroxyl group content 32.0 mol% Acetylation degree 1.0 mol%) 10 parts by weight, ethyl acrylate 12 parts by weight, benzyl acrylate 6 parts by weight, 4-hydroxybutyl acrylate 9 parts by weight, acrylic acid 3 parts by weight, polymerization 65 parts by weight of ethyl acetate as a solvent was added, and the polyvinyl acetal resin was dissolved while stirring.
- 3GO triethylene glycol di-2-ethylhexanoate
- the obtained solution was applied onto a release-treated PET film and dried at 80 ° C. for 1 hour to obtain a film formed of a polyvinyl acetal resin composition.
- a laminated glass was produced by the same operation as in Example 1.
- Example 13 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 67.0 mol%, hydroxyl group content 32.0 mol% Acetylation degree 1.0 mol%) 10 parts by weight, ethyl acrylate 3 parts by weight, benzyl acrylate 6 parts by weight, butyl acrylate 6 parts by weight, 4-hydroxybutyl acrylate 9 parts by weight, 3 parts by weight of acrylic acid, 3 parts by weight of glycidyl methacrylate, and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 14 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 65.2 mol%, hydroxyl group content 33.9 mol% Acetylation degree 0.9 mol%) 10 parts by weight, polybutadiene elastomer (“RB810” manufactured by JSR) 30 parts by weight, and 8 parts by weight of triethylene glycol di-2-ethylhexanoate (3GO) as a plasticizer And kneaded sufficiently with a mixing roll to obtain a film formed of the polyvinyl acetal resin composition.
- polyvinyl butyral resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 65.2 mol%, hydroxyl group content 33.9 mol% Acetylation degree 0.9 mol%
- RB810 polybutadiene elastomer
- 3GO triethylene glycol di-2
- a laminated glass was produced by the same operation as in Example 1.
- Example 15 (Preparation of a film formed from a polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 65.2 mol%, hydroxyl group content 33.9 mol% Acetylation degree 0.9 mol%) 10 parts by weight and 30 parts by weight of styrene butadiene copolymer ("Tough Tech H1221" manufactured by Asahi Kasei Co., Ltd.) are added and kneaded sufficiently with a mixing roll to form a polyvinyl acetal resin composition. Film was obtained.
- a laminated glass was produced by the same operation as in Example 1.
- Example 16 (Preparation of intermediate layer film formed of polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 65.2 mol%, hydroxyl group content 33.9 mol% Acetylation degree 0.9 mol%) 10 parts by weight, 6.6 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, and 8.4% of butyl acrylate.
- Part by weight and 60 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- (Preparation of intermediate layer (intermediate film)) A film formed from the obtained polyvinyl acetal resin composition was molded using an extruder to produce an intermediate layer of an intermediate film having a thickness of 0.1 mm.
- (Preparation of surface layer) 100 parts by weight of polyvinyl acetal resin (polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 65.2 mol%, hydroxyl group content 33.9 mol%, acetylation degree 0.9 mol%) 30 parts by weight of ethylene glycol di-2-ethylhexanoate (3GO) was molded using an extruder to produce an intermediate film (surface layer) having a thickness of 0.33 mm.
- (Preparation of interlayer film) A surface layer, an intermediate layer, and a surface layer were laminated in this order to produce an intermediate film.
- a laminated glass was produced by the same operation as in Example 1.
- Example 17 (Preparation of intermediate layer film formed of polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 67.0 mol%, hydroxyl group content 32.0 mol% Acetylation degree 1.0 mol%) 10 parts by weight, 6.6 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, and 8.4 butyl acrylate.
- Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 18 (Preparation of intermediate layer film formed of polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 3300, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% Acetylation degree 1.2 mol%) 10 parts by weight, 6.6 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, and 8.4 butyl acrylate.
- Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Example 19 (Preparation of intermediate layer film formed of polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 800, butyralization degree 65.2 mol%, hydroxyl group content 33.9 mol% Acetylation degree 0.9 mol%) 10 parts by weight, 8.4 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, 6.6 parts of butyl acrylate Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- 3GO triethylene glycol di-2-ethylhexanoate
- the obtained solution was applied onto a release-treated PET film and dried at 80 ° C. for 1 hour to obtain a film formed of a polyvinyl acetal resin composition.
- a laminated glass was produced by the same operation as in Example 1.
- Example 20 (Preparation of intermediate layer film formed of polyvinyl acetal resin composition)
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 67.0 mol%, hydroxyl group content 32.0 mol% Acetylation degree 1.0 mol%) 10 parts by weight, 8.4 parts by weight of ethyl acrylate, 6 parts by weight of benzyl acrylate, 9 parts by weight of 2-hydroxyethyl acrylate, 6.6 parts of butyl acrylate Part by weight and 65 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- 3GO triethylene glycol di-2-ethylhexanoate
- the obtained solution was applied onto a release-treated PET film and dried at 80 ° C. for 1 hour to obtain a film formed of a polyvinyl acetal resin composition.
- a laminated glass was produced by the same operation as in Example 1.
- Comparative Example 1 In Comparative Example 1, the second resin component was not used.
- a laminated glass was produced by the same operation as in Example 1.
- Comparative Example 2 In Comparative Example 2, the second resin component was not used.
- resin composition (1) for forming sound insulation layer (1) To 100 parts by weight of polyvinyl acetal resin (polyvinyl butyral resin, average polymerization degree 2100, butyralization degree 65 mol%, hydroxyl group content 22 mol%, acetylation degree 13 mol%), triethylene glycol di-diene which is a plasticizer. A resin composition (1) was prepared by adding 30 parts by weight of 2-ethylhexanoate (3GO) and thoroughly kneading with a mixing roll.
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 2100, butyralization degree 65 mol%, hydroxyl group content 22 mol%, acetylation degree 13 mol%
- a resin composition (1) was prepared by adding 30 parts by weight of 2-ethylhexanoate (3GO) and thoroughly kneading with a mixing roll.
- resin composition (2) for forming sound insulation layer (2) To 100 parts by weight of polyvinyl acetal resin (polyvinyl butyral resin, average polymerization degree 2100, butyralization degree 65 mol%, hydroxyl group content 22 mol%, acetylation degree 13 mol%), triethylene glycol diester as a plasticizer A resin composition (2) was prepared by adding 60 parts by weight of -2-ethylhexanoate (3GO) and thoroughly kneading with a mixing roll.
- polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 2100, butyralization degree 65 mol%, hydroxyl group content 22 mol%, acetylation degree 13 mol%
- 3GO -2-ethylhexanoate
- resin composition (3) for forming the intermediate layer To 100 parts by weight of a polyvinyl acetal resin (polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 65 mol%, hydroxyl group content 34 mol%, acetylation degree 1 mol%), triethylene glycol di-ethylene as a plasticizer A resin composition (3) was prepared by adding 40 parts by weight of 2-ethylhexanoate (3GO) and thoroughly kneading with a mixing roll.
- a polyvinyl acetal resin polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 65 mol%, hydroxyl group content 34 mol%, acetylation degree 1 mol%
- a resin composition (3) was prepared by adding 40 parts by weight of 2-ethylhexanoate (3GO) and thoroughly kneading with a mixing roll.
- the resin composition (1) was sandwiched between two fluororesin sheets via a clearance plate (thickness: 100 ⁇ m) and press molded at 150 ° C. to obtain a sound insulation layer (1) having a thickness of 100 ⁇ m.
- the resin composition (2) was sandwiched between two fluororesin sheets via a clearance plate (thickness: 100 ⁇ m) and press molded at 150 ° C. to obtain a sound insulation layer (2) having a thickness of 100 ⁇ m.
- the resin composition (3) was sandwiched between two fluororesin sheets via a clearance plate (thickness: 600 ⁇ m) and press molded at 150 ° C. to obtain an intermediate layer having a thickness of 600 ⁇ m.
- a laminated body in which the sound insulation layer (1), the intermediate layer, and the sound insulation layer (2) are laminated in this order is sandwiched between two fluororesin sheets via a clearance plate (thickness: 800 ⁇ m), and the temperature is increased to 150 ° C. And an interlayer film for laminated glass having a thickness of 800 ⁇ m was obtained.
- the obtained interlayer film was cut into a length of 30 mm and a width of 320 mm.
- an intermediate film is sandwiched between two transparent float glasses (length 25 mm ⁇ width 305 mm ⁇ thickness 2.0 mm), placed in a rubber bag, deaerated at a vacuum degree of 2.6 kPa for 20 minutes, Vacuum pressing was performed at 90 ° C. for 30 minutes.
- the laminated body preliminarily pressure-bonded in this manner was pressure-bonded for 20 minutes in an autoclave under conditions of 135 ° C. and a pressure of 1.2 MPa to produce a laminated body.
- the intermediate film portion protruding from the glass was cut off to obtain a laminated glass used for measurement of the loss factor.
- Comparative Example 3 (Comparative Example 3) In Comparative Example 3, an intermediate film having no sea-island structure was produced.
- a reaction vessel equipped with a thermometer, a stirrer, a nitrogen introduction tube, and a cooling tube, and then nitrogen gas is added to 30 parts by weight.
- the reaction vessel was purged with nitrogen for a minute and then heated to 85 ° C. with stirring in the reaction vessel.
- a polymerization initiator solution obtained by diluting 0.1 parts by weight of t-butylperoxy-2-ethylhexanoate as a polymerization initiator with 5 parts by weight of ethyl acetate was placed in the reaction vessel for 3 hours.
- Comparative Example 4 In Comparative Example 4, the second resin component was not used. As a resin component similar to the second resin component, a resin component having a glass transition temperature of 15 ° C. was used.
- polyvinyl acetal resin (polyvinyl butyral resin, average polymerization degree 1700, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% , Degree of acetylation 1.2 mol%) 10 parts by weight, 40 parts by weight of benzyl acrylate and 60 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Comparative Example 5 (Comparative Example 5) In Comparative Example 5, a large amount of polyvinyl acetal resin and a small amount of the second resin component were used.
- polyvinyl acetal resin (polyvinyl butyral resin, average polymerization degree 800, butyralization degree 68.0 mol%, hydroxyl group content 30.8 mol% , Degree of acetylation 1.2 mol%) 25 parts by weight, 15 parts by weight of ethyl acrylate and 60 parts by weight of ethyl acetate as a polymerization solvent were added, and the polyvinyl acetal resin was dissolved while stirring.
- the obtained solution was apply
- a laminated glass was produced by the same operation as in Example 1.
- Resin was deposited to a thickness of 0.5 mm or more by hot pressing.
- the obtained film was cut into a circle having a diameter of 8 mm, and the rate of temperature increase was measured using a viscoelasticity measuring apparatus (“ARES” manufactured by Rheometrics) under the conditions of a strain amount of 1.0% and a frequency of 1 Hz.
- the glass transition temperature was measured by measuring the temperature distribution of dynamic viscoelasticity at 5 ° C./min.
- the obtained interlayer film was cut into a circle with a diameter of 8 mm, and the temperature was raised by using a viscoelasticity measuring device (“ARES” manufactured by Rheometrics) under the conditions of a strain amount of 1.0% and a frequency of 1 Hz.
- RAS viscoelasticity measuring device
- the obtained intermediate film was processed with a microtome to produce a slice having a thickness of about 100 nm.
- the resin constituting the sea part of the sea-island structure is a polyvinyl acetal resin (PVB) or a second resin component (R2 ).
- the loss factor was measured by a central vibration method using a measuring device (“SA-01” manufactured by Rion Co., Ltd.) at 20 ° C. The fourth-order mode of the resonance frequency of the obtained loss factor. The loss factor (20 ° C. loss factor) at (around 3150 Hz) was evaluated.
- the loss factor was measured by the central excitation method at 30 ° C.
- the loss factor (30 ° C. loss factor) in the sixth-order mode (around 6300 Hz) of the resonance frequency of the obtained loss factor was evaluated.
- the obtained laminated glass was stored at 23 ° C. for 1 month, and then the 20 ° C. loss coefficient and the 30 ° C. loss coefficient were measured.
Abstract
Description
上記中間膜の周波数1Hzでの動的粘弾性スペクトルにおいて、上記ポリビニルアセタール樹脂に由来する損失正接の極大値を示す温度は好ましくは50℃以上であり、より好ましくは60℃以上であり、更に好ましくは64℃以上である。上記ポリビニルアセタール樹脂に由来する損失正接の極大値を示す温度は100℃以下であってもよい。
上記第2の樹脂成分のガラス転移温度は-15℃以上、5℃以下である。遮音性をより一層高める観点からは、上記中間膜の周波数1Hzでの動的粘弾性スペクトルにおいて、上記第2の樹脂成分に由来する損失正接の極大値を示す温度は好ましくは-15℃以上、好ましくは5℃以下であり、更に上記第2の樹脂成分に由来する損失正接の極大値は好ましくは0.35以上、より好ましくは0.4以上、更に好ましくは0.5以上である。上記第2の樹脂成分に由来する損失正接の極大値は特に好ましくは1以上である。
上記中間膜は、相溶化剤を含んでいてもよい。上記相溶化剤は、海島構造を良好に維持可能なように適宜選択される。上記相溶化剤としては特に限定されず、例えばポリビニルアセタール樹脂と第2の樹脂成分とのブロックコポリマー又はグラフトコポリマー(特にポリビニルアセタール樹脂と(メタ)アクリレートとのブロックコポリマー又はグラフトコポリマー)、並びにイオン的相互作用による相溶化剤等が挙げられる。上記イオン的相互作用を有する相溶化剤としては、特定の官能基を有する化合物が挙げられ、該化合物はポリマーであってもよい。
上記中間膜は、可塑剤を含まないか、又は上記中間膜100重量%中で、可塑剤を40重量%以下で含むことが好ましい。上記中間膜が可塑剤を含む場合に、上記中間膜は、上記中間膜100重量%中で、可塑剤をより好ましくは30重量%以下、更に好ましくは20重量%以下、特に好ましくは10重量%以下で含む。上記中間膜は、可塑剤を含まないことがより好ましい。すなわち、上記中間膜が可塑剤を含む場合には、可塑剤の含有量は少ないほどよい。上記可塑剤の含有量が少ないほど、上記可塑剤が樹脂間で移行し難くなり、上記中間膜の遮音性が作製直後から長期にわたってより一層安定的に発揮され、上記中間膜の他の様々な物性もより一層変化し難くなる。例えば、複数の層が積層されており、かつ各層で可塑剤の含有量の異なる多層の中間膜では、可塑剤の移行が平衡に達するまで、上記多層の中間膜の物性が変わることがあるのに対し、本発明に係る中間膜では、時間の経過によって物性が変わるのを抑えることができ、製造工程を短縮することもできる。また、可塑剤の含有量が少ないと、中間膜を軽量化することができる。このため、例えば、中間膜を備える合わせガラスを用いた自動車の燃費をより一層良好にすることができる。
上記中間膜は、必要に応じて酸化防止剤、紫外線遮蔽剤、光安定剤、難燃剤、帯電防止剤、顔料、染料、接着力調整剤、耐湿剤、蛍光増白剤及び赤外線吸収剤等の添加剤を含んでいてもよい。
本発明に係る合わせガラス用中間膜の厚みは特に限定されない。実用面の観点、並びに遮熱性を充分に高める観点からは、上記中間膜の厚みは、好ましくは0.1mm以上、より好ましくは0.25mm以上、好ましくは3mm以下、より好ましくは1.5mm以下である。中間膜の厚みが上記下限以上であると、合わせガラスの耐貫通性が高くなる。
図1に、本発明の一実施形態に係る合わせガラス用中間膜を用いた合わせガラスの一例を断面図で示す。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)10重量部と、アクリル酸エチル30重量部と、重合溶媒である酢酸エチル60重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
得られたポリビニルアセタール樹脂組成物により形成されたフィルムを、押出機を用いて成形し、厚みが0.5mmである単層の中間膜を作製した。
得られた中間膜を、縦30mm×横320mmに切り出した。次に、2枚の透明なフロートガラス(縦25mm×横305mm×厚み2.0mm)の間に中間膜を挟み込み、真空ラミネーターに90℃で30分間保持し、真空プレスし、積層体を得た。積層体において、ガラスからはみ出た中間膜部分を切り落とし、損失係数の測定に用いる合わせガラスを得た。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル15重量部と、アクリル酸2-エチルヘキシル7.5重量部と、アクリル酸ベンジル7.5重量部と、重合溶媒である酢酸エチル60重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)5重量部と、アクリル酸エチル20重量部と、重合溶媒である酢酸エチル75重量部とを加え、撹拌しながらポリビニルブチラールを溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度3300、ブチラール化度67.0モル%、水酸基の含有率30.8モル%、アセチル化度2.2モル%)5重量部と、アクリル酸エチル43重量部と、重合溶媒である酢酸エチル100重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)20重量部と、アクリル酸エチル25重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル20重量部と、重合溶媒である酢酸エチル70重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル25重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度65.0モル%、水酸基の含有率34.0モル%、アセチル化度1.0モル%)10重量部と、アクリル酸エチル6.6重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル8.4重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度65.8モル%、水酸基の含有率33.0モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル6.6重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル8.4重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度2500、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル6.6重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル8.4重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル15重量部と、アクリル酸ベンジル6重量部と、アクリル酸4-ヒドロキシブチル9重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)10重量部と、アクリル酸エチル12重量部と、アクリル酸ベンジル6重量部と、アクリル酸4-ヒドロキシブチル9重量部と、アクリル酸3重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)10重量部と、アクリル酸エチル3重量部と、アクリル酸ベンジル6重量部と、アクリル酸ブチル6重量部と、アクリル酸4-ヒドロキシブチル9重量部と、アクリル酸3重量部と、メタクリル酸グリシジル3重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度65.2モル%、水酸基の含有率33.9モル%、アセチル化度0.9モル%)10重量部と、ポリブタジエンエラストマー(JSR社製「RB810」)30重量部と、可塑剤としてトリエチレングリコールジ-2-エチルヘキサノエート(3GO)8重量部とを加え、ミキシングロールにて充分混練し、ポリビニルアセタール樹脂組成物により形成されたフィルムを得た。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成されたフィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度65.2モル%、水酸基の含有率33.9モル%、アセチル化度0.9モル%)10重量部と、スチレンブタジエンコポリマー(旭化成社製「タフテックH1221」)30重量部とを加え、ミキシングロールにて充分混練し、ポリビニルアセタール樹脂組成物により形成されたフィルムを得た。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成された中間層用フィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度65.2モル%、水酸基の含有率33.9モル%、アセチル化度0.9モル%)10重量部と、アクリル酸エチル6.6重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル8.4重量部と、重合溶媒である酢酸エチル60重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
得られたポリビニルアセタール樹脂組成物により形成されたフィルムを、押出機を用いて成形し、厚みが0.1mmである中間膜の中間層を作製した。
(表面層の作製)
ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度65.2モル%、水酸基の含有率33.9モル%、アセチル化度0.9モル%)100重量部と、可塑剤としてトリエチレングリコールジ-2-エチルヘキサノエート(3GO)30重量部とを押出機を用いて成形し、厚みが0.33mmである中間膜(表面層)を作製した。
(中間膜の作製)
表面層、中間層、及び表面層をこの順番に積層して中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成された中間層用フィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)10重量部と、アクリル酸エチル6.6重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル8.4重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例16と同様の操作により中間膜を作製した。表面層は実施例16と同じである。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成された中間層用フィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度3300、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸エチル6.6重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル8.4重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例16と同様の操作により中間膜を作製した。表面層は実施例16と同じである。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成された中間層用フィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度65.2モル%、水酸基の含有率33.9モル%、アセチル化度0.9モル%)10重量部と、アクリル酸エチル8.4重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル6.6重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例16と同様の操作により中間膜を作製した。表面層は実施例16と同じである。
実施例1と同様の操作により合わせガラスを作製した。
(ポリビニルアセタール樹脂組成物により形成された中間層用フィルムの作製)
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)10重量部と、アクリル酸エチル8.4重量部と、アクリル酸ベンジル6重量部と、アクリル酸2-ヒドロキシエチル9重量部と、アクリル酸ブチル6.6重量部と、重合溶媒である酢酸エチル65重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例16と同様の操作により中間膜を作製した。表面層は実施例16と同じである。
実施例1と同様の操作により合わせガラスを作製した。
比較例1では、第2の樹脂成分を用いなかった。
ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)40重量部を、溶剤(メタノールとトルエンとの混合溶剤、メタノール:トルエン=1:1(重量比))により希釈し、固形分20重量%の溶液を得た。得られた溶液に、可塑剤であるフタル酸ジオクチル2.5重量部(得られる中間膜中で5.9重量%)を添加した。次に、可塑剤が添加された溶液を離型処理されたPETフィルム上に塗布し、80℃で1時間乾燥させて、ポリビニルアセタール樹脂と可塑剤とにより形成されたフィルムを得た。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
比較例2では、第2の樹脂成分を用いなかった。
ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度2100、ブチラール化度65モル%、水酸基の含有率22モル%、アセチル化度13モル%)100重量部に、可塑剤であるトリエチレングリコール-ジ-2-エチルヘキサノエート(3GO)30重量部を添加し、ミキシングロールで充分に混練することにより、樹脂組成物(1)を調製した。
ポリビニルアセアタール樹脂(ポリビニルブチラール樹脂、平均重合度2100、ブチラール化度65モル%、水酸基の含有率22モル%、アセチル化度13モル%)100重量部に、可塑剤であるトリエチレングリコール-ジ-2-エチルヘキサノエート(3GO)60重量部を添加し、ミキシングロールで充分に混練することにより、樹脂組成物(2)を調製した。
ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度65モル%、水酸基の含有率34モル%、アセチル化度1モル%)100重量部に、可塑剤であるトリエチレングリコール-ジ-2-エチルヘキサノエート(3GO)40重量部を添加し、ミキシングロールで充分に混練することにより、樹脂組成物(3)を調製した。
樹脂組成物(1)を2枚のフッ素樹脂シート間に、クリアランス板(厚み100μm)を介して挟み込み、150℃にてプレス成形して、厚みが100μmである遮音層(1)を得た。
得られた中間膜を、縦30mm×横320mmに切り出した。次に、2枚の透明なフロートガラス(縦25mm×横305mm×厚み2.0mm)の間に中間膜を挟み込み、ゴムバック内に入れ、2.6kPaの真空度で20分間脱気した後、90℃で30分間、真空プレスした。このようにして予備圧着された積層体を、オートクレーブで135℃、圧力1.2MPaの条件で20分間圧着を行い、積層体を作製した。積層体において、ガラスからはみ出た中間膜部分を切り落とし、損失係数の測定に用いる合わせガラスを得た。
比較例3では、海島構造を有さない中間膜を作製した。
ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度67.0モル%、水酸基の含有率32.0モル%、アセチル化度1.0モル%)10重量部を、溶剤(メタノールとトルエンとの混合溶剤、メタノール:トルエン=1:1(重量比))により希釈し、固形分20重量%の溶液を得た。次に、得られた溶液を離型処理されたPETフィルム上に塗布し、常温(23℃)で1時間風乾した後、熱風乾燥機で80℃で1時間乾燥して、ポリビニルアセタール樹脂により形成されたフィルムを得た。
得られたポリビニルアセタール樹脂により形成されたフィルムを、押出機を用いて成形し、厚みが0.125mmである単層の中間膜を作製した。次に、得られたポリアクリル酸エステル樹脂により形成されたフィルムを、押出機を用いて成形し、厚みが0.375mmである単層の中間膜を作製した。
得られた2つの中間膜を積層し、実施例1と同様の操作により、合わせガラスを作製した。
比較例4では、第2の樹脂成分を用いなかった。第2の樹脂成分に類似する樹脂成分として、ガラス転移温度が15℃である樹脂成分を用いた。
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度1700、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)10重量部と、アクリル酸ベンジル40重量部と、重合溶媒である酢酸エチル60重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
比較例5では、ポリビニルアセタール樹脂を多く、第2の樹脂成分を少なく用いた。
温度計、攪拌機、窒素導入管及び冷却管を備えた反応容器内に、ポリビニルアセタール樹脂(ポリビニルブチラール樹脂、平均重合度800、ブチラール化度68.0モル%、水酸基の含有率30.8モル%、アセチル化度1.2モル%)25重量部と、アクリル酸エチル15重量部と、重合溶媒である酢酸エチル60重量部とを加え、撹拌しながらポリビニルアセタール樹脂を溶解させた。
実施例1と同様の操作により中間膜を作製した。
実施例1と同様の操作により合わせガラスを作製した。
(ガラス転移温度の測定)
用いた樹脂のガラス転移温度は、以下のようにして測定した。
得られた中間膜を直径8mmの円形に切り抜き、粘弾性測定装置(レオメトリックス社製「ARES」)を用いて、せん断法にて、ひずみ量1.0%及び周波数1Hzの条件で、昇温速度5℃/分で動的粘弾性の温度分散測定を行うことにより、最も低温側に現れる損失正接のピーク温度、及び、最も低温側に現れる損失正接のピーク温度における損失正接の最大値(極大値)を測定した。
得られた中間膜をマイクロトームで処理することにより、厚さ100nm程度の切片を作製した。得られた切片を四酸化オスミウムにて染色し、透過型電子顕微鏡で観察することにより、海島構造の海部を構成する樹脂が、ポリビニルアセタール樹脂(PVB)であるか、第2の樹脂成分(R2)であるかを確認した。
得られた合わせガラスについて、測定装置(リオン社製「SA-01)を用いて、20℃の条件で中央加振法により損失係数を測定した。得られた損失係数の共振周波数の4次モード(3150Hz付近)での損失係数(20℃損失係数)を評価した。
得られた合わせガラスを23℃にて1カ月保存した後、上記20℃損失係数及び上記30℃損失係数を測定した。
2…中間膜
2a…第1の表面
2b…第2の表面
11…合わせガラス
12…中間膜
13…第1の層(中間膜)
14…第2の層(中間膜)
15…第3の層(中間膜)
13a…外側の表面
15a…外側の表面
21…第1の合わせガラス部材
22…第2の合わせガラス部材
Claims (11)
- ポリビニルアセタール樹脂と、ガラス転移温度が-15℃以上、5℃以下である第2の樹脂成分とを含み、
前記ポリビニルアセタール樹脂と前記第2の樹脂成分との合計100重量%中、前記ポリビニルアセタール樹脂の含有量が10重量%以上、50重量%以下であり、前記第2の樹脂成分の含有量が50重量%以上、90重量%以下であり、
中間膜中で、前記ポリビニルアセタール樹脂と前記第2の樹脂成分とが海島構造を有する、合わせガラス用中間膜。 - 中間膜中で、前記ポリビニルアセタール樹脂と前記第2の樹脂成分とが全体で海島構造を有する、請求項1に記載の合わせガラス用中間膜。
- 周波数1Hzでの動的粘弾性スペクトルにおいて、前記ポリビニルアセタール樹脂に由来する損失正接の極大値を示す温度が50℃以上であり、前記第2の樹脂成分に由来する損失正接の極大値を示す温度が-15℃以上、5℃以下であり、かつ、前記第2の樹脂成分に由来する損失正接の極大値が0.4以上である、請求項1又は2に記載の合わせガラス用中間膜。
- 可塑剤を含まないか、又は中間膜100重量%中で、可塑剤を40重量%以下で含む、請求項1~3のいずれか1項に記載の合わせガラス用中間膜。
- 可塑剤を含まないか、又は中間膜100重量%中で、可塑剤を20重量%以下で含む、請求項4に記載の合わせガラス用中間膜。
- 可塑剤を含まないか、又は中間膜100重量%中で、可塑剤を10重量%以下で含む、請求項5に記載の合わせガラス用中間膜。
- 可塑剤を含まない、請求項6に記載の合わせガラス用中間膜。
- 前記ポリビニルアセタール樹脂の少なくとも一部と前記第2の樹脂成分の少なくとも一部とが重合している、請求項1~7のいずれか1項に記載の合わせガラス用中間膜。
- 前記第2の樹脂成分が、(メタ)アクリル樹脂である、請求項1~8のいずれか1項に記載の合わせガラス用中間膜。
- 前記ポリビニルアセタール樹脂の存在下で、(メタ)アクリロイル基を有するモノマーを重合させることにより得られる、請求項1~9のいずれか1項に記載の合わせガラス用中間膜。
- 第1の合わせガラス部材と、
第2の合わせガラス部材と、
請求項1~10のいずれか1項に記載の合わせガラス用中間膜とを備え、
前記第1の合わせガラス部材と前記第2の合わせガラス部材との間に、前記合わせガラス用中間膜が配置されている、合わせガラス。
Priority Applications (7)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020157027034A KR20160065045A (ko) | 2013-09-30 | 2014-09-30 | 접합 유리용 중간막 및 접합 유리 |
EP14848708.5A EP3053890B1 (en) | 2013-09-30 | 2014-09-30 | Intermediate film for laminated glass, and laminated glass |
JP2014549238A JP5744345B1 (ja) | 2013-09-30 | 2014-09-30 | 合わせガラス用中間膜及び合わせガラス |
RU2016116969A RU2646641C2 (ru) | 2013-09-30 | 2014-09-30 | Промежуточная пленка для многослойного стекла и многослойное стекло |
US14/917,510 US11014340B2 (en) | 2013-09-30 | 2014-09-30 | Intermediate film for laminated glass, and laminated glass |
CN201480031360.6A CN105324345B (zh) | 2013-09-30 | 2014-09-30 | 夹层玻璃用中间膜及夹层玻璃 |
MX2016003514A MX2016003514A (es) | 2013-09-30 | 2014-09-30 | Pelicula intermedia para vidrio laminado, y vidrio laminado. |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013-204323 | 2013-09-30 | ||
JP2013204323 | 2013-09-30 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2015046583A1 true WO2015046583A1 (ja) | 2015-04-02 |
Family
ID=52743704
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2014/076142 WO2015046583A1 (ja) | 2013-09-30 | 2014-09-30 | 合わせガラス用中間膜及び合わせガラス |
Country Status (8)
Country | Link |
---|---|
US (1) | US11014340B2 (ja) |
EP (1) | EP3053890B1 (ja) |
JP (2) | JP5744345B1 (ja) |
KR (1) | KR20160065045A (ja) |
CN (1) | CN105324345B (ja) |
MX (1) | MX2016003514A (ja) |
RU (1) | RU2646641C2 (ja) |
WO (1) | WO2015046583A1 (ja) |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015125932A1 (ja) * | 2014-02-20 | 2015-08-27 | 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 |
WO2016052671A1 (ja) * | 2014-09-30 | 2016-04-07 | 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 |
WO2016158694A1 (ja) * | 2015-03-31 | 2016-10-06 | 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 |
WO2018181748A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181751A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181747A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181754A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181757A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181755A1 (ja) * | 2017-03-31 | 2018-10-04 | 積水化学工業株式会社 | 成形体及び合わせガラス |
WO2018181758A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
EP3357990A4 (en) * | 2015-09-30 | 2019-05-08 | Sekisui Chemical Co., Ltd. | ADHESIVE |
JP2019147705A (ja) * | 2018-02-27 | 2019-09-05 | 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 |
US10711128B2 (en) | 2015-09-30 | 2020-07-14 | Sekisui Chemical Co., Ltd. | Modified polyvinyl acetal resin composition |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP3476811B1 (en) * | 2016-06-24 | 2022-01-26 | Agc Inc. | Laminated glass |
WO2018029995A1 (ja) * | 2016-08-12 | 2018-02-15 | 旭硝子株式会社 | 合わせガラス |
JP7028769B2 (ja) * | 2017-03-31 | 2022-03-02 | 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 |
US10438575B2 (en) | 2017-11-20 | 2019-10-08 | Chang Chun Petrochemical Co., Ltd. | Multilayer film, interlayer film comprising the multilayer film and laminated glass and sound-insulating glass laminate comprising the interlayer film |
JP2019147707A (ja) * | 2018-02-27 | 2019-09-05 | 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 |
CN112789312B (zh) * | 2018-09-26 | 2023-03-03 | 可乐丽欧洲有限责任公司 | 吸收增塑剂而成的聚乙烯醇缩醛树脂薄膜的制造方法 |
WO2020130117A1 (ja) | 2018-12-21 | 2020-06-25 | 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 |
KR102169978B1 (ko) * | 2019-03-18 | 2020-10-27 | 에스케이씨 주식회사 | 유리접합용 필름 및 이를 포함하는 광투과적층체 |
WO2021117835A1 (ja) * | 2019-12-11 | 2021-06-17 | 積水化学工業株式会社 | 樹脂組成物、該樹脂組成物からなる樹脂フィルム、該樹脂フィルムを備えるガラス積層体 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07118347A (ja) * | 1993-10-22 | 1995-05-09 | Sekisui Chem Co Ltd | 遮音性中間膜 |
JP2000272936A (ja) * | 1999-03-25 | 2000-10-03 | Sekisui Chem Co Ltd | 合わせガラス用中間膜及び合わせガラス |
JP2007070200A (ja) | 2005-09-09 | 2007-03-22 | Asahi Glass Co Ltd | 合わせガラス |
JP2007297571A (ja) * | 2006-05-08 | 2007-11-15 | Sekisui Chem Co Ltd | 透明積層体用中間膜及び透明積層体 |
WO2012026393A1 (ja) * | 2010-08-23 | 2012-03-01 | 株式会社クラレ | 太陽電池用封止材および合わせガラス用中間膜 |
JP2014224234A (ja) * | 2013-04-26 | 2014-12-04 | 積水化学工業株式会社 | ポリビニルアセタール系樹脂組成物 |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5914739B2 (ja) * | 1976-06-24 | 1984-04-05 | コニカ株式会社 | カラ−拡散転写法 |
JPS6016839A (ja) * | 1983-07-05 | 1985-01-28 | Nippon Sheet Glass Co Ltd | 積層ガラスのプレスロ−ル装置 |
US6383647B1 (en) * | 1998-09-30 | 2002-05-07 | Sekisui Chemical Co., Ltd. | Intermediate film for laminated glass and laminated glass |
JP3898378B2 (ja) * | 1998-11-13 | 2007-03-28 | 積水化学工業株式会社 | 合わせガラス用中間膜 |
US20040157078A1 (en) * | 2001-01-25 | 2004-08-12 | Takahiro Yoshida | Polyvinyl acetal, polyvinyl acetal composition, ink coating material, dispersant, heat-developable photosensitive material,ceramic green sheet, primer for plastic lens, recording agent for water-based ink and adhesive for metal foil |
EP1483319B1 (en) * | 2002-03-12 | 2007-08-01 | E.I. du Pont de Nemours and Company | Low-color pvb sheet and a process for making same |
DE60302726T2 (de) * | 2002-07-23 | 2006-08-03 | KURARAY CO., LTD, Kurashiki | Polyvinylacetal und dessen Verwendung |
KR100918732B1 (ko) * | 2006-04-25 | 2009-09-24 | 세키스이가가쿠 고교가부시키가이샤 | 합판 유리용 중간막 및 합판 유리 |
KR101333964B1 (ko) * | 2006-10-23 | 2013-11-27 | 가부시키가이샤 구라레 | 아크릴계 열가소성 수지 조성물, 아크릴계 수지 필름, 및 아크릴계 수지 복합체 |
JPWO2008105380A1 (ja) | 2007-02-28 | 2010-06-03 | 株式会社クラレ | フィルム及びそれからなる合わせガラス用中間膜 |
CN101668715A (zh) * | 2007-02-28 | 2010-03-10 | 可乐丽股份有限公司 | 膜及包含该膜的夹层玻璃用中间膜 |
WO2008143195A1 (ja) | 2007-05-17 | 2008-11-27 | Sekisui Chemical Co., Ltd. | ポリビニルアセタール含有樹脂 |
JP5568301B2 (ja) * | 2008-04-22 | 2014-08-06 | 株式会社クラレ | アクリル系熱可塑性樹脂組成物 |
KR101626993B1 (ko) * | 2008-11-13 | 2016-06-03 | 세키스이가가쿠 고교가부시키가이샤 | 폴리비닐아세탈 수지 조성물 |
WO2010074046A1 (ja) | 2008-12-22 | 2010-07-01 | 積水化学工業株式会社 | 合わせガラス用積層体及び合わせガラス用中間膜 |
JP5528156B2 (ja) * | 2010-02-25 | 2014-06-25 | 京セラ株式会社 | セラミックグリーンシートおよびその製造方法 |
-
2014
- 2014-09-30 JP JP2014549238A patent/JP5744345B1/ja active Active
- 2014-09-30 KR KR1020157027034A patent/KR20160065045A/ko not_active Application Discontinuation
- 2014-09-30 CN CN201480031360.6A patent/CN105324345B/zh active Active
- 2014-09-30 WO PCT/JP2014/076142 patent/WO2015046583A1/ja active Application Filing
- 2014-09-30 MX MX2016003514A patent/MX2016003514A/es unknown
- 2014-09-30 RU RU2016116969A patent/RU2646641C2/ru not_active IP Right Cessation
- 2014-09-30 EP EP14848708.5A patent/EP3053890B1/en active Active
- 2014-09-30 US US14/917,510 patent/US11014340B2/en active Active
-
2015
- 2015-04-28 JP JP2015091278A patent/JP2015187075A/ja active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH07118347A (ja) * | 1993-10-22 | 1995-05-09 | Sekisui Chem Co Ltd | 遮音性中間膜 |
JP2000272936A (ja) * | 1999-03-25 | 2000-10-03 | Sekisui Chem Co Ltd | 合わせガラス用中間膜及び合わせガラス |
JP2007070200A (ja) | 2005-09-09 | 2007-03-22 | Asahi Glass Co Ltd | 合わせガラス |
JP2007297571A (ja) * | 2006-05-08 | 2007-11-15 | Sekisui Chem Co Ltd | 透明積層体用中間膜及び透明積層体 |
WO2012026393A1 (ja) * | 2010-08-23 | 2012-03-01 | 株式会社クラレ | 太陽電池用封止材および合わせガラス用中間膜 |
JP2014224234A (ja) * | 2013-04-26 | 2014-12-04 | 積水化学工業株式会社 | ポリビニルアセタール系樹脂組成物 |
Non-Patent Citations (1)
Title |
---|
See also references of EP3053890A4 |
Cited By (25)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2015125932A1 (ja) * | 2014-02-20 | 2015-08-27 | 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 |
US11274200B2 (en) | 2014-02-20 | 2022-03-15 | Sekisui Chemical Co., Ltd. | Interlayer for laminated glass, and laminated glass |
WO2016052671A1 (ja) * | 2014-09-30 | 2016-04-07 | 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 |
WO2016052670A1 (ja) * | 2014-09-30 | 2016-04-07 | 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 |
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 |
JPWO2016052671A1 (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 |
WO2016158694A1 (ja) * | 2015-03-31 | 2016-10-06 | 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 |
JPWO2016158694A1 (ja) * | 2015-03-31 | 2017-04-27 | 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 |
US10711128B2 (en) | 2015-09-30 | 2020-07-14 | Sekisui Chemical Co., Ltd. | Modified polyvinyl acetal resin composition |
EP3357990A4 (en) * | 2015-09-30 | 2019-05-08 | Sekisui Chemical Co., Ltd. | ADHESIVE |
WO2018181755A1 (ja) * | 2017-03-31 | 2018-10-04 | 積水化学工業株式会社 | 成形体及び合わせガラス |
JPWO2018181755A1 (ja) * | 2017-03-31 | 2020-02-06 | 積水化学工業株式会社 | 成形体及び合わせガラス |
WO2018181754A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181758A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181747A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
JP7036716B2 (ja) | 2017-03-31 | 2022-03-15 | 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 |
JPWO2018181754A1 (ja) * | 2017-03-31 | 2020-02-06 | 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 |
WO2018181757A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
JPWO2018181758A1 (ja) * | 2017-03-31 | 2020-02-06 | 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 |
JPWO2018181757A1 (ja) * | 2017-03-31 | 2020-02-06 | 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 |
JPWO2018181751A1 (ja) * | 2017-03-31 | 2020-02-06 | 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 |
JPWO2018181748A1 (ja) * | 2017-03-31 | 2020-02-06 | 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 |
WO2018181751A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
WO2018181748A1 (ja) * | 2017-03-31 | 2018-10-04 | 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 |
JP2019147705A (ja) * | 2018-02-27 | 2019-09-05 | 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 |
Also Published As
Publication number | Publication date |
---|---|
KR20160065045A (ko) | 2016-06-08 |
CN105324345B (zh) | 2017-11-21 |
EP3053890A4 (en) | 2017-07-05 |
CN105324345A (zh) | 2016-02-10 |
JP2015187075A (ja) | 2015-10-29 |
RU2646641C2 (ru) | 2018-03-06 |
JPWO2015046583A1 (ja) | 2017-03-09 |
EP3053890B1 (en) | 2018-03-07 |
MX2016003514A (es) | 2016-06-28 |
EP3053890A1 (en) | 2016-08-10 |
US11014340B2 (en) | 2021-05-25 |
RU2016116969A (ru) | 2017-11-10 |
US20160214355A1 (en) | 2016-07-28 |
JP5744345B1 (ja) | 2015-07-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP5744345B1 (ja) | 合わせガラス用中間膜及び合わせガラス | |
JP6609277B2 (ja) | 積層体及び合わせガラス | |
JP4751966B1 (ja) | 合わせガラス用中間膜及び合わせガラス | |
JP2016172684A (ja) | 合わせガラス用中間膜及び合わせガラス | |
JPWO2012008582A1 (ja) | 合わせガラス用中間膜及び合わせガラス | |
WO2010008053A1 (ja) | 合わせガラス用中間膜 | |
JPH05104687A (ja) | 遮音性中間膜 | |
WO2017171043A1 (ja) | 合わせガラス用中間膜及び合わせガラス | |
JP2003252655A (ja) | 合わせガラス用中間膜及び合わせガラス | |
JP2003252656A (ja) | 合わせガラス用中間膜及び合わせガラス | |
JP2003252657A (ja) | 合わせガラス用中間膜及び合わせガラス | |
JP6833578B2 (ja) | 合わせガラス用中間膜および合わせガラス | |
JPWO2017171042A1 (ja) | ポリビニルアセタールアイオノマー樹脂フィルム及び合わせガラス | |
JP7028769B2 (ja) | 合わせガラス用中間膜及び合わせガラス | |
CN108779210A (zh) | 聚乙烯醇缩醛离聚物树脂材料、聚乙烯醇缩醛离聚物树脂膜以及夹层玻璃 | |
JP6974212B2 (ja) | 合わせガラス用中間膜及び合わせガラス | |
WO2020031558A1 (ja) | 合わせガラス用中間膜及び合わせガラス | |
WO2020250906A1 (ja) | 樹脂組成物、樹脂フィルム、及びガラス積層体 | |
CN113454041A (zh) | 夹层玻璃用中间膜和夹层玻璃 | |
JP2018138504A (ja) | 合わせガラス用中間膜、及び合わせガラス | |
EP3901113A1 (en) | Interlayer film for laminated glass, and laminated glass | |
WO2022112045A1 (en) | Interlayer films for use in laminated glass and laminated glass | |
JP2018138503A (ja) | 合わせガラス用中間膜、及び合わせガラス | |
JP2023548404A (ja) | 改善された音響特性を有する複層中間膜 | |
JP2010042982A (ja) | 合わせガラス用中間膜、及び、合わせガラス |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 201480031360.6 Country of ref document: CN |
|
ENP | Entry into the national phase |
Ref document number: 2014549238 Country of ref document: JP Kind code of ref document: A |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 14848708 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 20157027034 Country of ref document: KR Kind code of ref document: A |
|
REEP | Request for entry into the european phase |
Ref document number: 2014848708 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 2014848708 Country of ref document: EP |
|
WWE | Wipo information: entry into national phase |
Ref document number: 14917510 Country of ref document: US |
|
WWE | Wipo information: entry into national phase |
Ref document number: MX/A/2016/003514 Country of ref document: MX |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
ENP | Entry into the national phase |
Ref document number: 2016116969 Country of ref document: RU Kind code of ref document: A |