WO2014188544A1 - Stratifié ayant d'excellentes caractéristiques d'isolation sonore - Google Patents

Stratifié ayant d'excellentes caractéristiques d'isolation sonore Download PDF

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Publication number
WO2014188544A1
WO2014188544A1 PCT/JP2013/064261 JP2013064261W WO2014188544A1 WO 2014188544 A1 WO2014188544 A1 WO 2014188544A1 JP 2013064261 W JP2013064261 W JP 2013064261W WO 2014188544 A1 WO2014188544 A1 WO 2014188544A1
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mass
laminate
laminated glass
compound
parts
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PCT/JP2013/064261
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English (en)
Japanese (ja)
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芳聡 浅沼
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株式会社クラレ
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Priority to PCT/JP2013/064261 priority Critical patent/WO2014188544A1/fr
Priority to JP2013525030A priority patent/JP5373231B1/ja
Publication of WO2014188544A1 publication Critical patent/WO2014188544A1/fr

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    • 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

Definitions

  • the present invention relates to a laminate containing polyvinyl acetal.
  • a sheet containing polyvinyl acetal and a plasticizer is widely used as an interlayer film for laminated glass because of its excellent adhesion and transparency to glass and mechanical strength.
  • the interlayer film for laminated glass is usually used in a state containing a small amount of water.
  • the moisture content of the interlayer film for laminated glass needs to be appropriately selected depending on the type of the laminated glass manufacturing process. For example, when producing laminated glass on a large scale, due to its high productivity, the glass and the laminated glass interlayer film are temporarily bonded with a nip roll, and then heated and pressurized with an autoclave to perform main bonding.
  • the method is widely used. Since this method does not include a reduced pressure treatment step in a series of steps, the risk of water volatilizing during the production of laminated glass and foaming in the interlayer film for laminated glass is low. Therefore, in this method, from the viewpoint of simplifying the humidity control process, a laminated glass interlayer film having a relatively high moisture content (for example, about 0.4 to 0.7%) is used.
  • a vacuum bag or a vacuum laminator is used for producing laminated glass, particularly when it is difficult to introduce a large and expensive apparatus.
  • a laminated glass is produced by heat-treating a glass and a laminated glass interlayer film under reduced pressure, so there is a risk that water will foam in the laminated glass interlayer film, resulting in bubbles and loss of appearance. high. Therefore, from the viewpoint of improving the yield in the production of laminated glass, the moisture content of the interlayer film for laminated glass is usually adjusted to be relatively low (for example, about 0.01 to 0.3%).
  • the interlayer film for laminated glass generally contains a plasticizer, but the plasticizer is extracted by water adhering to the exposed portion of the interlayer film at the end of the laminated glass, and the glass and the interlayer film are separated.
  • the appearance of the laminated glass may be impaired due to peeling or bubbles.
  • the plasticizer may volatilize from the edge of the laminated glass when a reduced pressure process is performed during the production of the laminated glass or when the laminated glass is used for a long time.
  • the present invention solves the above problems, and the plasticizer contained in the laminate is difficult to be extracted by water and hardly volatilized.
  • the plasticizer contained in the laminate is difficult to be extracted by water and hardly volatilized.
  • sound insulation is achieved even when the moisture content is changed. It aims at providing the laminated body from which a change of property does not occur.
  • the object described above is based on the general formula (I): 100 parts by mass of polyvinyl acetal (A) having an average residual hydroxyl group content of 25 to 45 mol%: (Wherein R 1 and R 2 represent a hydrocarbon group having 7 to 11 carbon atoms, which may be the same or different, and m represents a natural number of 3 to 10) Content of Compound (I) a1 is 20 to 60 parts by mass, and the general formula (II): (Wherein R 3 is the same as either R 1 or R 2 , n represents a natural number of 3 to 10) and the content of the compound (II) is A2 parts by mass, The content b1 of the compound (I) is 35 to 75 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (B) having an average residual hydroxyl group content of 10 to 35 mol%, and the content of the compound (II) is b2 parts by mass.
  • A2 is 0 or (b2 / b1) / (a2 / a1)> 1, (b1-a1)> 0, and a2 / a1 is 0 to 0. This is preferably achieved by providing a laminate having a ratio of 05 and b2 / b1 of 0.001 to 0.08.
  • the layer A preferably contains 0.001 to 0.1 parts by mass of a magnesium salt with respect to 100 parts by mass of the polyvinyl acetal (A).
  • M and n are preferably the same.
  • R 1 and R 2 are preferably the same.
  • R 1 and R 2 are preferably a 3-heptyl group.
  • both outermost layers are preferably A layers.
  • the above object is suitably achieved by providing a laminated glass including the laminate.
  • the plasticizer contained in the laminate is difficult to be extracted and volatilized by water, and when used as an interlayer film for laminated glass, the laminate does not cause a change in sound insulation even when the moisture content is changed. Can provide the body.
  • the average residual hydroxyl group content of the polyvinyl acetal (A) is 25 to 45 mol%, preferably 25 to 40 mol%, more preferably 25 to 35 mol%. If the average residual hydroxyl group content is less than 25 mol%, the mechanical strength of the laminate and the adhesion to glass may be reduced. If the average residual hydroxyl group content exceeds 45 mol%, the compound contained in the A layer The compatibility with (I) may be reduced.
  • the degree of acetalization of the polyvinyl acetal (A) is preferably 50 to 74 mol%, more preferably 60 to 74 mol%, and further preferably 65 to 74 mol%.
  • the average residual vinyl ester group amount of the polyvinyl acetal (A) is preferably 0.01 to 5 mol%, more preferably 0.01 to 4 mol%, and 0.01 to 3 mol%. More preferably. Polyvinyl acetal having an average residual vinyl ester group content of less than 0.01 mol% is difficult to produce industrially at low cost.
  • the average residual vinyl ester group amount of the polyvinyl acetal (A) exceeds 5 mol%, the average residual hydroxyl group amount of the polyvinyl acetal (A) is increased by hydrolysis of the vinyl ester group when the laminate is used over a long period of time.
  • the compatibility with compound (I) may change over time.
  • the average residual hydroxyl group content of the polyvinyl acetal (B) used in the present invention is 10 to 35 mol%, preferably 13 to 30 mol%, more preferably 15 to 25 mol%.
  • Polyvinyl acetal having an average residual hydroxyl group content of less than 10 mol% is difficult to produce industrially at low cost.
  • the average residual vinyl ester group amount of the polyvinyl acetal (B) exceeds 35 mol%, the compatibility with the compound (I) contained in the B layer may be lowered.
  • the degree of acetalization of the polyvinyl acetal (B) is preferably 60 to 85 mol%, more preferably 65 to 82 mol%, and further preferably 69 to 78 mol%.
  • the degree of acetalization of the polyvinyl acetal (A) is less than 60 mol%, the compatibility with the compound (I) contained in the B layer may be lowered.
  • Polyvinyl acetal having an acetalization degree exceeding 85 mol% is difficult to produce industrially at low cost.
  • the average residual vinyl ester group amount of the polyvinyl acetal (B) is preferably 0.01 to 20 mol%, more preferably 0.5 to 16 mol%, and 4 to 13 mol%. More preferably. Polyvinyl acetal having an average residual vinyl ester group content of less than 0.01 mol% is difficult to produce industrially at low cost.
  • the average residual vinyl ester group amount exceeds 20 mol%
  • the average residual hydroxyl group amount of the polyvinyl acetal (B) is increased by hydrolysis when used over a long period of time, and the compatibility with the compound (I) increases with time. May change significantly.
  • the polyvinyl acetal (A) and the polyvinyl acetal (B) used in the present invention are produced using polyvinyl alcohol as a raw material.
  • Polyvinyl alcohol can be obtained by a conventionally known method. That is, it can be obtained by polymerizing a vinyl ester compound and saponifying the obtained polymer.
  • a method for polymerizing the vinyl ester compound conventionally known methods such as a solution polymerization method, a bulk polymerization method, a suspension polymerization method, and an emulsion polymerization method can be applied.
  • As a polymerization initiator used in these polymerization methods an azo initiator, a peroxide initiator, a redox initiator, or the like can be used as appropriate.
  • the saponification reaction is carried out by subjecting the vinyl ester group of the polymer to alcoholysis or hydrolysis using a conventionally known alkali catalyst or acid catalyst.
  • a conventionally known alkali catalyst or acid catalyst e.g., methanol as a solvent and caustic soda (NaOH) as a catalyst is simple and most preferable.
  • vinyl ester compound examples include conventionally known carboxylic acid vinyl esters such as vinyl formate, vinyl acetate, vinyl propionate, vinyl butyrate, vinyl stearate, vinyl benzoate, and vinyl acetate is preferred.
  • a modified polyvinyl alcohol obtained by saponifying a copolymer obtained by copolymerizing a vinyl ester compound and a monomer copolymerizable with the vinyl ester compound is used.
  • the monomer copolymerizable with the vinyl ester compound is usually used in a proportion of less than 10 mol% with respect to the vinyl ester compound.
  • the viscosity average degree of polymerization of polyvinyl alcohol used as a raw material for the polyvinyl acetal used in the present invention is not particularly limited and can be appropriately selected depending on the application, but is usually preferably 150 to 3000, more preferably 800 to 2500, and more preferably 1000 to 2000. Is more preferable.
  • the viscosity average polymerization degree of polyvinyl alcohol is lower than 150, the resulting laminate tends to have insufficient mechanical strength, and when it is higher than 3000, the laminate is easy to handle, especially laminated glass for use as an interlayer film for laminated glass. The ease of manufacturing tends to decrease.
  • the polyvinyl acetal used in the present invention can be produced by a conventionally known method.
  • it can be produced by a precipitation method under the following reaction conditions.
  • an aqueous polyvinyl alcohol solution having a concentration of 3 to 40% by mass is maintained in a temperature range of 80 to 100 ° C., and then gradually cooled over 10 to 60 minutes.
  • an aldehyde and an acid catalyst are added, and an acetalization reaction is performed for 30 to 300 minutes while keeping the temperature constant.
  • polyvinyl acetal having a certain degree of acetalization is deposited.
  • the reaction solution is heated to a temperature of 30 to 80 ° C. over 30 to 300 minutes, and the temperature is maintained for 10 to 500 minutes.
  • a basic compound is added to the reaction solution, the acid catalyst is neutralized, washed with water, and dried to obtain polyvinyl acetal.
  • the acid catalyst used in the acetalization reaction is not particularly limited, and any of organic acids such as acetic acid and paratoluenesulfonic acid or inorganic acids such as nitric acid, sulfuric acid and hydrochloric acid can be used. Preferably used.
  • the aldehyde used in the acetalization reaction is not particularly limited, but it is preferable to acetalize with an aldehyde having 1 to 8 carbon atoms. Of these, aldehydes having 4 to 6 carbon atoms are preferably used, and n-butyraldehyde is particularly preferably used. In the present invention, polyvinyl acetal obtained by using two or more aldehydes in combination can also be used.
  • R 1 and R 2 represent a hydrocarbon group having 7 to 11 carbon atoms which may be the same or different.
  • the hydrocarbon group has more preferably 7 to 10 carbon atoms, and more preferably 7 to 9 carbon atoms. If the carbon number is less than 7, the volatility of the compound (I) may be increased, which may be a problem. If the carbon number exceeds 11, the compatibility between the compound (I) and polyvinyl acetal may be reduced, or the compound ( The plasticizing effect of I) on polyvinyl acetal may be reduced.
  • the hydrocarbon group may be linear or branched, and may have an unsaturated bond. Moreover, some hydrogen atoms in the hydrocarbon group may be substituted with other atoms or substituents other than hydrogen atoms.
  • R 1 and R 2 include alkyl groups such as heptyl group, octyl group, nonyl group, decanyl group, isodecanyl group, and 3-heptyl group; alkenyl groups such as 3-hept-3-ene group; A chlorooctyl group etc. are mentioned. Among them, a hydrocarbon group having a branched structure is preferable in that it is not easily hydrolyzed. Particularly, when R 1 and R 2 are both 3-heptyl groups, compatibility with polyvinyl acetal and plasticization to polyvinyl acetal are preferable. It is particularly preferable from the viewpoint of effect.
  • R 1 and R 2 are preferably the same from the viewpoint of obtaining compound (I) at low cost.
  • the compound (I) contained in the A layer and the compound (I) contained in the B layer may be the same or different, but are preferably the same from the viewpoint of availability.
  • the compound (I) contained in the A layer and the B layer may be one kind alone or a mixture of two or more kinds.
  • M represents a natural number of 3 to 10, preferably 3 to 8, and more preferably 3 to 4.
  • a compound (I) has a low polarity and is preferable in that it is difficult to extract when the A layer and water contact. If m is less than 3, the volatility of the compound (I) may be increased, which may cause a problem. If m exceeds 10, the compatibility between the compound (I) and polyvinyl acetal may be reduced, or the compound (I) The plasticizing effect on polyvinyl acetal may decrease.
  • the compound (I) include triethylene glycol di-2-ethylhexanoate, tetraethylene glycol di-2-ethylhexanoate, octaethylene glycol di-2-ethylhexanoate, triethylene glycol di-2-octanoate. And triethylene glycol didodecanoate. Among them, triethylene glycol di-2-ethylhexanoate is preferable because it is excellent in compatibility with polyvinyl acetal, has excellent plasticizing effect on polyvinyl acetal, and is not easily hydrolyzed.
  • the content a1 of the compound (I) in the layer A is 20 to 60 parts by mass, preferably 25 to 55 parts by mass, more preferably 30 to 50 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (A). It is. When a1 is less than 20 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (A), sufficient sound insulation may not be exhibited when the obtained laminate is used for laminated glass. On the other hand, when a1 exceeds 60 parts by mass, sufficient mechanical strength may not be exhibited when the obtained laminate is used for laminated glass.
  • the content b1 of the compound (I) in the B layer is 35 to 75 parts by mass, preferably 40 to 72 parts by mass, more preferably 52 to 70 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (B). is there.
  • b1 is less than 35 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (B)
  • sufficient sound insulation may not be exhibited when the obtained laminate is used for laminated glass.
  • b1 exceeds 70 parts by mass, the compatibility between the polyvinyl acetal (B) and the compound (I) in the B layer is lowered, and the transparency of the resulting laminate is impaired, or sufficient mechanical strength is obtained. It may not develop.
  • (b1-a1)> 0 preferably 40> (b1-a1)> 7, more preferably 40> (b1-a1)> 15, and optimally 40 > (B1-a1)> 20.
  • (b1-a1)> 0 sufficient sound insulation is exhibited when the laminate is used for laminated glass.
  • (b1-a1) is 40 or more, sound insulation may be insufficient.
  • R 3 is the same as either R 1 or R 2 , and n represents a natural number of 3 to 10.
  • Compound (II) is similar to the chemical structure of Compound (I) and has excellent compatibility with Compound (I). Therefore, it is difficult to extract even when the laminate is in contact with water. It is also suitable for long-term use as an interlayer film. From the above viewpoint, it is particularly preferable that m of compound (I) and n of compound (II) are the same.
  • the compound (II) examples include triethylene glycol mono 2-ethylhexanoate, tetraethylene glycol mono 2-ethyl hexanoate, octaethylene glycol mono 2-ethyl hexanoate, triethylene glycol mono 2-octanoate. And triethylene glycol monododecanoate.
  • the preferred compound (I) used in the present invention is triethylene glycol di-2-ethylhexanoate, it is preferable to use triethylene glycol mono-2-ethylhexanoate as the compound (II).
  • the content a2 of the compound (II) in the A layer is preferably 0 to 2.5 parts by mass, more preferably 0.005 to 2.2 parts by mass, and more preferably 0.035 to 2.2 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (A). 2 parts by mass is more preferred.
  • a2 is within the above range, the adhesiveness between the laminate and the glass hardly changes even when the amount of moisture changes. Further, when the laminate is used as an interlayer film for laminated glass, the compound (II) is hardly extracted into water even if the laminate is in contact with water.
  • the content b2 of the compound (II) in the B layer is preferably 0.01 to 3 parts by mass, more preferably 0.02 to 2.4 parts by mass, and further preferably 0.1 to 2.2 parts by mass.
  • b1 is less than 0.01 parts by mass, sound insulation may be lowered when the moisture content of the laminate is changed.
  • b1 is more than 3 parts by mass, for example, when the laminate is used for an interlayer film for laminated glass, when the laminate is in contact with water, a part of the compound (II) is extracted into water, and the appearance of the laminated glass The above disadvantages may occur.
  • the compound (II) contained in the A layer and the compound (II) contained in the B layer may be the same or different, but are preferably the same from the viewpoint of availability. Further, the compound (II) contained in each of the A layer and the B layer may be a single type or a mixture of two or more types.
  • a2 / a1 is 0 to 0.05, preferably 0.0007 to 0.045, and more preferably 0.001 to 0.04.
  • the sound insulation may be lowered when the moisture content of the laminate is changed when used as an interlayer film for laminated glass.
  • b2 / b1 is 0.001 to 0.08, preferably 0.0015 to 0.07, and more preferably 0.002 to 0.06.
  • the sound insulation may be lowered when the moisture content of the laminate is changed. .
  • a2 is 0 or (b2 / b1) / (a2 / a1)> 1.0.
  • a2 is 0 or when a2 is not 0, (b2 / b1) / (a2 / a1)> 1.1.
  • a2 is 0 or when a2 is not 0, [(b2 / b1) / (a2 / a1)]> 1.4.
  • [(b2 / b1) / (a2 / a1)] is 1.0 or less, when the moisture content of the laminate is changed and used as an interlayer film for laminated glass, sound insulation May decrease.
  • the laminate of the present invention may further contain an antioxidant, an ultraviolet absorber, an adhesion improver, and other additives.
  • the type of antioxidant that the laminate of the present invention may contain.
  • conventionally known phenolic antioxidants, phosphorus antioxidants, sulfur antioxidants, and the like can be used. Of these, phenolic antioxidants are preferred.
  • Antioxidants may be used alone or in combination of two or more.
  • the amount thereof is not particularly limited, but is usually in the range of 0.0001 to 5% by mass, preferably 0.001 to 1% by mass with respect to the mass of the laminate. When the amount is less than 0.0001% by mass, a sufficient effect as an antioxidant may not be obtained, and when the amount is more than 5% by mass, a remarkable effect cannot be expected.
  • the type of ultraviolet absorber that the laminate of the present invention may contain.
  • conventionally known benzotriazole ultraviolet absorbers, oxalic anilide ultraviolet absorbers, benzoate ultraviolet absorbers, and the like can be used.
  • the ultraviolet absorbers may be used alone or in combination of two or more.
  • the amount thereof is not particularly limited, but is usually 0.0001 to 5% by mass, preferably 0.001 to 1% by mass with respect to the mass of the laminate. When the amount is less than 0.0001% by mass, a sufficient effect as an ultraviolet absorber may not be obtained, and when the amount is more than 5% by mass, a remarkable effect cannot be expected.
  • the laminate of the present invention is particularly preferably used as an interlayer film for laminated glass.
  • an adhesion adjusting agent is added to the layer that adheres to the glass.
  • the adhesion adjusting agent include sodium salt, potassium salt, magnesium salt and the like of organic acids such as acetic acid, propionic acid, butanoic acid, hexanoic acid, 2-ethylbutanoic acid and 2-ethylhexanoic acid. More than one kind may be added.
  • the addition amount of the adhesion adjusting agent is 0.001 to 0.1 parts by mass with respect to 100 parts by mass of the polyvinyl acetal (A) from the viewpoint of penetration resistance of the laminated glass and prevention of glass piece scattering when the laminated glass is broken. Is preferably 0.005 to 0.08 parts by mass, more preferably 0.01 to 0.06 parts by mass, and particularly preferably 0.03 to 0.055 parts by mass.
  • the method for producing the laminate of the present invention is not particularly limited, and conventionally known methods can be applied.
  • the component constituting the A layer and the component constituting the B layer are each melt-kneaded with an extruder and subsequently co-extruded with a multilayer film forming machine; the A layer and the B prepared individually by hot pressing or casting after the melt-kneading
  • stacking a layer and sticking by hot press etc. as needed is mentioned.
  • the laminate of the present invention When the laminate of the present invention is used as an interlayer film for laminated glass, it exhibits a certain characteristic with a wide range of moisture content. Therefore, the moisture content of the interlayer film for laminated glass that is temporarily bonded by an autoclave after temporary bonding with a nip roll Laminated glass can be produced by a method in which the moisture content of the laminated glass interlayer film that is heat-treated under reduced pressure using a vacuum bag or a vacuum laminator is adjusted to a relatively low level.
  • the moisture content of the laminate of the present invention is preferably from 0.01 to 1.0% by mass, more preferably from 0.02 to 0.9% by mass, and even more preferably from 0.03 to 0.8% by mass.
  • the moisture content of the laminate of the present invention is less than 0.01% by mass because it takes a long time to adjust to such a moisture content, and the moisture content of the laminate of the present invention is not preferred.
  • the amount exceeds 1.0% by mass the adhesion of the laminate to the glass and the transparency may change, which is not preferable.
  • the thickness of the A layer and the B layer in the laminate of the present invention is not particularly limited.
  • the thickness of the A layer is usually preferably 0.05 to 1.2 mm, more preferably 0.07 to 1 mm, further preferably 0.1 to 0.6 mm, and particularly preferably 0.12 to 0.5 mm. If the thickness is less than 0.05 mm, the mechanical strength of the laminate of the present invention tends to decrease, and for example, it may be insufficient for use as a laminated glass interlayer. When it is thicker than 1.2 mm, the laminate of the present invention tends to have insufficient flexibility. For example, in use as a laminated glass interlayer, the safety of the resulting laminated glass may be lowered.
  • the thickness of the B layer is usually preferably 0.01 to 1 mm, more preferably 0.02 to 0.6 mm, and further preferably 0.05 to 0.4 mm. If the thickness is less than 0.01 mm, the sound insulation performance of the laminated glass using the laminate of the present invention as an intermediate film may deteriorate, and even if it is thicker than 1 mm, the mechanical strength and sound insulation performance of the laminate of the present invention are more than that. There is a tendency not to improve.
  • the laminate of the present invention is used as an interlayer film for laminated glass
  • the laminate is composed of three or more layers, and the outermost layers are both A layers. It is preferable from the viewpoint of adjustment.
  • Examples of the laminate in which the outermost layers are both A layers include A layer / B layer / A layer, A layer / B layer / A layer / B layer / A layer, and the like.
  • the thickness of each layer may be the same or different.
  • two or more B layers are included, the thickness of each layer may be the same or different. .
  • the thickness of the laminate is not particularly limited, but is usually preferably 0.2 to 2 mm, more preferably 0.25 to 1.8 mm, and More preferably, the thickness is 3 to 1.5 mm. If the thickness of the laminate is thinner than 0.2 mm, the mechanical strength tends to be insufficient, and if it is thicker than 2 mm, the flexibility tends to be insufficient.
  • the glass material when using the laminate of the present invention as an interlayer film for laminated glass is not particularly limited, inorganic glass such as float plate glass, heat tempered glass, chemically tempered glass; organic glass such as polymethyl methacrylate, polycarbonate, etc. Conventionally known glass can be used. These may be colorless or colored, transparent or non-transparent, and two or more of them may be used in combination. Although there is no limitation in particular in the thickness of glass, Usually, 20 mm or less is preferable and 10 mm or less is more preferable.
  • the shape of the outermost surface of the laminated body is not particularly limited, but considering the handleability when producing a laminated glass (for example, bubble removal in the laminate), It is preferable to form a concavo-convex structure on the outermost surface of the laminate by a conventionally known method such as melt fracture or embossing.
  • the method of producing laminated glass using the laminate of the present invention as an interlayer film for laminated glass is not particularly limited.
  • a method of undergoing a decompression step using a vacuum laminator device or a vacuum bag is mentioned, such as the method of not passing through the pressure reduction process to process.
  • An example of manufacturing conditions when using a vacuum laminator is as follows: treatment at a temperature of 100 to 200 ° C., preferably 130 to 160 ° C. for 10 to 300 minutes under a reduced pressure of 1 ⁇ 10 ⁇ 6 to 3 ⁇ 10 ⁇ 2 MPa. Then, an interlayer film for laminated glass is laminated with glass. In the case of using a vacuum bag, for example, it is laminated by treatment at 130 to 145 ° C. for 10 to 300 minutes under a pressure of 2 ⁇ 10 ⁇ 4 to 3 ⁇ 10 ⁇ 2 MPa.
  • the laminated glass is produced by the method of passing through these pressure reduction steps, it is preferable to use a laminate having a moisture content of 0.01 to 0.3% by mass, and bubbles are generated in the laminate during lamination. From the viewpoint of preventing this, it is preferable.
  • An example of the operating conditions of the nip roll in the method of pre-bonding with a nip roll and then processing with an autoclave is to heat the glass and the laminate to 50 to 120 ° C. with an infrared heater or the like, and then pressure-bond them temporarily with a roll.
  • the autoclaving step is performed, for example, at a temperature of 130 to 145 ° C. for 30 to 200 minutes under a pressure of 1.0 to 1.5 MPa.
  • the moisture content of the laminate is 0.4 to 0.7% by mass from the viewpoint of simplifying the humidity control (drying) step of the laminate. It is preferable to use one made to a degree.
  • PVB-1 polyvinyl butyral
  • PVB-3 (Preparation of PVB-3) In the preparation of PVB-1, after changing PVA-1 to 330 g PVA-2 (viscosity average polymerization degree 1700, saponification 92 mol%) and butyraldehyde use amount to 198 g, and further carrying out a butyralization reaction at 5 ° C. PVB-3 was obtained in the same manner except that the temperature was raised to 67 ° C. over 70 minutes and the reaction was carried out at 67 ° C. for 120 minutes. The PVB-3 thus obtained was measured according to JIS K6728. As shown in Table 1, the average degree of acetalization was 74 mol%, the average residual vinyl ester group amount was 7 mol%, and the average residual hydroxyl group amount was 19 mol. %Met.
  • PVB-4 (Preparation of PVB-4)
  • PVA-2 was changed to 330 g of PVA-3 (viscosity average polymerization degree 1700, saponification 90 mol%)
  • butyraldehyde was used in an amount of 204 g
  • a butyralization reaction was carried out at 5 ° C.
  • PVB-4 was obtained in the same manner except that the temperature was raised to 67 ° C. over 70 minutes and the reaction was carried out at 67 ° C. for 120 minutes.
  • the properties of the obtained PVB-4 were measured according to JIS K6728. As shown in Table 1, the average degree of acetalization was 75 mol%, the average residual vinyl ester group amount was 9 mol%, and the average residual hydroxyl group amount was 16 mol. %Met.
  • Example 1 (Production of laminate) 100 parts by weight of PVB-1, 36 parts by weight of triethylene glycol di-2-ethylhexanoate as compound (I), 0.3 parts by weight of triethylene glycol mono-2-ethylhexanoate as compound (II) and 0.048 parts by mass of magnesium acetate tetrahydrate was kneaded in a Laboplast mill at 160 ° C. for 8 minutes. The obtained kneaded material was pressed for 30 minutes in a mold having a thickness of 0.38 mm under the conditions of 160 ° C. and 50 kg / cm 2 to obtain a sheet A having a thickness of 0.38 mm.
  • Laminate-1 of 30 cm ⁇ 30 cm was stored in a desiccator adjusted to 23 ° C. and 5 to 10% RH for 5 days to adjust the humidity (dry).
  • the layered product-1 after humidity control is quickly sandwiched between two float glasses (30 cm x 30 cm x 2.2 mm), placed in a vacuum bag, and the inside of the vacuum bag is depressurized to 3 x 10 -3 MPa at room temperature. While maintaining the degree of vacuum, the mixture was heated to 135 ° C. over 30 minutes, and held at 135 ° C. for 2 hours to obtain laminated glass-1 (V).
  • the moisture content of laminate-1 in the obtained laminated glass-1 (V) was 0.11%.
  • the moisture content is as follows.
  • Laminated glass-1 is quickly taken out by hitting a portion of laminated glass-1 (V) that is more than 1 cm away from the edge with a hammer and breaking the glass.
  • V laminated glass-1
  • VA-200 water vaporizer
  • Laminated glass-1 (V) and laminated glass-1 (NA) were each cut to a size of 2.5 cm ⁇ 30 cm, and were shaken under an atmosphere of 25 ° C. (EMIC Corporation, small vibration generator 512-A).
  • the frequency response function at that time was detected with an FFT analyzer (DS-2100, manufactured by Ono Sokki Co., Ltd.), and at 3000 Hz using servo analysis software (DS-0242, manufactured by Ono Sokki Co., Ltd.).
  • the loss factor was calculated. The larger the loss factor, the better the sound insulation performance of the laminated glass.
  • Laminated glass cooling test Laminated glass-1 (V) and laminated glass-1 (NA) were held at 80 ° C. for 2 hours, then cooled from 80 ° C. to ⁇ 20 ° C. over 50 minutes, and further held at ⁇ 20 ° C. for 2 hours. The mixture was heated from ⁇ 20 ° C. to 80 ° C. over 50 minutes (this treatment is defined as one cycle). After repeating this cycle a total of 30 times, check if there is no separation between the glass and the laminate, and between the A layer and the B layer in the laminate. A sample having only a portion of 0 to 1 cm was designated as B, and a sample having peeling at a portion exceeding 1 cm from the edge of the glass was designated as C.
  • Laminated glass hot water treatment test Laminated glass-1 (NA) was immersed in warm water of 60 ° C. for 12 hours, and then allowed to stand in an atmosphere of 23 ° C. and 28% RH for 108 hours (this treatment is defined as one cycle). After repeating this process 10 times, at the end of each laminated glass, the presence or absence of occurrence of defects (peeling of glass and interlayer film for laminated glass, peeling of interlayer of interlayer film) due to extraction of components contained in the laminate is visually observed. confirmed.
  • Examples 2 to 33, Comparative Examples 1 to 9 A laminate and a laminated glass were produced in the same manner as in Example 1 except that the compositions of the A layer and the B layer were changed as shown in Table 2 and Table 4. The obtained laminated glass was evaluated in the same manner as in Example 1. The results are shown in Table 3 and Table 5.
  • the laminate of the present invention When the laminate of the present invention is used as an interlayer film for laminated glass, it is produced with a low moisture content by a vacuum laminator or a vacuum bag, or is produced with a high moisture content by an autoclave after temporary bonding with a nip roll. Can exhibit the same excellent characteristics.
  • the plasticizer contained in the laminate is difficult to be extracted by water and is not easily volatilized.
  • the plasticizer contained in the laminate is difficult to be extracted by water and is not easily volatilized.
  • the moisture content is changed, even if the moisture content is changed, a change in sound insulation properties does not occur. Absent.

Landscapes

  • Joining Of Glass To Other Materials (AREA)
  • Laminated Bodies (AREA)

Abstract

L'invention concerne un stratifié qui présente une excellente compatibilité avec de l'acétal polyvinylique et un excellent effet de fusion d'acétal polyvinylique, et utilise un plastifiant qui ne peut pas être extrait avec de l'eau ni se volatiliser, un changement de sa teneur en eau ne changeant pas ses caractéristiques d'isolation sonore. Un stratifié comprend : une couche A qui contient 100 parties en masse d'un acétal polyvinylique (A) ayant une quantité moyenne de groupe hydroxyle résiduel comprise dans la plage allant de 25 à 45 % en mole, un composé (I) ayant une quantité (a1) allant de 20 à 60 parties en masse et représenté par la formule (I), et un composé (II) ayant une quantité (a2) et représenté par la formule (II) ; et une couche B qui contient 100 parties en masse d'un acétal polyvinylique (B) ayant une quantité moyenne de groupe hydroxyle résiduel comprise dans la plage allant de 10 à 35 % en mole, le composé (I) ayant une quantité (b1) de 35-75 parties en masse, et le composé (II) ayant une quantité (b2). Dans la présente invention, a2 est 0 ou (b2/b1)/(a2/a1)>1, (b1-a1)>0, a2/a1 est 0-0.05, et b2/b1 est 0.001-0.08.
PCT/JP2013/064261 2013-05-22 2013-05-22 Stratifié ayant d'excellentes caractéristiques d'isolation sonore WO2014188544A1 (fr)

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WO2018061861A1 (fr) 2016-09-27 2018-04-05 株式会社クラレ Film intermédiaire pour verre feuilleté
KR20180128036A (ko) 2016-03-28 2018-11-30 주식회사 쿠라레 합판 유리용 중간막

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JPH11323055A (ja) * 1998-05-18 1999-11-26 Sekisui Chem Co Ltd 可塑剤
JPH11323056A (ja) * 1998-05-18 1999-11-26 Sekisui Chem Co Ltd 合わせガラス用中間膜および合わせガラス
WO2011078314A1 (fr) * 2009-12-25 2011-06-30 積水化学工業株式会社 Film intermédiaire pour verre laminé, et verre laminé

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JP5749095B2 (ja) * 2011-06-23 2015-07-15 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
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JPH11323055A (ja) * 1998-05-18 1999-11-26 Sekisui Chem Co Ltd 可塑剤
JPH11323056A (ja) * 1998-05-18 1999-11-26 Sekisui Chem Co Ltd 合わせガラス用中間膜および合わせガラス
WO2011078314A1 (fr) * 2009-12-25 2011-06-30 積水化学工業株式会社 Film intermédiaire pour verre laminé, et verre laminé

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Publication number Priority date Publication date Assignee Title
KR20180128036A (ko) 2016-03-28 2018-11-30 주식회사 쿠라레 합판 유리용 중간막
US11325354B2 (en) 2016-03-28 2022-05-10 Kuraray Co., Ltd. Interlayer film for laminated glass
WO2018061861A1 (fr) 2016-09-27 2018-04-05 株式会社クラレ Film intermédiaire pour verre feuilleté
KR20190061016A (ko) 2016-09-27 2019-06-04 주식회사 쿠라레 합판 유리용 중간막

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