JP2001261383A - Interlayer for laminated glass and laminated glass - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain both an interlayer for a laminated glass having excellent heat insulating properties and transparency, not the electromagnetic wave transmission properties, having excellent adhesiveness at the interface between glass and the interlayer and a laminated glass using the same. SOLUTION: This interlayer for an laminated glass comprises a plasticized polyvinyl acetal resin which is composed of 100 pts.wt. of a polyvinyl acetal resin, 30-50 pts.wt. of a plasticizer, 0.13-5.0 pts.wt. of a zinc oxide particle containing one or more kinds of metal elements capable of being a trivalent and/or a tetravalent metal and 10-150 ppm of magnesium salt and/or potassium salt of a 2-10C carboxylic acid.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to transparency, heat shielding,
The present invention relates to an interlayer film for laminated glass having excellent light resistance and electromagnetic wave transmittance and excellent adhesion to glass, and a laminated glass using the same.

[0002]

2. Description of the Related Art Conventionally, laminated glass in which an interlayer film is sandwiched between transparent glass plates is safe even if broken by an external impact, because fragments of the glass plate are less likely to scatter and are safe. Widely used for window glass of vehicles, aircrafts, buildings and the like. As such an intermediate film, a polyvinyl butyral resin plasticized with a plasticizer is widely used.

[0003] However, such laminated glass is excellent in safety as described above, but has a problem in that it is inferior in heat insulation. Among rays, infrared rays having a wavelength of 780 nm or more have a small energy amount of about 10% as compared with ultraviolet rays, but have a large thermal effect. When absorbed by a substance, they are released as heat and cause a temperature rise. Therefore, it is called a hot wire.

[0004] Therefore, by blocking the infrared rays entering from the windshield and the side glass to suppress a rise in the temperature of the vehicle, it is possible to enhance the heat shielding property. As such a glass plate, for example, a heat ray cut glass or the like is commercially available.

[0005] The above-mentioned heat ray cut glass has a multi-layer coating of metal / metal oxide applied to the surface of a glass plate by metal deposition, sputtering or the like for the purpose of blocking direct sunlight. However, since this multilayer coating is vulnerable to external abrasion and has poor chemical resistance, for example, a method of laminating an interlayer made of plasticized polyvinyl butyral resin or the like to form a laminated glass has been adopted.

However, the heat-cut glass in which the above-mentioned interlayer film made of the plasticized polyvinyl butyral resin or the like is laminated is expensive, and the multilayer coating is thick, so that the transparency (visible light transmittance) is reduced. Problems such as reduced adhesiveness to the interlayer, peeling or whitening of the interlayer, or impeding the transmission of electromagnetic waves, impairing communication functions such as mobile phones, car navigation systems, garage openers, and automatic cash collection. There was a point.

As a solution to such a problem, for example, JP-B-61-52093 and JP-A-64-36
No. 442 and the like propose a laminated glass in which a metal-deposited polyester film is laminated between plasticized polyvinyl butyral resin sheets. However,
The laminated glass has a problem in the adhesiveness between the plasticized polyvinyl butyral resin sheet and the polyester film, and has problems such as peeling off at the interface and insufficient electromagnetic wave transmission.

Further, laminated glass in which fine particles of a heat-insulating inorganic substance are dispersed in an intermediate film layer for the purpose of imparting heat insulating performance to the intermediate film itself is disclosed in JP-A-8-259279 and JP-A-2000-16481. And so on. In these technologies, infrared rays are blocked by these functional fine particles, and by suppressing the temperature rise of vehicles and buildings,
It can be expected to improve the heat insulation.

However, in the above technique, unless these functional fine particles are uniformly and finely dispersed in the interlayer film, the haze (cloudiness) of the laminated glass increases, and the transparency deteriorates. Therefore, in general, an intermediate film is formed by adding a dispersion liquid in which fine particles are finely dispersed in a plasticizer using a dispersant when kneading the resin.

[0010] However, the dispersant used to disperse the functional fine particles in the plasticizer affects the adhesive force between the glass and the intermediate film, causing peeling and lowering the penetration resistance of the laminated glass. Or by bleeding the dispersant,
There were problems such as a change in adhesive strength over time.

[0011]

SUMMARY OF THE INVENTION In view of the above, the present invention has excellent heat shielding properties, good transparency, does not impair electromagnetic wave transmission, and has good adhesion at the interface between glass and an intermediate film. An object of the present invention is to provide a good interlayer film for laminated glass and a laminated glass using the same.

[0012]

The present invention relates to an interlayer for laminated glass comprising a plasticized polyvinyl acetal resin, wherein the plasticized polyvinyl acetal resin comprises 100 parts by weight of a polyvinyl acetal resin and 30 to 50 parts by weight of a plasticizer. 0.13 to 5.0 parts by weight of zinc oxide particles containing at least one metal element capable of taking a trivalent and / or tetravalent state, and a magnesium salt and / or potassium of a carboxylic acid having 2 to 10 carbon atoms. It is an interlayer film for laminated glass consisting of 10 to 150 ppm of salt. Hereinafter, the present invention will be described in detail.

The polyvinyl acetal resin is composed of a vinyl acetal component, a vinyl alcohol component and a vinyl acetate component. The amount of each of these components is
For example, it can be measured in accordance with JIS K 6728 "Testing method for polyvinyl butyral", infrared absorption spectrum (IR) method and the like.

The polyvinyl alcohol (hereinafter referred to as PVA) used in the polyvinyl acetal resin preferably has an average degree of polymerization of 500 to 5,000. When the average degree of polymerization is less than 500, the penetration resistance of the obtained interlayer film for laminated glass may decrease. When the average degree of polymerization exceeds 5,000, molding of the obtained resin may be difficult, and the strength of the resin film may be too strong, so that the impact absorption and penetration resistance of the obtained interlayer film for laminated glass may be reduced. There is. More preferably, the average polymerization degree is from 1,000 to 2,500.

In the interlayer film for laminated glass of the present invention, it is preferable that the vinyl acetal component of the polyvinyl acetal resin is set to 30 mol% or less. Therefore, the saponification degree of PVA is preferably 70 mol% or more. Used for If the degree of saponification of PVA is less than 70 mol%, the transparency and heat resistance of the obtained polyvinyl acetal resin may decrease, and the reactivity may decrease. Here, the average degree of polymerization and the degree of saponification of PVA can be measured, for example, in accordance with JIS K 6726 “Testing method for polyvinyl alcohol”.

In the interlayer film for laminated glass of the present invention,
The aldehyde used to obtain the polyvinyl acetal resin is not particularly limited.
And aldehydes of 10 to 10 are preferably used. If the carbon number of the aldehyde is less than 3, the moldability of the obtained resin may be insufficient, and if it exceeds 10, the reactivity of acetalization decreases, and the resin blocks during the reaction. And it may be difficult to synthesize the resin.
More preferably, it is an aldehyde having 4 to 8 carbon atoms.

Among them, the polyvinyl acetal resin used as the interlayer film for laminated glass of the present invention is preferably a polyvinyl butyral (hereinafter, referred to as PVB) resin obtained by acetalization with n-butyraldehyde having 4 carbon atoms. . PVB resin is easy to manufacture,
Further, by using the PVB resin, the adhesive strength between the obtained interlayer film for laminated glass and the glass becomes more appropriate. Furthermore,
The obtained interlayer film for laminated glass also has excellent light resistance, weather resistance, and the like.

The method for producing the polyvinyl acetal resin is not particularly limited. For example, PVA is dissolved in warm water, and the obtained aqueous solution is heated to a predetermined temperature, for example, from 0 to 95%.
A method in which the required acid catalyst and aldehyde are added, and the acetalization reaction is completed with stirring, followed by neutralization, washing and drying of the acid catalyst to obtain a powder of a polyvinyl acetal resin. Is adopted.

The plasticized polyvinyl acetal resin used for the interlayer film for laminated glass of the present invention is a polyvinyl acetal resin obtained by plasticizing a plasticizer with a plasticizer.
The plasticizer is not particularly limited. For example, triethylene glycol-di-2-ethylhexanoate (hereinafter referred to as 3GO), oligoethylene glycol-di-
2-ethylhexanoate (hereinafter referred to as NGO), tetraethylene glycol-di-n-heptanoate (hereinafter referred to as 4G7), triethylene glycol-di-2
-Ethyl butyrate (hereinafter referred to as 3GH) and the like. These may be used alone or in combination of two or more.

The above-mentioned 3GO can be obtained by reacting triethylene glycol with 2-ethylhexylic acid in an amount equivalent to twice or more thereof under a catalyst. The NGO can be obtained by reacting oligoethylene glycol with 2-ethylhexylic acid in an amount equivalent to or more than twice the amount thereof in the presence of a catalyst.
The above-mentioned oligoethylene glycol contains 90% by weight or more of ethylene glycol units having 3 to 9 ethylene glycol units, and is commercially available from, for example, Mitsui Toatsu Chemicals, Mitsubishi Chemical, Nisso Chemical, and the like. The above 4G7 can be obtained by reacting tetraethylene glycol with n-heptanoic acid in an amount equivalent to or more than twice the amount thereof under a catalyst. Further, the above 3GH can be obtained by reacting triethylene glycol with 2-ethylbutyric acid in an amount equivalent to or more than twice the amount thereof in the presence of a catalyst.

When the amount of the plasticizer is less than 30 parts by weight based on 100 parts by weight of the polyvinyl acetal resin, the resulting interlayer film for laminated glass has reduced impact resistance. If it exceeds 50 parts by weight, the plasticizer bleeds out and the adhesive strength decreases.

The interlayer film for laminated glass of the present invention comprises a trivalent and / or a tetravalent resin in the plasticized polyvinyl acetal resin.
Oxide particles containing one or more metal elements capable of taking a valence (hereinafter, referred to as metal-doped zinc oxide) 0.13 to 5.0
Parts by weight and 10 to 150 ppm of a magnesium salt and / or potassium salt of a carboxylic acid having 2 to 10 carbon atoms are dispersed therein. By dispersing the metal-doped zinc oxide in the film, the obtained interlayer film for laminated glass has excellent heat shielding properties.

In the metal-doped zinc oxide, the metal element capable of being trivalent and / or tetravalent is not particularly limited. For example, B, Al, Ga, In, Tl, C, Si,
Ge, Sn, Pb, Sc, Y, Ti, Zr, Hf, V,
Nb, Ta, Cr, Mo, W, Mn, Tc, Re, F
e, Ru, Os, Rh, Ir, La, Ce, Sb and the like. These may be contained in one or more zinc oxide particles.

In the interlayer film for laminated glass of the present invention,
When the content of the metal-doped zinc oxide is less than 0.13 parts by weight with respect to 100 parts by weight of the polyvinyl acetal resin, the obtained interlayer film for laminated glass is less likely to have an infrared shielding effect, and has a poor heat shielding property. descend. 5.0
If the amount is more than 10 parts by weight, the transmittance of visible light of the obtained interlayer film for laminated glass decreases. Preferably, 0.13-
3.0 parts by weight.

In the interlayer film for laminated glass of the present invention,
The magnesium salt and the potassium salt of the carboxylic acid having 2 to 10 carbon atoms function as an adhesion regulator. The magnesium salt of a carboxylic acid having 2 to 10 carbon atoms is not particularly limited, for example, magnesium acetate,
Examples include magnesium propanoate, magnesium butanoate, magnesium pentanoate, magnesium hexanoate, magnesium 2-ethylbutyrate, magnesium heptanoate, magnesium octanoate, and magnesium 2-ethylhexylate. The potassium salt of the carboxylic acid having 2 to 10 carbon atoms is not particularly limited, and includes, for example, potassium acetate, potassium propanoate, potassium butanoate, potassium pentanoate, potassium hexanoate, potassium 2-ethylbutyrate, potassium heptanoate, Potassium octoate, 2
-Potassium ethylhexylate. These may be used alone or in combination of two or more, but preferably used in combination of two or more. The above salt is 2
By using more than one kind, the adhesive force can be adjusted with a small amount.

When the content of the magnesium salt and / or potassium salt of the carboxylic acid having 2 to 10 carbon atoms is 10 ppm
If it is less than 3, it becomes impossible to adjust the adhesive strength of the obtained interlayer film for laminated glass. If it exceeds 150 ppm, the moisture resistance and transparency of the obtained interlayer film for laminated glass will be reduced.

In the interlayer film for laminated glass of the present invention, it is preferable that the metal-doped zinc oxide is uniformly dispersed in the plasticized polyvinyl acetal resin.
By uniformly dispersing the metal-doped zinc oxide in the film, the heat shielding property of the obtained interlayer film for laminated glass is high throughout the film.

The method for dispersing the metal-doped zinc oxide in the plasticized polyvinyl acetal resin is not particularly limited, but it is preferable to add a dispersion in which the metal-doped zinc oxide is dispersed in an organic solvent using a dispersant. preferable. According to the above method, the metal-doped zinc oxide is uniformly dispersed in the film.

The metal-doped zinc oxide dispersed in the organic solvent preferably has a particle size of 0.2 μm or less. When the particle size exceeds 0.2 μm, scattering of visible light by the particles becomes remarkable, and the transparency of the obtained interlayer film for laminated glass may be impaired.

The dispersant is preferably one or more compounds selected from the group consisting of polyvinyl acetal resin, carboxyl-modified silicone oil and amine-modified silicone oil. As the organic solvent for dispersing the metal-doped zinc oxide, an organic solvent having good compatibility with a dispersant such as polyvinyl acetal resin, carboxyl-modified silicone oil and amine-modified silicone oil is used, and a plasticizer and the like are preferable.

The polyvinyl acetal resin used as a dispersant is not particularly limited, and those produced by the above-described method for producing a polyvinyl acetal resin can be used. Further, the polyvinyl acetal resin used as a dispersant preferably has a degree of polymerization of 100 to 5,000. If the degree of polymerization is less than 100, a sufficient dispersing effect may not be obtained. If it exceeds 5,000, the compatibility with the organic solvent is deteriorated, so that it may not act as a dispersant. Further, the content of the vinyl component to which the hydroxyl group is bonded in the polyvinyl acetal resin is preferably 20 to 80 mol%. If the content of the vinyl component to which the hydroxyl group is bonded is less than 20 mol%, the ability to disperse the metal-doped zinc oxide may be insufficient.
If it exceeds 80 mol%, the solubility in the organic solvent decreases,
The preparation of the dispersion may be difficult.

The amount of the polyvinyl acetal resin used as a dispersing agent is 100
It is preferably at least 1 part by weight based on parts by weight. 1
If the amount is less than parts by weight, a sufficient dispersing effect may not be obtained.

The carboxy-modified silicone oil and amine-modified silicone oil are not particularly limited.
For example, generally a pale yellow transparent viscous liquid obtained by reacting a polysiloxane with a compound having a carboxyl group or an amine group, etc.
More than one species is preferably used. Further, the carboxy-modified silicone oil and the amine-modified silicone oil,
In order to improve the compatibility with the plasticizer used in the above-mentioned plasticized polyvinyl acetal resin, it is preferable that the modification rate is appropriately adjusted.

The amount of the carboxy-modified silicone oil and / or amine-modified silicone oil to be added is not particularly limited, and is 0.5 parts by weight or more based on 100 parts by weight of the metal-doped zinc oxide, and is a plasticized polyvinyl acetal. It is preferably 0.5 part by weight or less based on 100 parts by weight of polyvinyl acetal resin which is a main component of the resin. If the amount of the carboxy-modified silicone oil and / or the amine-modified silicone oil is less than 0.5 part by weight with respect to 100 parts by weight of the metal-doped zinc oxide, a sufficient dispersing effect may not be obtained. When the addition amount of the carboxy-modified silicone oil and / or amine-modified silicone oil exceeds 0.5 parts by weight based on 100 parts by weight of the polyvinyl acetal resin, the adhesive strength between the obtained interlayer film for laminated glass and glass changes with time. Sometimes.

In the interlayer film for laminated glass of the present invention,
The method of dispersing the metal-doped zinc oxide in an organic solvent is not particularly limited, but a mixture of an organic solvent, a dispersant, and a metal-doped zinc oxide, which is generally used for dispersing or blending a coating material, such as a sand mill, a ball mill, a homogenizer, and an atomizer. It can be dispersed by a device such as a lighter, a high-speed rotary stirring device, and an ultrasonic dispersion device.

The dispersion obtained by dispersing the metal-doped zinc oxide obtained by the above-mentioned method is prepared so that the ratio of the metal-doped zinc oxide contained in the interlayer film for laminated glass is within the above range. May be added directly to the plasticizer, or may be added in advance to the plasticizer and then mixed with the polyvinyl acetal resin.

The interlayer film for laminated glass of the present invention may further contain, if necessary, an ultraviolet absorber, a light stabilizer, an antioxidant,
One or more known additives generally used in an interlayer film for laminated glass, such as a surfactant and a colorant, may be contained.

The ultraviolet absorber is not particularly restricted but includes, for example, benzotriazole-based products such as "Tinuvin P", "Tinuvin 320", "Tinuvin 326" and "Tinuvin 328" (trade names, manufactured by Ciba Geigy). No. These may be used alone or in combination of two or more.

The light stabilizer is not particularly limited, and may be, for example, a trade name “ADEGASTAB LA-5” manufactured by Asahi Denka Kogyo.
7 "and the like. These may be used alone or in combination of two or more.

The antioxidant is not particularly limited.
For example, the product name “Sumilyzer BH” manufactured by Sumitomo Chemical Co., Ltd.
T ”, trade name“ Irganox 10 ”manufactured by Ciba Geigy
And phenolic compounds such as "10". These may be used alone or in combination of two or more.

The above surfactant is not particularly limited.
For example, sodium lauryl sulfate, sodium alkylbenzene sulfonate and the like can be mentioned. These may be used alone or in combination of two or more.

The method for forming the interlayer film for laminated glass of the present invention is not particularly limited, and examples thereof include the polyvinyl acetal resin, a plasticizer, a magnesium salt and / or a potassium salt of a carboxylic acid having 2 to 10 carbon atoms, and a metal. Each predetermined amount of the doped zinc oxide and the above-mentioned various additives to be added as necessary are blended, and after uniformly kneading the mixture, a sheet is formed by an extrusion method, a calendar method, a pressing method, a casting method, an inflation method, or the like. And an intermediate film for laminated glass.

In the interlayer film for laminated glass of the present invention,
The film made of the plasticized polyvinyl acetal resin may be used as an intermediate film for laminated glass in a single layer, or may be used in a state where two or more sheets are laminated.

The total thickness of the interlayer film for laminated glass of the present invention is not particularly limited, but practically, considering the minimum penetration resistance and weather resistance required for laminated glass, practically, It is preferably 0.3 to 0.8 mm.

Since the interlayer film for laminated glass of the present invention has the above-mentioned structure, it is excellent in transparency, heat shielding property, electromagnetic wave transmission property, light resistance and the like, and has good adjustment of adhesive strength with glass. It is. The present invention 2 has the interlayer film for laminated glass of the present invention 1 interposed between at least a pair of glass plates,
It is a laminated glass that is integrated.

The laminated glass of the present invention 2 has a wavelength of 380-380.
Visible light transmittance Tv at 780 nm, 340 to 1800 n
m, solar transmittance Ts, haze H, 10 to 2000 MH
The electromagnetic wave shielding performance ΔdB and the Pummel value P at z
It is preferable that the following conditions are satisfied. Tv ≧ 75% Ts ≦ 60% H ≦ 1.0% ΔdB ≦ 2dB P = 3-7 When the above Tv is less than 75%, the transparency of the laminated glass is low, which is not preferable in practical use. Ts is 60
%, The heat insulation of the laminated glass is not sufficient. If the H exceeds 1.0%, the transparency of the laminated glass is low, which is not preferable for practical use. The above ΔdB is 2 dB
If it exceeds, the electromagnetic wave transmittance becomes insufficient. If the value of P is outside the above range, the adhesion between the interlayer film for laminated glass and the glass is not within an appropriate range, so that peeling of the interlayer film may occur.

The method for producing the laminated glass of the present invention 2 is not particularly limited. For example, an interlayer film for a laminated glass of the present invention 1 is sandwiched between two transparent glass plates, and this is placed in a rubber bag and decompressed. The pre-bonding is performed at a temperature of about 70 to 110 ° C. with suction, and then the main bonding is performed using an autoclave at a temperature of about 120 to 150 ° C. and a pressure of about 1 to 1.5 MPa to obtain a desired laminated glass. Can be obtained.

The glass plate is not particularly limited, and may be, for example, a float glass, a polished glass, a template glass,
Various inorganic glass plates, such as a netted glass, a lined glass, and a colored plate glass, may be used. These may be used alone or in combination of two or more.

The interlayer film for laminated glass of the present invention may be sandwiched by an organic glass other than the inorganic glass, that is, a transparent member having high rigidity. Examples of the transparent body include those made of a polycarbonate resin.

[0050]

The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.

Example 1 (Synthesis of PVB resin) An average degree of polymerization of 1
700 and 275 g of PVA having a saponification degree of 99.2 mol% were added and dissolved by heating. The temperature of the reaction system was adjusted to 15 ° C., 201 g of 35% by weight hydrochloric acid and 157 g of n-butyraldehyde were added, and the temperature was maintained to precipitate a reaction product. Thereafter, the reaction system was maintained at a temperature of 60 ° C. for 3 hours to complete the reaction, washed with excess water to wash away unreacted n-butyraldehyde, and neutralized the hydrochloric acid catalyst with an aqueous sodium hydroxide solution. Further, after washing with excess water for 2 hours, drying was performed to obtain a white powdery PVB resin. The average degree of butyralization of the obtained PVB resin was 68.5 mol%.

(Preparation of Dispersion) Zinc oxide powder doped with 5 mol% of indium with respect to zinc so as to be 10% by weight in 3GO was charged, and at the same time, an average polymerization degree of 1700 and a saponification degree of 99.2 were used as dispersants. A PVB powder having an average degree of butyralization of 65.3 mol% synthesized from PVA of 5 mol% was mixed with 5 parts by weight of indium-doped zinc oxide in an amount of 5 parts by weight.
The mixture was charged into an attritor so as to be 0 parts by weight, and dispersed for 10 hours to prepare a dispersion.

(Production of interlayer film for laminated glass) 39 parts by weight of 3GO in which 1.0 part by weight of indium-doped zinc oxide was dispersed, 20 parts by weight of magnesium acetate and 20 ppm by weight of 100 parts by weight of the PVB resin obtained above. After adding 40 ppm of magnesium ethyl butyrate and sufficiently melting and kneading with a mixing roll, the mixture was press-formed at 150 ° C. for 30 minutes using a press-forming machine to obtain an interlayer film for laminated glass having an average film thickness of 0.76 mm.

(Manufacture of laminated glass) The interlayer film for laminated glass obtained above was sandwiched from both ends with a transparent float glass (30 cm × 30 cm × 3 mm in thickness), and this was placed in a rubber bag and placed in a rubber bag. After degassing at a degree of vacuum of 0.7 kPa for 20 minutes, the substrate was transferred to an oven while being degassed, and further vacuum-pressed while being held at 90 ° C. for 30 minutes. The thus preliminarily bonded laminated glass was heated and pressed in an autoclave at 135 ° C. and a pressure of 1.2 MPa for 20 minutes to perform final bonding, thereby obtaining a laminated glass. Using the obtained laminated glass, evaluation was performed by the following evaluation method. Table 2 shows the evaluation results.

Evaluation method (1) Optical characteristics The transmittance of the laminated glass at 340 to 1800 nm was measured using a spectrophotometer (UV3100, manufactured by Shimadzu Corporation), and the results were measured according to JIS Z 8722, JIS R 3106 and JIS Z 8701. 380-780 nm according to
, A solar light transmittance Ts of 340 to 1800 nm was determined.

(2) Haze H Measured according to JIS K 6714. (3) Electromagnetic wave permeability According to the KEC method measurement (electromagnetic wave shielding effect test),
The reflection loss value (dB) of 10 to 2000 MHz was compared with a normal float glass single plate having a thickness of 3 mm. The maximum value of the difference at the above frequency was evaluated as ΔdBmax.

(4) Pummel Value The adhesion of the interlayer film for laminated glass to glass was evaluated by the Pummel value. The details of the test method are as follows. The laminated glass is brought to a temperature of -1.8 ± 0.6 ° C.
The glass was adjusted by leaving it for a period of time, and the head was hammered with a hammer of 0.45 kg and ground until the particle diameter of the glass became 6 mm or less. Next, the degree of exposure of the interlayer film after the glass was partially peeled was determined using a preliminarily graded limit sample, and the result was expressed as a Pummel value according to the criteria shown in Table 1. The higher the Pummel value, the higher the adhesion between the interlayer and the glass, and the lower the Pummel value, the lower the adhesion between the interlayer and the glass.

[0058]

[Table 1]

(5) Peeling After Moisture Resistance Test The laminated glass was left in an atmosphere of 80 ° C. and a relative humidity of 95% for 2 weeks, and immediately after being taken out, the peeled state of the edge of the laminated glass was observed.

Example 2 In the production of an interlayer film for laminated glass, zinc oxide doped with aluminum in a molar ratio of 4% to zinc and tin in the same manner as 1.5% instead of 1.0 part by weight of indium-doped zinc oxide. Example 1 except that 1.0 part by weight was used.
A laminated glass was produced in the same manner as described above. In addition, evaluation was performed using the laminated glass according to the evaluation method described above.
Table 2 shows the evaluation results.

Example 3 A laminated glass was produced in the same manner as in Example 1 except that the amount of indium-doped zinc oxide was changed to 0.14 parts by weight in the production of the interlayer film for laminated glass. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

Example 4 In the production of an interlayer film for laminated glass, except that the addition amount of indium-doped zinc oxide was 2.8 parts by weight.
A laminated glass was produced in the same manner as in Example 1. Also,
This laminated glass was evaluated by the above-described evaluation method. Table 2 shows the evaluation results.

Example 5 In the preparation of an additive dispersion, PVB powder 5 was used as a dispersant with respect to 100 parts by weight of indium-doped zinc oxide.
A laminated glass was produced in the same manner as in Example 1, except that 10 parts by weight of the carboxy-modified silicone oil was used instead of 0 parts by weight. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

Comparative Example 1 A laminated glass was produced in the same manner as in Example 1, except that indium-doped zinc oxide was not added in the production of the interlayer film for laminated glass. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

Comparative Example 2 In the production of the interlayer film for laminated glass, the procedure of Example 1 was repeated except that no indium-doped zinc oxide was added and that instead of the transparent float glass, a glass on which zinc oxide was deposited was used. In the same manner as in Example 1, a laminated glass was produced. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

Comparative Example 3 In the production of an interlayer film for laminated glass, an interlayer film having a thickness of 0.38 mm was produced without adding indium-doped zinc oxide. A laminated glass was prepared by using a 50 μm-thick polyester film having tin-doped indium oxide deposited between the two intermediate films as an intermediate film for laminated glass. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

Comparative Example 4 A laminated glass was produced in the same manner as in Example 1 except that the amount of indium-doped zinc oxide was changed to 0.03 parts by weight in the production of the interlayer film for laminated glass. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

Comparative Example 5 In the production of an interlayer film for laminated glass, except that the addition amount of indium-doped zinc oxide was 5.5 parts by weight.
The same operation as in Example 1 was performed to produce a laminated glass. In addition, evaluation was performed using the laminated glass according to the evaluation method described above. Table 2 shows the evaluation results.

[0069]

[Table 2]

From Table 2, it can be seen that the laminated glass using the interlayer film for laminated glass obtained in Examples 1 to 5 has excellent transparency such as visible light transmittance and haze, heat shielding property, electromagnetic wave transmitting property, and the like.
The adhesiveness and weather resistance were also excellent. In contrast, the laminated glass of Comparative Example 1 in which no metal-doped zinc oxide was used had poor electromagnetic wave transmission. The laminated glass of Comparative Example 2 using a glass on which tin-doped indium oxide was deposited was inferior in electromagnetic wave transmission, adhesion, and moisture resistance. The laminated glass of Comparative Example 3 using a polyester film having a thickness of 50 μm on which tin-doped zinc oxide was deposited was inferior in electromagnetic wave transmission and moisture resistance. The laminated glass of Comparative Example 4 in which the addition amount of the metal-doped zinc oxide was less than 0.13 parts by weight was inferior in electromagnetic wave transmission. Further, the laminated glass of Comparative Example 5 in which the addition amount of the metal-doped zinc oxide exceeded 5.0 parts by weight was inferior in transparency such as visible light transmittance and haze.

[0071]

Since the interlayer film for laminated glass of the present invention has the above-mentioned structure, it is excellent in transparency, weather resistance, penetration resistance, heat shielding property, electromagnetic wave transmission property and adhesion to glass. Demonstrates excellent performance. Therefore, the laminated glass using the interlayer film for laminated glass of the present invention is suitably used as a window glass of a vehicle, a building, or the like.

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI theme coat ゛ (Reference) C08K 5/00 C08K 5/00 5/09 5/09 C08L 29/14 C08L 29/14 83/06 83 / 06 83/08 83/08 F term (reference) 4F071 AA30 AA51 AA67 AB06 AB08 AB09 AB10 AB18 AC09 AE04 AF07Y AF29Y AF30 AH19 BC01 BC02 BC09 BC17 4G061 AA04 AA29 BA01 BA02 CB12 CB16 CB18 CD02 CD03 CD18 4J05 BE06X BE05X06 CH05X06 DA088 DA098 DA108 DE107 EG029 EG039 EH046 FB077 FD02X FD02Y FD026 FD040 GP00 HA05

Claims (5)

[Claims] 1. An interlayer film for laminated glass comprising a plasticized polyvinyl acetal resin, wherein the plasticized polyvinyl acetal resin is a polyvinyl acetal resin.
Parts by weight, 30 to 50 parts by weight of a plasticizer, 0.13 to 5.0 parts by weight of zinc oxide particles containing one or more metal elements capable of taking a trivalent and / or tetravalent form, and 2 to 10 carbon atoms. Magnesium and / or potassium salts of carboxylic acids
An interlayer for laminated glass, comprising 150 ppm. 2. The plasticized polyvinyl acetal resin comprises 3
2. A laminated glass according to claim 1, wherein a dispersion is prepared by dispersing zinc oxide particles containing at least one metal element capable of valency and / or tetravalence in an organic solvent with a dispersant. For intermediate film. 3. The dispersant is a polyvinyl acetal resin,
3. The interlayer for laminated glass according to claim 2, wherein the interlayer is at least one compound selected from the group consisting of a carboxyl-modified silicone oil and an amine-modified silicone oil. 4. An interlayer film for laminated glass according to claim 1, interposed between at least a pair of glass plates,
Laminated glass characterized by being integrated. 5. The visible light transmittance Tv at a wavelength of 380 to 780 nm, the solar transmittance Ts at 340 to 1800 nm, the haze H, the electromagnetic wave shielding performance ΔdB at 10 to 2000 MHz and the Pummel value P satisfy the following conditions. The laminated glass according to claim 4, characterized in that: Tv ≧ 75% Ts ≦ 60% H ≦ 1.0% ΔdB ≦ 2dB P = 3-7