WO2020189335A1 - 合わせガラス中間膜用樹脂組成物、合わせガラス中間膜および合わせガラス - Google Patents
合わせガラス中間膜用樹脂組成物、合わせガラス中間膜および合わせガラス Download PDFInfo
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- WO2020189335A1 WO2020189335A1 PCT/JP2020/009651 JP2020009651W WO2020189335A1 WO 2020189335 A1 WO2020189335 A1 WO 2020189335A1 JP 2020009651 W JP2020009651 W JP 2020009651W WO 2020189335 A1 WO2020189335 A1 WO 2020189335A1
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- laminated glass
- interlayer film
- glass interlayer
- resin composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B32B17/10614—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 comprising particles for purposes other than dyeing
- B32B17/10623—Whitening agents reflecting visible light
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- 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
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- 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
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- 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
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- B32B17/10614—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 comprising particles for purposes other than dyeing
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- 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
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- B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
- B32B17/10816—Making laminated safety glass or glazing; Apparatus therefor by pressing
- B32B17/10871—Making laminated safety glass or glazing; Apparatus therefor by pressing in combination with particular heat treatment
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- B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
- B32B17/10899—Making laminated safety glass or glazing; Apparatus therefor by introducing interlayers of synthetic resin
- B32B17/10935—Making laminated safety glass or glazing; Apparatus therefor by introducing interlayers of synthetic resin as a preformed layer, e.g. formed by extrusion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Definitions
- the present invention relates to a resin composition for a laminated glass interlayer film, a laminated glass interlayer film and a laminated glass.
- laminated glass As a laminated glass with enhanced design, a laminated glass exhibiting a milky white color is known.
- Examples of the technique related to such laminated glass include those described in Patent Document 1 in which alumina trihydrate, alumina, or the like is used as a pigment.
- the technical level required for laminated glass is becoming higher and higher.
- the present inventors have found the following problems with respect to laminated glass. It has become clear that it is difficult to achieve both improvement in optical properties and improvement in adhesiveness to glass in a resin composition containing a pigment having a particle size and type as described in Patent Document 1. ..
- the present invention has been made in view of the above problems, and an object of the present invention is to provide a resin composition for a laminated glass interlayer film having improved optical properties and adhesiveness to glass.
- the present invention is a resin composition for a laminated glass interlayer film used for forming a laminated glass interlayer film.
- Ionomer (A) an ethylene / unsaturated carboxylic acid copolymer, Inorganic filler (B) and Including
- a resin composition for a laminated glass interlayer film wherein the volume-based cumulative 10% diameter (D 10 ) of the inorganic filler (B) measured by a laser diffraction / scattering method is 0.1 ⁇ m or more and 10 ⁇ m or less.
- D 10 volume-based cumulative 10% diameter of the inorganic filler measured by a laser diffraction / scattering method
- a laminated glass interlayer film composed of the above-mentioned resin composition for a laminated glass interlayer film.
- a laminated glass provided with the above-mentioned laminated glass interlayer film and transparent plate-shaped members provided on both sides of the laminated glass interlayer film.
- the resin composition for a laminated glass interlayer film according to the embodiment is a resin composition for a laminated glass interlayer film used for forming a laminated glass interlayer film.
- the resin composition for a laminated glass interlayer film contains an ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) and an inorganic filler (B).
- A ethylene / unsaturated carboxylic acid-based copolymer ionomer
- B inorganic filler
- the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer according to the present embodiment has at least a part of the carboxyl group of the polymer obtained by copolymerizing ethylene and at least one of the unsaturated carboxylic acids. It is a resin neutralized with metal ions.
- a copolymer containing ethylene and an unsaturated carboxylic acid can be exemplified.
- the unsaturated carboxylic acid in the ethylene / unsaturated carboxylic acid-based copolymer examples include acrylic acid, methacrylic acid, 2-ethylacrylic acid, crotonic acid, maleic acid, fumaric acid, itaconic acid, maleic anhydride, and fumaric anhydride. Examples thereof include acid, itaconic anhydride, monomethyl maleate, and monoethyl maleate.
- the unsaturated carboxylic acid is preferably at least one selected from acrylic acid and methacrylic acid from the viewpoint of productivity, hygiene and the like of the ethylene / unsaturated carboxylic acid copolymer. These unsaturated carboxylic acids may be used alone or in combination of two or more.
- a particularly preferable ethylene / unsaturated carboxylic acid-based copolymer is an ethylene / (meth) acrylic acid copolymer.
- ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) when the total structural unit constituting the ethylene / unsaturated carboxylic acid-based copolymer is 100% by mass, it is derived from ethylene.
- the structural unit to be used is preferably 65% by mass or more and 95% by mass or less, and more preferably 75% by mass or more and 92% by mass or less.
- the structural unit derived from ethylene is at least the above lower limit value, the heat resistance, mechanical strength, water resistance, processability, etc.
- the structural unit derived from ethylene when the total structural unit constituting the ethylene / unsaturated carboxylic acid-based copolymer is 100% by mass, the unsaturated carboxylic acid
- the structural unit derived from the acid is preferably 5% by mass or more and 35% by mass or less, and more preferably 8% by mass or more and 25% by mass or less.
- the structural unit derived from the unsaturated carboxylic acid is at least the above lower limit value, the transparency and flexibility of the obtained laminated glass interlayer film, the adhesiveness to the glass, and the like can be further improved. Further, when the structural unit derived from the unsaturated carboxylic acid is not more than the above upper limit value, the heat resistance, mechanical strength, water resistance, processability and the like of the obtained laminated glass interlayer film can be further improved.
- the ethylene / unsaturated carboxylic acid-based copolymer preferably contains 0% by mass or more and 30% by mass or less when the total structural unit constituting the ethylene / unsaturated carboxylic acid-based copolymer is 100% by mass. More preferably, structural units derived from other copolymerizable monomers of 0% by mass or more and 25% by mass or less may be contained.
- Other copolymerizable monomers include unsaturated esters, for example vinyl esters such as vinyl acetate and vinyl propionate; methyl (meth) acrylate, ethyl (meth) acrylate, isobutyl (meth) acrylate, (meth) acrylic.
- Examples thereof include (meth) acrylic acid esters such as n-butyl acid and 2-ethylhexyl (meth) acrylic acid.
- structural units derived from other copolymerizable monomers are contained in the above range, it is preferable in that the flexibility and transparency of the laminated glass interlayer film obtained by using the resin composition for the laminated glass interlayer film are improved. ..
- Examples of the metal ions constituting the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer include monovalent metal ions such as lithium ion, potassium ion, silver ion, mercury ion and copper ion; calcium ion, magnesium ion, etc. Examples thereof include multivalent metal ions such as zinc ion, aluminum ion, barium ion, beryllium ion, strontium ion, copper ion, cadmium ion, mercury ion, tin ion, lead ion, iron ion, cobalt ion and nickel ion.
- monovalent metal ions such as lithium ion, potassium ion, silver ion, mercury ion and copper ion; calcium ion, magnesium ion, etc.
- Examples thereof include multivalent metal ions such as zinc ion, aluminum ion, barium ion, beryllium ion, strontium
- the upper limit of the degree of neutralization of the ethylene / unsaturated carboxylic acid copolymer (A) according to the present embodiment is the flexibility of the laminated glass interlayer obtained by using the resin composition for the laminated glass interlayer and the glass. From the viewpoint of improving the adhesiveness, mechanical strength, processability, etc., 95% or less is preferable, 90% or less is more preferable, 80% or less is further preferable, 70% or less is further preferable, and 60% or less. Is particularly preferable.
- the lower limit of the degree of neutralization of the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer according to the present embodiment is the transparency of the laminated glass interlayer film obtained by using the resin composition for the laminated glass interlayer film. From the viewpoint of improving heat resistance, water resistance and the like, 5% or more is preferable, 10% or more is more preferable, 15% or more is further preferable, and 20% or more is particularly preferable.
- the degree of neutralization of the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer is neutralized by metal ions among all the carboxyl groups contained in the ethylene / unsaturated carboxylic acid-based copolymer. Refers to the proportion (%) of carboxyl groups.
- the method for producing the ethylene / unsaturated carboxylic acid-based copolymer according to the present embodiment is not particularly limited, and it can be produced by a known method. For example, it can be obtained by radical copolymerizing each polymerization component under high temperature and high pressure. Further, the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer according to the present embodiment can be obtained by reacting the ethylene / unsaturated carboxylic acid-based copolymer with a metal compound. Further, as the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer, a commercially available one may be used.
- the melt flow rate (JIS K7210-1999) at 190 ° C. and a load of 2160 g is 0.1 to 150 g / g in consideration of processability and mechanical strength. It is preferably 10 minutes, more preferably 0.1 to 50 g / 10 minutes.
- the lower limit of the content of the ethylene / unsaturated carboxylic acid copolymer (A) in the entire resin composition for the laminated glass interlayer film is preferably 75% by mass or more, more preferably 78% by mass or more, and 80% by mass. The above is more preferable.
- the upper limit of the content of the ethylene / unsaturated carboxylic acid copolymer (A) in the entire resin composition for the laminated glass interlayer is preferably 99% by mass or less, more preferably 98% by mass or less, and 95% by mass. The following is more preferable, 90% by mass or less is particularly preferable, and 87% by mass or less is most preferable.
- the adhesiveness to glass, water resistance, and rigidity can be sufficiently improved.
- the content of ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer is set to the above lower limit value or more.
- the optical property, kneadability and film forming property of the resin composition for laminated glass interlayer film are sufficient. Can be.
- Inorganic filler (B) examples of the metal constituting the inorganic filler (B) include one or more selected from calcium, magnesium, zinc, barium, beryllium, strontium, copper, tin, and lead. Of these, calcium, magnesium and barium are preferably used.
- the metal may be contained as an oxide, a carbonate or a sulfate, and the carbonate or the sulfate is more preferable. From the viewpoint of the balance of optical properties, at least one selected from calcium carbonate, barium carbonate, barium sulfate, magnesium sulfate, magnesium oxide, and magnesium hydroxide is preferable, and calcium carbonate is particularly preferable.
- the lower limit of the volume-based cumulative 10% diameter (D 10 ) of the inorganic filler (B) measured by the laser diffraction / scattering method is 0.1 ⁇ m or more, preferably 0.5 ⁇ m or more, and more preferably 1 ⁇ m or more.
- the upper limit of the volume-based cumulative 10% diameter (D 10 ) of the inorganic filler (B) is 10 ⁇ m or less, preferably 7 ⁇ m or less, and more preferably 5 ⁇ m or less.
- the total light transmittance of the laminated glass obtained by using the resin composition for the laminated glass interlayer film is increased, and the blinding property of the laminated glass is improved. It can be in an appropriate range.
- the surface of the inorganic filler (B) may be coated.
- the surface of the inorganic filler (B) may be coated with at least one treatment agent selected from the group consisting of. According to this, the dispersibility of the inorganic filler (B) in the ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer during the molding process is improved, and a uniform milky white appearance is obtained and the laminated glass is laminated.
- the film forming property of the resin composition for an interlayer film can be further improved.
- the lower limit of the content of the inorganic filler (B) with respect to the entire resin composition for the laminated glass interlayer film is preferably 1% by mass or more, more preferably 2% by mass or more, further preferably 5% by mass or more, and 10% by mass or more. It is particularly preferable, and 13% by mass or more is most preferable.
- the upper limit of the content of the inorganic filler (B) in the entire resin composition for the laminated glass interlayer film is preferably 25% by mass or less, more preferably 22% by mass or less, still more preferably 20% by mass or less.
- the content of the inorganic filler (B) By setting the content of the inorganic filler (B) to the above lower limit value or more, the haze of the laminated glass obtained by using the resin composition for a laminated glass interlayer film can be increased, and the appearance of the laminated glass can be made milky white. it can.
- the content of the inorganic filler (B) By setting the content of the inorganic filler (B) to the above upper limit or less, the total light transmittance of the laminated glass obtained by using the resin composition for a laminated glass interlayer film is increased, and the transparency of the laminated glass is appropriately adjusted. Can be a range.
- the resin composition for a laminated glass interlayer film according to the present embodiment preferably further contains a silane coupling agent.
- a silane coupling agent By including a silane coupling agent, the film forming property can be improved.
- the silane coupling agent include silane coupling agents such as alkoxysilane having an amino group, a glycidyl group or an epoxy group.
- ⁇ -glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 3-glycidoxypropylmethyldiethoxysilane, N-2 (aminoethyl) 3-aminopropyltrimethoxy Silane, N-2 (aminoethyl) 3-aminopropylmethyldiethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, N-phenyl-3-aminoppiltrimethoxysilane and N-phenyl -3-Aminopropyltriethoxysilane and the like can be mentioned.
- silane coupling agents may be used alone or in combination of two or more.
- amino group, glycidyl group or epoxy group are used from the viewpoint of further improving the performance balance of the optical characteristics, water resistance and adhesiveness to the glass of the obtained laminated glass and stabilizing the film forming property during sheet processing.
- a silane coupling agent having an amino group is preferable, and a silane coupling agent having an amino group is more preferable.
- the content of the silane coupling agent is from the viewpoint of further improving the performance balance of the optical characteristics, water resistance and adhesiveness to the obtained laminated glass.
- the total amount of the resin composition for the laminated glass interlayer is 100% by mass, it is preferably 0.001% by mass or more and 5% by mass or less, more preferably 0.005% by mass or more and 2% by mass or less, and further preferably 0. It is 0.01% by mass or more and 1% by mass or less.
- the resin composition for a laminated glass interlayer film according to the present embodiment may contain various additives as long as the object of the present invention is not impaired.
- the various additives are not particularly limited, but for example, plasticizers, antioxidants, ultraviolet absorbers, wavelength converters, antistatic agents, surfactants, colorants, light stabilizers, foaming agents, lubricants, crystal nuclei.
- thermoplastic resins other than ionomer (A) of ethylene / unsaturated carboxylic acid copolymers heat Curable resin, inorganic filler, organic filler, impact resistance improver, slip agent, cross-linking agent, cross-linking aid, tackifier, processing aid, mold release agent, hydrolysis inhibitor, heat stabilizer, anti Examples thereof include blocking agents, antifogging agents, flame retardants, flame retardant aids, light diffusing agents, antibacterial agents, anticorrosive agents, dispersants and other resins.
- the various additives may be used alone or in combination of two or more.
- the resin composition for a laminated glass interlayer film of the present embodiment has a haze of 80% or more measured by the following method from the viewpoint of making the appearance of the laminated glass milky white and setting the transparency in an appropriate range, and the total light beam.
- the transmittance is preferably 50% or more and less than 80%, the haze is 90% or more, the total light transmittance is more preferably 50% or more and less than 80%, and the haze is 90% or more and all. It is more preferable that the light transmittance is 60% or more and less than 70%.
- the obtained glass interlayer film was sandwiched between two glass plates of 120 mm ⁇ 75 mm ⁇ 3.2 mm, vacuum-held at 140 ° C. for 5 minutes with a vacuum laminator, and then at 0.1 MPa (gauge pressure) 3 Press for minutes to obtain a laminated glass.
- the haze and total light transmittance of the obtained laminated glass are measured by a haze meter according to JIS K7136: 2000.
- the adhesive strength to the glass plate measured by the following method is preferably 14 N / 15 mm or more, and more preferably 20 N / 15 mm or more.
- the adhesive strength to the glass plate is at least the above lower limit value, the interlayer adhesiveness of the obtained laminated glass can be further improved.
- the content and type of the silane coupling agent to be used may be appropriately adjusted.
- the obtained laminated glass interlayer film was laminated on the non-tin surface of a glass plate of 120 mm ⁇ 75 mm ⁇ 3.9 mm, vacuum-held at 140 ° C. for 3 minutes with a vacuum laminator, and then 0.1 MPa (gauge pressure). )
- the laminated glass interlayer film is pulled away from the glass plate at an angle of 180 ° at a tensile speed of 100 mm / min, and the maximum stress is calculated as the adhesive strength (N / 15 mm) to the glass plate.
- the appearance of the laminated glass in which the resin composition for laminated glass interlayer film is used as the laminated glass interlayer film is made milky white, the optical characteristics of the laminated glass are improved, and the glass It is possible to achieve both improvement of adhesiveness to the board.
- the laminated glass interlayer film according to the present embodiment is composed of a resin composition for a laminated glass interlayer film according to the present embodiment.
- the laminated glass interlayer film can be formed by a known method using a T-die extruder, a calendar forming machine, an inflation forming machine or the like.
- the masterbatch may contain an ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) and a dispersant.
- the ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) used in the masterbatch is the same as or different from the component of the ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) added separately from the masterbatch. May be.
- the total amount of the ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) used in the master batch and the ethylene / unsaturated carboxylic acid-based copolymer ionomer (A) added separately from the master batch is preferably in the range of the content of ionomer (A) of the ethylene / unsaturated carboxylic acid-based copolymer with respect to the entire resin composition for the laminated glass interlayer film described above.
- the content of the masterbatch in the entire resin composition for the laminated glass interlayer film is not particularly limited, but by setting it to 10% by mass or more and 30% by mass or less, the kneadability of the resin composition for the laminated glass interlayer film can be improved. Extrudability can be improved.
- the dispersant include a polyether-based dispersant.
- the thickness of the laminated glass interlayer film is not particularly limited, but is usually about 0.05 to 1.2 mm.
- the laminated glass according to the present embodiment includes two transparent plate-shaped members and a laminated glass interlayer film according to the present embodiment arranged between the two transparent plate-shaped members.
- the laminated glass according to the present embodiment is excellent in optical characteristics and adhesiveness between the transparent plate-shaped member and the laminated glass interlayer film by providing the laminated glass interlayer film according to the present embodiment.
- Examples of the structure of the laminated glass include a structure of a transparent plate-shaped member / a laminated glass interlayer film / a transparent plate-shaped member. Two or more layers of the laminated glass interlayer film may be used, or a layer made of another resin may be sandwiched between two laminated glass interlayer films to form three or more layers.
- the transparent plate-shaped member is not particularly limited, but for example, a commonly used transparent plate glass can be used, for example, a float plate glass, a polished plate glass, a template glass, a meshed plate glass, a lined plate glass, a colored plate glass, and the like.
- examples thereof include inorganic glass such as heat ray absorbing plate glass, heat ray reflecting plate glass, and green glass. It is also possible to use organic plastic plates such as polycarbonate plates, poly (meth) acrylate plates, polymethyl (meth) acrylate plates, polystyrene plates, cyclic polyolefin plates, polyethylene terephthalate plates, polyethylene naphthalate plates, and polyethylene butyrate plates. it can.
- the transparent plate-shaped member may be appropriately subjected to surface treatment such as corona treatment, plasma treatment, and frame treatment.
- the thickness of the transparent plate-shaped member is not particularly limited, but is usually 20 mm or less, preferably 10 mm or less. Although the lower limit of the thickness of the transparent plate-shaped member is not limited, it is usually 0.1 mm or more, preferably 0.5 mm or more.
- the same transparent plate-shaped members may be used on both sides of the laminated glass interlayer film, or different plate-shaped members may be used in combination.
- the method for producing the laminated glass according to the present embodiment is not particularly limited, and for example, conventionally known production methods such as a nip roll method, an autoclave method, a vacuum bag method, and a vacuum laminator method can be used. One of these methods may be used for production, or two or more types of production methods may be combined for production.
- a method for producing a laminated glass according to the present embodiment for example, the laminated glass interlayer film is placed between two sheets of glass and thermocompression bonded under heating and pressure.
- the heating temperature is preferably about 100 ° C. to 250 ° C.
- the pressure is preferably about 10 kPa to 3 MPa (0.1 kg / cm 2 to 30 kg / cm 2 ).
- These laminated glasses can be used for various purposes, for example, they are used for architectural laminated glass, automobile laminated glass, general buildings, agricultural buildings, railway windows, etc., and these uses It is not limited to.
- Ionomer 2 Ethylene / methacrylic acid copolymer ionomer (ethylene content 91% by mass, methacrylic acid content: 9% by mass, metal ion: zinc ion, neutralization degree: 18%, MFR (JIS K7210: 1999 compliant) Then, measured under the condition of 190 ° C.
- Ionomer 3 Ethylene / methacrylic acid copolymer ionomer (ethylene content 80% by mass, methacrylic acid content: 20% by mass, metal ion: magnesium ion, neutralization degree: 40%, MFR (JIS K7210: 1999 compliant) Then, measured under the condition of 190 ° C.
- Ionomer 4 Ethylene / methacrylic acid copolymer ionomer (ethylene content 80% by mass, methacrylic acid content: 20% by mass, metal ion: zinc ion, neutralization degree: 40%, MFR (JIS K7210: 1999 compliant) (Measured under the condition of 190 ° C. and 2160 g load): 1.6 g / 10 minutes)
- White pigment resin A Calcium carbonate obtained by surface-treating ionomer 1 (50 parts by mass) with a polyether-based dispersant (volume-based cumulative 10% diameter (D 10 ) 5.0 ⁇ m measured by laser diffraction / scattering method)
- a white pigment resin A was obtained by melt-kneading at 160 ° C. with a twin-screw extruder together with 50 parts by mass.
- White pigment resin B Barium sulfate (volume standard cumulative 10% diameter (D 10 ) 180 nm measured by laser diffraction / scattering method) 50 mass, which is surface-treated with a polyether-based dispersant with respect to ionomer 1 (50 parts by mass).
- a white pigment resin B was obtained by melt-kneading together with the portion at 160 ° C. using a twin-screw extruder.
- White pigment resin C Titanium oxide (volume standard cumulative 10% diameter (D 10 ) 50 nm measured by laser diffraction / scattering method) 50 mass, which is surface-treated with a polyether-based dispersant with respect to ionomer 1 (50 parts by mass).
- a white pigment resin C was obtained by melt-kneading together with the portion at 160 ° C. with a twin-screw extruder.
- Si-C Silane coupling agent having an amino group (N- (2-aminoethyl) -aminopropylmethyldimethoxysilane, KBM-602, manufactured by Shin-Etsu Chemical Co., Ltd.)
- Examples 1 to 10 and Comparative Examples 1 and 2 Ionomer, a white pigment resin, and a silane coupling agent, which are ethylene / unsaturated carboxylic acid-based copolymers, were melt-kneaded at 160 ° C. in the blending ratios shown in Table 1 to obtain a resin composition for a laminated glass interlayer film.
- the resin composition for a laminated glass interlayer film was extruded into an extrusion sheet under the conditions of a die outlet resin temperature of 160 ° C. and a processing speed of 5 m / min to obtain a laminated glass interlayer film having a thickness of 0.4 mm.
- the resin compositions for laminated glass interlayer films of Examples 1 to 10 and Comparative Examples 1 and 2 had no problem in the moldability of the laminated glass interlayer film (sheet) (Table 1 shows that the sheet moldability was ⁇ (good)).
- the white pigment resins A, B, and C are master batches containing the ionomer 1 and the inorganic filler (B) as described above.
- Example 1 95 parts by mass of the ionomer 1 is used.
- Example 10 includes 80 parts by mass of ionomer 3 and 10 parts by mass of ionomer 1.
- the laminated glass interlayer film composed of the resin composition for the laminated glass interlayer film obtained in Examples and Comparative Examples was cut into a size of 120 mm ⁇ 75 mm ⁇ thickness 0.4 mm.
- the obtained laminated glass interlayer film was sandwiched between two glass plates (manufactured by Asahi Glass Co., Ltd., product name: float plate glass) of 120 mm ⁇ 75 mm ⁇ 3.2 mm, and vacuum-held at 140 ° C. for 5 minutes with a vacuum laminator. Then, it was pressed at 0.1 MPa (gauge pressure) for 3 minutes to obtain a laminated glass.
- the obtained laminated glass was cooled by slow cooling so as to return to room temperature over 30 minutes.
- the haze and total light transmittance of the obtained laminated glass were measured by a haze meter (manufactured by Murakami Color Co., Ltd., product name: haze meter HM150) according to JIS K7136: 2000.
- the haze evaluation results were classified based on the obtained haze value and the following evaluation criteria.
- the evaluation results of the total light transmittance were classified based on the obtained total light transmittance value and the following evaluation criteria.
- the laminated glass interlayer film composed of the resin compositions for each laminated glass interlayer film obtained in Examples and Comparative Examples was cut into a size of 120 mm ⁇ 75 mm ⁇ 0.4 mm.
- the obtained laminated glass interlayer film was laminated on the non-tin surface of a glass plate (manufactured by Asahi Glass Co., Ltd., product name: blue plate glass) of 120 mm ⁇ 75 mm ⁇ 3.9 mm, and used in a vacuum laminator at 140 ° C. for 3 minutes. After holding in a vacuum, the glass was pressed at 0.1 MPa (gauge pressure) for 30 minutes to adhere the laminated glass interlayer film to the non-tin surface of the glass plate.
- a glass plate manufactured by Asahi Glass Co., Ltd., product name: blue plate glass
- the obtained sample was held at 85 ° C. and 90% humidity for 500 hours, and then the sample was cooled to room temperature, and then the laminated glass interlayer film was applied to the glass plate at room temperature (25 ° C.) at a tensile speed of 100 mm / min.
- the maximum stress was calculated as the adhesive strength (N / 15 mm) to the glass plate.
- the adhesiveness of the laminated glass interlayer film to the glass plate was evaluated according to the following criteria.
- the resin compositions for laminated glass interlayer films of Examples 1 to 10 have excellent or good haze and total light transmittance, and have good sheet formability (denoted as ⁇ in Table 1). There was, and the glass adhesiveness was excellent or good. On the other hand, the resin compositions for laminated glass interlayer films of Comparative Examples 1 and 2 had poor haze and total light transmittance, respectively.
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Abstract
Description
特許文献1に記載されているような粒径および種類の顔料を含む樹脂組成物では、光学特性の向上と、ガラスに対する接着性の向上とを両立させることが困難であることが明らかになった。
本発明は上述のような課題を鑑みたものであり、光学特性およびガラスに対する接着性が向上した合わせガラス中間膜用樹脂組成物を提供することを目的とする。
エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)と、
無機フィラー(B)と、
を含み、
レーザー回折散乱法により測定される前記無機フィラー(B)の体積基準累積10%径(D10)が0.1μm以上10μm以下である、合わせガラス中間膜用樹脂組成物が提供される。
また、本発明によれば、上述した合わせガラス中間膜用樹脂組成物により構成された合わせガラス中間膜が提供される。
また、本発明によれば、上述した合わせガラス中間膜と、前記合わせガラス中間膜の両面に設けられた透明板状部材と、を備える合わせガラスが提供される。
本実施形態に係るエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)は、エチレンと、不飽和カルボン酸の少なくとも1種とを共重合した重合体に対し、カルボキシル基の少なくとも一部を金属イオンで中和した樹脂である。エチレン・不飽和カルボン酸系共重合体としては、エチレンと不飽和カルボン酸とを含む共重合体を例示することができる。
エチレン・不飽和カルボン酸系共重合体における不飽和カルボン酸としては、例えば、アクリル酸、メタクリル酸、2-エチルアクリル酸、クロトン酸、マレイン酸、フマル酸、イタコン酸、無水マレイン酸、無水フマル酸、無水イタコン酸、マレイン酸モノメチル、マレイン酸モノエチル等が挙げられる。これらの中でも、上記不飽和カルボン酸としては、エチレン・不飽和カルボン酸系共重合体の生産性、衛生性等の観点から、アクリル酸およびメタクリル酸から選ばれる少なくとも1種であることが好ましい。これらの不飽和カルボン酸は1種単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
本実施形態において、特に好ましいエチレン・不飽和カルボン酸系共重合体は、エチレン・(メタ)アクリル酸共重合体である。
本実施形態に係るエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)において、エチレン・不飽和カルボン酸系共重合体を構成する構造単位の全体を100質量%としたとき、エチレンに由来する構造単位は、好ましくは65質量%以上95質量%以下、より好ましくは75質量%以上92質量%以下である。
エチレンに由来する構造単位が上記下限値以上であると、得られる合わせガラス中間膜の耐熱性や機械的強度、耐水性、加工性等をより良好にすることができる。また、エチレンに由来する構造単位が上記上限値以下であると、得られる合わせガラス中間膜の透明性や柔軟性、ガラスに対する接着性等をより良好にすることができる。
本実施形態に係るエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)において、エチレン・不飽和カルボン酸系共重合体を構成する構造単位の全体を100質量%としたとき、不飽和カルボン酸に由来する構造単位は、好ましくは5質量%以上35質量%以下、より好ましくは8質量%以上25質量%以下である。
不飽和カルボン酸に由来する構造単位が上記下限値以上であると、得られる合わせガラス中間膜の透明性や柔軟性、ガラスに対する接着性等をより良好にすることができる。また、不飽和カルボン酸に由来する構造単位が上記上限値以下であると、得られる合わせガラス中間膜の耐熱性や機械的強度、耐水性、加工性等をより良好にすることができる。
これらの中でもリチウムイオン、カリウムイオン、カルシウムイオン、マグネシウムイオン、亜鉛イオン、アルミニウムイオン、およびバリウムイオンから選択される1種または2種以上を含むことが好ましく、カリウムイオン、亜鉛イオンおよびマグネシウムイオンから選択される少なくとも1種を含むことがより好ましく、マグネシウムイオンおよび亜鉛イオンから選択される少なくとも1種を含むことが特に好ましい。
なお、上述した金属イオンでエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)を構成することにより、金属イオンとしてナトリウムイオンを用いた場合に比べて、合わせガラス中間膜の成膜時に発泡やゲル化が生じにくく、製造安定性を高めることができる。
また、本実施形態に係るエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の中和度の下限は、合わせガラス中間膜用樹脂組成物を用いて得られる合わせガラス中間膜の透明性や耐熱性、耐水性等をより良好にする観点から、5%以上が好ましく、10%以上がより好ましく、15%以上がさらに好ましく、20%以上が特に好ましい。
ここで、エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の中和度は、エチレン・不飽和カルボン酸系共重合体中に含まれる全カルボキシル基のうち、金属イオンによって中和されているカルボキシル基の割合(%)を指す。
合わせガラス中間膜用樹脂組成物全体に対するエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の含有率の上限は、99質量%以下が好ましく、98質量%以下がより好ましく、95質量%以下がさらに好ましく、90質量%以下が特に好ましく、87質量%以下が最も好ましい。
エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の含有率を上記下限値以上とすることにより、ガラスに対する接着性および耐水性、剛性を十分に高めることができる。
エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の含有率を上記上限値以下とすることにより、合わせガラス中間膜用樹脂組成物の光学性、混錬性や成膜性を十分なものとすることができる。
無機フィラー(B)を構成する金属として、カルシウム、マグネシウム、亜鉛、バリウム、ベリリウム、ストロンチウム、銅、錫、および鉛から選択される1種以上が挙げられる。これらの中で、カルシウム、マグネシウムおよびバリウムが好ましく用いられる。
上記金属は、酸化物、炭酸塩、硫酸塩として含まれていてもよく、炭酸塩、硫酸塩がより好ましい。光学特性のバランスの観点から、炭酸カルシウム、炭酸バリウム、硫酸バリウム、硫酸マグネシウム、酸化マグネシウム、および水酸化マグネシウムから選ばれる少なくとも1種が好ましく、炭酸カルシウムが特に好ましい。
レーザー回折散乱法により測定される無機フィラー(B)の体積基準累積10%径(D10)の下限は、0.1μm以上であり、0.5μm以上が好ましく、1μm以上がより好ましい。無機フィラー(B)の体積基準累積10%径(D10)の上限は、10μm以下であり、7μm以下が好ましく、5μm以下がより好ましい。
無機フィラー(B)のD10を上記下限値以上とすることにより、合わせガラス中間膜用樹脂組成物を用いて得られる合わせガラスのヘイズが増大し、当該合わせガラスの外観を乳白色とすることができる。また、無機フィラー(B)のD10を上記上限値以下とすることにより、合わせガラス中間膜用樹脂組成物を用いて得られる合わせガラスの全光線透過率を高め、当該合わせガラスの目隠し性を適切な範囲とすることができる。
合わせガラス中間膜用樹脂組成物全体に対する無機フィラー(B)の含有率の下限は、1質量%以上が好ましく、2質量%以上がより好ましく、5質量%以上がさらに好ましく、10質量%以上が特に好ましく、13質量%以上が最も好ましい。
合わせガラス中間膜用樹脂組成物全体に対する無機フィラー(B)の含有率の上限は、25質量%以下が好ましく、22質量%以下がより好ましく、20質量%以下がさらに好ましい。
無機フィラー(B)の含有率を上記下限値以上とすることにより、合わせガラス中間膜用樹脂組成物を用いて得られる合わせガラスのヘイズが増大し、当該合わせガラスの外観を乳白色とすることができる。
無機フィラー(B)の含有率を上記上限値以下とすることにより、合わせガラス中間膜用樹脂組成物を用いて得られる合わせガラスの全光線透過率を高め、当該合わせガラスの透明性を適切な範囲とすることができる。
シランカップリング剤としては、アミノ基、グリシジル基またはエポキシ基を有するアルコキシシランなどのシランカップリング剤が挙げられる。より具体的には、γ-グリシドキシプロピルトリメトキシシラン、3-グリシドキシプロピルメチルジメトキシシラン、3-グリシドキシプロピルメチルジエトキシシラン、N-2(アミノエチル)3-アミノプロピルトリメトキシシラン、N-2(アミノエチル)3-アミノプロピルメチルジエトキシシラン、3-アミノプロピルトリメトキシシラン、3-アミノプロピルトリエトキシシラン、N-フェニル-3-アミノプピルトリメトキシシランおよびN-フェニル-3-アミノプロピルトリエトキシシラン等が挙げられる。これらのシランカップリング剤は1種単独で用いてもよいし、2種以上を組み合わせて用いてもよい。
これらの中でも、得られる合わせガラスの光学特性、耐水性およびガラスに対する接着性の性能バランスをより一層良好にし、シート加工時の成膜性を安定させる観点から、アミノ基、グリシジル基またはエポキシ基を有するシランカップリング剤が好ましく、アミノ基を有するシランカップリング剤がより好ましい。
本実施形態に係る合わせガラス中間膜用樹脂組成物において、シランカップリング剤の含有量は、得られる合わせガラスの光学特性、耐水性およびガラスに対する接着性の性能バランスをより一層良好にする観点から、合わせガラス中間膜用樹脂組成物の全体を100質量%としたとき、好ましくは0.001質量%以上5質量%以下、より好ましくは0.005質量%以上2質量%以下、さらに好ましくは0.01質量%以上1質量%以下である。
(ヘイズおよび全光線透過率の評価方法)
本実施形態に係る合わせガラス中間膜用樹脂組成物により構成された120mm×75mm×厚み0.35~0.45mmのガラス中間膜を得る。次いで、得られた上記ガラス中間膜を120mm×75mm×3.2mmの2枚のガラス板で挟み、真空ラミネーターにて140℃、5分間、真空保持したのち、0.1MPa(ゲージ圧)で3分間プレスを行い、合わせガラスを得る。次いで、得られた上記合わせガラスのヘイズおよび全光線透過率をJIS K7136:2000に準じてヘイズメータにより測定する。
このようなガラス板に対する接着強度を達成するためには、本実施形態に係る合わせガラス中間膜用樹脂組成物中のエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)や必要に応じて用いるシランカップリング剤の含有量や種類等を適宜調整すればよい。
(接着強度の評価方法)
本実施形態に係る合わせガラス中間膜用樹脂組成物により構成された120mm×75mm×厚み0.35~0.45mmの合わせガラス中間膜を得る。次いで、得られた上記合わせガラス中間膜を120mm×75mm×3.9mmのガラス板の非スズ面に積層し、真空ラミネーターにて140℃、3分間、真空保持したのち、0.1MPa(ゲージ圧)で30分間プレスを行い、上記合わせガラス中間膜を上記ガラス板の非スズ面に接着させる。次いで、引張速度100mm/分で上記合わせガラス中間膜を上記ガラス板から180°の角度で引き離し、最大応力をガラス板に対する接着強度(N/15mm)として算出する。
合わせガラス中間膜の成形は、T-ダイ押出機、カレンダー成形機、インフレーション成形機などを使用する公知の方法によって行なうことができる。例えば、無機フィラー(B)を含むマスターバッチと、エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)と、必要に応じ、酸化防止剤、光安定剤、紫外線吸収剤及びシランカップリング剤等の添加剤と、を予めドライブレンドして押出機にそのホッパーから供給し、シート状に押出成形することにより得ることができる。
上記マスターバッチは、無機フィラー(B)の他に、エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)および分散剤を含んでもよい。マスターバッチに用いられるエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)は、マスターバッチとは別に加えられるエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の成分と同一でも異なっていてもよい。ただし、マスターバッチに用いられるエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)と、マスターバッチとは別に加えられるエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)との合計量を、上述した合わせガラス中間膜用樹脂組成物全体に対するエチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の含有率の範囲とすることが好ましい。
また、合わせガラス中間膜用樹脂組成物全体に対するマスターバッチの含有率は、特に限定されないが、10質量%以上30質量%以下とすることにより、合わせガラス中間膜用樹脂組成物の混錬性や押出性を良好とすることができる。
分散剤としては、ポリエーテル系分散剤などが挙げられる。
合わせガラス中間膜の厚みは、特に制限されるものではないが、通常は0.05~1.2mm程度である。
本実施形態に係る合わせガラスは、本実施形態に係る合わせガラス中間膜を備えることにより、光学特性及び透明板状部材と合わせガラス中間膜との接着性に優れている。
合わせガラスの構成としては、例えば、透明板状部材/合わせガラス中間膜/透明板状部材の構成が挙げられる。合わせガラス中間膜は2層以上使用してもよく、また他の樹脂からなる層を2枚の合わせガラス中間膜の間に挟んで3層以上としてもよい。
透明板状部材は特に限定されないが、例えば、一般に使用されている透明板ガラスを使用することができ、例えば、フロート板ガラス、磨き板ガラス、型板ガラス、網入り板ガラス、線入り板ガラス、着色された板ガラス、熱線吸収板ガラス、熱線反射板ガラス、グリーンガラス等の無機ガラスが挙げられる。また、ポリカーボネート板、ポリ(メタ)アクリレート板、ポリメチル(メタ)アクリレート板、ポリスチレン板、環式ポリオレフィン板、ポリエチレンテレフタレート板、ポリエチレンナフタレート板、ポリエチレンブチレート板等の有機プラスチックス板を用いることもできる。
また透明板状部材は、コロナ処理、プラズマ処理、フレーム処理等の表面処理を適宜施していてもよい。
透明板状部材の厚みは特に制限がないが、通常は20mm以下、好ましくは10mm以下である。透明板状部材の厚みの下限は制限が無いものの、通常は0.1mm以上、好ましくは0.5mm以上である。本実施形態に係る合わせガラスにおいて、合わせガラス中間膜の両面に設けられるそれぞれの透明板状部材は、同一のものを用いてもよく、異なる板状部材を組み合わせて用いてもよい。
本実施形態に係る合わせガラスの製造方法は特に限定されず、例えば、ニップロール法、オートクレーブ法、真空バッグ法、真空ラミネーター法等の従来公知の製造方法を用いることができる。これらの手法を1種類用いて製造をしてもよいし、2種以上の製造方法を組み合わせて製造することもできる。
本実施形態に係る合わせガラスの製造方法としては、例えば、2枚のシート状のガラスの間に前記合わせガラス中間膜を入れ、加熱及び加圧下で熱圧着することで行うことができる。加熱温度は、例えば、100℃~250℃程度が好ましく、圧力は、例えば、10kPa~3MPa(0.1kg/cm2~30kg/cm2)程度が好ましい。
これらの合わせガラスは、種々の用途に使用することができ、例えば、建築用合わせガラス、自動車用合わせガラス、一般建造物、農業用建造物、鉄道用窓等に使用されるが、これらの用途に限定されるものではない。
合わせガラスの作製に用いた材料の詳細は以下の通りである。
<エチレン・不飽和カルボン酸系共重合体のアイオノマー>
アイオノマー1:エチレン・メタクリル酸共重合体のアイオノマー(エチレン含有量85質量%、メタクリル酸含有量:15質量%、金属イオン:亜鉛イオン、中和度:21%、MFR(JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定):16g/10分)
アイオノマー2:エチレン・メタクリル酸共重合体のアイオノマー(エチレン含有量91質量%、メタクリル酸含有量:9質量%、金属イオン:亜鉛イオン、中和度:18%、MFR(JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定):5.5g/10分)
アイオノマー3:エチレン・メタクリル酸共重合体のアイオノマー(エチレン含有量80質量%、メタクリル酸含有量:20質量%、金属イオン:マグネシウムイオン、中和度:40%、MFR(JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定):2.1g/10分))
アイオノマー4:エチレン・メタクリル酸共重合体のアイオノマー(エチレン含有量80質量%、メタクリル酸含有量:20質量%、金属イオン:亜鉛イオン、中和度:40%、MFR(JIS K7210:1999に準拠し、190℃、2160g荷重の条件で測定):1.6g/10分)
白色顔料樹脂A:アイオノマー1(50質量部)に対し、ポリエーテル系分散剤で表面処理を施した炭酸カルシウム(レーザー回折散乱法により測定した体積基準累積10%径(D10)5.0μm)50質量部とともに2軸押し出し機にて160℃で溶融混錬し、白色顔料樹脂Aを得た。
白色顔料樹脂B:アイオノマー1(50質量部)に対し、ポリエーテル系分散剤で表面処理を施した硫酸バリウム(レーザー回折散乱法により測定した体積基準累積10%径(D10)180nm)50質量部とともに2軸押し出し機にて160℃で溶融混錬し、白色顔料樹脂Bを得た。
白色顔料樹脂C:アイオノマー1(50質量部)に対し、ポリエーテル系分散剤で表面処理を施した酸化チタン(レーザー回折散乱法により測定した体積基準累積10%径(D10)50nm)50質量部とともに2軸押し出し機にて160℃で溶融混錬し、白色顔料樹脂Cを得た。
Si―C:アミノ基を有するシランカップリング剤(N-(2-アミノエチル)-アミノプロピルメチルジメトキシシラン、KBM-602、信越化学工業社製)
表1に示す配合割合で、エチレン・不飽和カルボン酸系共重合体のアイオノマー、白色顔料樹脂およびシランカップリング剤を160℃で溶融混練し、合わせガラス中間膜用樹脂組成物を得た。当該合わせガラス中間膜用樹脂組成物をダイ出口樹脂温度160℃、加工速度5m/分の条件で押出シート成形することにより、厚さ0.4mmの合わせガラス中間膜をそれぞれ得た。
実施例1~10および比較例1、2の合わせガラス中間膜用樹脂組成物は、合わせガラス中間膜(シート)の成形性に問題がなかった(表1に、シート成形性が○(良好)と記載した)。
なお、表1において、白色顔料樹脂A、BおよびCは、上述したように、アイオノマー1と無機フィラー(B)とを含むマスターバッチであり、たとえば、実施例1は、95質量部のアイオノマー1を含み、実施例10は80質量部のアイオノマー3と10質量部のアイオノマー1とを含む。
[光学特性-ヘイズおよび全光線透過率]
実施例および比較例で得られた合わせガラス中間膜用樹脂組成物により構成された合わせガラス中間膜を120mm×75mm×厚み0.4mmのサイズに裁断した。次いで、得られた合わせガラス中間膜を120mm×75mm×3.2mmの2枚のガラス板(旭硝子社製、製品名:フロート板ガラス)で挟み、真空ラミネーターにて140℃、5分間、真空保持したのち、0.1MPa(ゲージ圧)で3分間プレスを行い、合わせガラスを得た。なお、得られた合わせガラスは30分かけて室温に戻るように徐冷にて冷却した。次いで、得られた合わせガラスのヘイズおよび全光線透過率をJIS K7136:2000に準じてヘイズメータ(村上色彩社製、製品名:ヘイズメータHM150)により測定した。得られたヘイズの値および以下の評価基準に基づいて、ヘイズの評価結果を分類した。また、得られた全光線透過率の値および以下の評価基準に基づいて、全光線透過率の評価結果を分類した。
<ヘイズの評価基準>
A(優良):ヘイズが90%以上
B(良好):ヘイズが80%以上90%未満
C(不良):ヘイズが80%未満
<全光線透過率の評価基準>
A(優良):全光線透過率が60%以上70%未満
B(良好):全光線透過率が50%以上60%未満、または70%以上80%未満
C(不良):全光線透過率が50%未満、または80%以上
実施例および比較例で得られた各合わせガラス中間膜用樹脂組成物により構成された合わせガラス中間膜を120mm×75mm×0.4mmのサイズに裁断した。次いで、得られた上記合わせガラス中間膜を120mm×75mm×3.9mmのガラス板(旭硝子社製、製品名:青板ガラス)の非スズ面に積層し、真空ラミネーターにて140℃、3分間、真空保持したのち、0.1MPa(ゲージ圧)で30分間プレスを行い、上記合わせガラス中間膜を上記ガラス板の非スズ面に接着させた。得られたサンプルを85℃、90%湿度下で500時間保持し、次いで、当該サンプルを室温まで冷却後、室温(25℃)にて引張速度100mm/分で上記合わせガラス中間膜を上記ガラス板から180°の角度で引き離し、最大応力をガラス板に対する接着強度(N/15mm)として算出した。次いで、以下の基準により、ガラス板に対する合わせガラス中間膜の接着性を評価した。
<ガラス接着性の評価基準>
A(優良):ガラス板(非スズ面)に対する接着強度が20N/15mm以上
B(良好):ガラス板(非スズ面)に対する接着強度が14N/15mm以上20N/15mm未満
C(不良):ガラス板(非スズ面)に対する接着強度が14N/15mm未満
Claims (9)
- 合わせガラス中間膜を形成するために用いられる合わせガラス中間膜用樹脂組成物であって、
エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)と、
無機フィラー(B)と、
を含み、
レーザー回折散乱法により測定される前記無機フィラー(B)の体積基準累積10%径(D10)が0.1μm以上10μm以下である、合わせガラス中間膜用樹脂組成物。 - 下記方法により測定されるヘイズが80%以上、全光線透過率が50%以上80%未満である請求項1に記載の合わせガラス中間膜用樹脂組成物。
(方法)
上記合わせガラス中間膜用樹脂組成物により構成された120mm×75mm×厚み0.35~0.45mmの合わせガラス中間膜を得る。次いで、得られた上記合わせガラス中間膜を120mm×75mm×3.2mmの2枚のガラス板で挟み、真空ラミネーターにて140℃、5分間、真空保持したのち、0.1MPa(ゲージ圧)で3分間プレスを行い、合わせガラスを得る。次いで、得られた前記合わせガラスのヘイズおよび全光線透過率をJIS K7136:2000に準じてヘイズメータにより測定する。 - 前記無機フィラー(B)を構成する金属が、カルシウム、マグネシウム、亜鉛、バリウム、ベリリウム、ストロンチウム、銅、錫、鉛から選択される1種以上を含む請求項1または2に記載の合わせガラス中間膜用樹脂組成物。
- 前記エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)を構成する金属イオンがリチウムイオン、カリウムイオン、銀イオン、水銀イオン、カルシウムイオン、マグネシウムイオン、亜鉛イオン、アルミニウムイオン、バリウムイオン、ベリリウムイオン、ストロンチウムイオン、銅イオン、カドミウムイオン、錫イオン、鉛イオン、鉄イオン、コバルトイオンおよびニッケルイオンからなる群より選ばれる1種以上である請求項1乃至3のいずれか1項に記載の合わせガラス中間膜用樹脂組成物。
- 前記エチレン・不飽和カルボン酸系共重合体のアイオノマー(A)の中和度が5%以上95%以下である請求項1乃至4のいずれか1項に記載の合わせガラス中間膜用樹脂組成物。
- シランカップリング剤をさらに含む請求項1乃至5のいずれか1項に記載の合わせガラス中間膜用樹脂組成物。
- 前記シランカップリング剤がアミノ基、グリシジル基またはエポキシ基を有するアルコキシシランである請求項6に記載の合わせガラス中間膜用樹脂組成物。
- 請求項1乃至7いずれか1項に記載の合わせガラス中間膜用樹脂組成物により構成された合わせガラス中間膜。
- 請求項8に記載の合わせガラス中間膜と、
前記合わせガラス中間膜の両面に設けられた透明板状部材と、
を備える合わせガラス。
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JP2021507205A JP7133084B2 (ja) | 2019-03-20 | 2020-03-06 | 合わせガラス中間膜用樹脂組成物、合わせガラス中間膜および合わせガラス |
CN202080022457.6A CN113597415B (zh) | 2019-03-20 | 2020-03-06 | 夹层玻璃中间膜用树脂组合物、夹层玻璃中间膜及夹层玻璃 |
KR1020217033381A KR102618416B1 (ko) | 2019-03-20 | 2020-03-06 | 접합 유리 중간막용 수지 조성물, 접합 유리 중간막 및 접합 유리 |
EP20774824.5A EP3943463A4 (en) | 2019-03-20 | 2020-03-06 | RESIN COMPOSITION FOR LAMINATED GLASS INTERLAYER, LAMINATED GLASS INTERLAYER AND LAMINATED GLASS |
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Cited By (2)
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WO2022270540A1 (ja) * | 2021-06-23 | 2022-12-29 | 株式会社クラレ | アイオノマー樹脂組成物を含んでなる層を有する樹脂シートおよび合わせガラス |
WO2023032909A1 (ja) * | 2021-08-30 | 2023-03-09 | 株式会社クラレ | アイオノマー樹脂組成物、樹脂シートおよび合わせガラス |
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JP2010024061A (ja) * | 2008-07-15 | 2010-02-04 | Sekisui Chem Co Ltd | 光拡散性合わせガラス用中間膜、及び、合わせガラス |
JP2015513586A (ja) * | 2012-02-24 | 2015-05-14 | イー・アイ・デュポン・ドウ・ヌムール・アンド・カンパニーE.I.Du Pont De Nemours And Company | 半透明白色ポリマー組成物ならびにガラス積層体および他の物品におけるその使用 |
JP2019053411A (ja) | 2017-09-13 | 2019-04-04 | 大日本印刷株式会社 | 考査処理装置及び印画物作製システム |
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EP1501672B1 (en) * | 2002-05-03 | 2015-02-25 | E.I. Du Pont De Nemours And Company | Interlayer composite structure for laminating glass with controlled diffusing properties at high transmission and a process for making same |
JP4884575B2 (ja) * | 2010-05-13 | 2012-02-29 | 三井・デュポンポリケミカル株式会社 | 多層材料、太陽電池用封止材、安全(合わせ)ガラス用中間膜、太陽電池モジュール及び安全(合わせ)ガラス |
JP6027829B2 (ja) * | 2012-09-14 | 2016-11-16 | 三井・デュポンポリケミカル株式会社 | 合わせガラス用中間膜および合わせガラス |
CN104769032B (zh) * | 2012-11-09 | 2017-08-04 | 三井—杜邦聚合化学株式会社 | 树脂组合物及成型体 |
EP3070063B1 (en) * | 2013-11-14 | 2022-10-19 | Sekisui Chemical Co., Ltd. | Intermediate film for laminated glass and laminated glass |
JP6635933B2 (ja) * | 2014-10-15 | 2020-01-29 | 三井・ダウポリケミカル株式会社 | 合わせガラス及び合わせガラス用中間膜 |
JP2016188158A (ja) * | 2015-03-30 | 2016-11-04 | 三井・デュポンポリケミカル株式会社 | 積層体及び合わせガラス |
EP3466899A4 (en) * | 2016-05-27 | 2020-01-15 | Nippon Kayaku Kabushiki Kaisha | INTERMEDIATE LAYER FOR LAMINATED GLASS AND GLASS USING THE SAME |
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EP3461266A4 (en) * | 2017-07-31 | 2020-05-06 | Kuraray America, Inc. | INTERMEDIATE IONOMER WITH IMPROVED ADHESIVE PROPERTIES |
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- 2020-03-06 EP EP20774824.5A patent/EP3943463A4/en active Pending
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WO2023032909A1 (ja) * | 2021-08-30 | 2023-03-09 | 株式会社クラレ | アイオノマー樹脂組成物、樹脂シートおよび合わせガラス |
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EP3943463A4 (en) | 2022-12-07 |
KR102618416B1 (ko) | 2023-12-28 |
BR112021018678A2 (pt) | 2021-11-23 |
JP7133084B2 (ja) | 2022-09-07 |
US20220184928A1 (en) | 2022-06-16 |
JPWO2020189335A1 (ja) | 2021-12-02 |
CN113597415A (zh) | 2021-11-02 |
KR20210138704A (ko) | 2021-11-19 |
CN113597415B (zh) | 2023-07-04 |
EP3943463A1 (en) | 2022-01-26 |
TW202045608A (zh) | 2020-12-16 |
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