JP2000103653A - Composition for interlayer, interlayer for laminated glass and laminated glass - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a composition for interlayer membrane that is suitable for obtaining the interlayer membrane that can hold the adhesion between the interlayer membrane and the glass within proper range in both cases, at the beginning and after passage of time, the interlayer membrane for laminated glass that is produced by using the same and laminated glass produced by using the interlayer membrane. SOLUTION: This composition for interlayer membrane comprises 100 pts.wt. of poly(vinyl butyral) and 20-60 pts.wt. of triethylene glycol di-(2-ethyl-hexanoate) and is prepared by dissolving 8 pts.wt. of the poly(vinyl butyral) to 100 pts.wt. of triethylene glycol 2-ethylhexanoate and has the cloud point of 90-130 deg.C. The interlayer membrane for laminated glass is prepared by forming the composition to a membrane. The laminated glass is prepared by intervening the interlayer membrane between at least two plates of glass and integrating them.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a composition for an interlayer film for laminated glass, an interlayer film for laminated glass produced using the composition, and a laminated film produced using the intermediate film. About glass.

[0002]

2. Description of the Related Art Conventionally, laminated glass has been widely used for windshields and side glasses of automobiles, window glasses of buildings, and the like. As a typical example of the laminated glass, an interlayer film for a laminated glass obtained by forming a polyvinyl butyral resin (composition for an interlayer film) plasticized by a plasticizer is interposed between at least two sheets of glass. And those manufactured integrally.

[0003] In such a laminated glass, when an impact is applied thereto, the glass is broken, but the interlayer film interposed between the glass is not easily broken, and the glass is adhered to the interlayer film even after the glass is broken. Since it is still worn, the shards are less likely to scatter, and thus have the function of preventing the human body inside the car or building from being injured by the shards of glass.

It is important that the composition for an interlayer used for producing the interlayer film for laminated glass has excellent compatibility between a polyvinyl butyral resin and a plasticizer.

[0005] The compatibility between a polyvinyl butyral resin and a plasticizer largely depends on the degree of butyralization of the polyvinyl butyral resin, the type of plasticizer, and the like. The plasticizer bleeds out on the surface of the film, resulting in poor blocking resistance during storage and transportation of the interlayer, and whitening of the interlayer caused by moisture absorption, making it impossible to obtain laminated glass with excellent performance. Occurs.

[0006] Conventionally, the evaluation of the compatibility between the polyvinyl butyral resin and the plasticizer is described in, for example, JP-A-56-364.
As disclosed in Examples of JP-A No. 32, "A resin composition comprising a polyvinyl butyral resin and a plasticizer is first formed into a film, and then the presence or absence of bleed-out of the plasticizer on the surface of the film. Or the presence or absence of a whitening phenomenon of the film, etc. ".

However, in the above-mentioned conventional evaluation method, since the resin composition must be formed into a film in advance, the amount of the polyvinyl butyral resin and the plasticizer used in the evaluation is increased, There is a problem that it takes a lot of time, and it cannot be said that it is a simple evaluation method.

When a laminated glass is manufactured using an interlayer film for a laminated glass, a portion (trim portion) of the interlayer film protruding from an end portion of the laminated glass is generated. When a plasticizer having a relatively low boiling point as described above is used, the plasticizer evaporates from the trim portion, and the trim portion becomes hard, resulting in a problem that the removability by trim cutting (trim cutting property) deteriorates.

Further, in general, in order to sufficiently exhibit the function as a laminated glass, the higher the adhesive strength between the interlayer film and the glass, the better it is not. It is necessary to adjust.

The above-mentioned adjustment of the adhesive force within an appropriate range is necessary, for example, in a car accident or the like, in order to absorb a shock or prevent penetration when a driver or a passenger collides with the glass. In a building, it is necessary to prevent penetration of a flying object from outside and to prevent scattering of glass.

That is, if the adhesive strength between the intermediate film and the glass is too small, the glass is peeled off from the intermediate film, and the fragments are easily scattered. If the force is too large, the glass and the intermediate film are simultaneously damaged, and a problem occurs that a human body or a flying object from the outside easily penetrates.

On the other hand, when the adhesive strength between the interlayer and the glass is within an appropriate range, the glass is damaged over a wide range and the glass is damaged, and at the same time, the partial interface between the interlayer and the glass is broken. Since a phenomenon occurs in which separation occurs and the intermediate film is stretched, the effect of absorbing shock and the effect of preventing penetration are increased.

[0013] In view of the above, various types of adhesive force modifiers for interlayer films have been conventionally studied in order to adjust the adhesive force between the interlayer film and glass within an appropriate range.

For example, in Japanese Patent Publication No. 48-5772, "In a glass obtained by laminating at least two pieces of glass with a plasticized polyvinyl acetal resin composition, the plasticized polyvinyl acetal resin composition contains 10 to 10 carbon atoms.
No. 22 ", a laminated glass characterized by containing a sodium metal salt of an aliphatic carboxylic acid.

However, in the laminated glass according to the above disclosure, since a metal salt of a carboxylic acid having a relatively large number of carbon atoms is used as an adhesive force adjusting agent, the adhesive force between the intermediate film and the glass changes over time (elapsed time). There is a problem that. That is, even if the initial adhesive strength is appropriate, the adhesive strength gradually decreases or increases with the passage of time, so that the glass is easily peeled when receiving an impact, or hardly peeled off.
In order to prevent this change in the adhesive force, the intermediate film may be
It is necessary to store and ripen in an atmosphere of 0 to 50 ° C. for 1 to 2 months, but since the interlayer has adhesiveness and self-adhesiveness, it can be stored for a long time in the above atmosphere. In practice, it is difficult, and even if aging is performed, the change with time of the adhesive force can be suppressed but cannot be eliminated completely, and the above-mentioned problem still remains.

[0016]

SUMMARY OF THE INVENTION The present invention solves the above-mentioned conventional problems by evaluating the compatibility between a polyvinyl butyral resin and a plasticizer in advance by a simple method, and It is possible to prevent the occurrence of bleed-out of the plasticizer, a decrease in the blocking resistance of the interlayer film, and the occurrence of a whitening phenomenon due to the moisture absorption of the interlayer film. An interlayer film composition suitable for obtaining an interlayer film for laminated glass in which the adhesive force with glass is maintained within an appropriate range both at the initial stage and after aging, and for a laminated glass produced using the composition. An object of the present invention is to provide an interlayer film and a laminated glass manufactured using the interlayer film.

[0017]

The composition for an interlayer according to the invention described in claim 1 (hereinafter referred to as "first invention") is based on 100 parts by weight of polyvinyl butyral resin and triethylene glycol di-2-amine. Ethyl hexanoate 20
And a solution obtained by dissolving 8 parts by weight of the polyvinyl butyral resin with respect to 100 parts by weight of the triethylene glycol di-2-ethylhexanoate has a cloud point of 90 to 130 ° C. It is characterized by being.

The composition for an intermediate film according to the second aspect of the invention (hereinafter referred to as "second invention") has an average degree of butyralization of a polyvinyl butyral resin in the composition for an intermediate film according to the first aspect. 65 to 72 mol%.

The composition for an intermediate film according to the invention described in claim 3 (hereinafter referred to as "third invention") is the same as the composition for an intermediate film according to the first invention or the second invention, but has 2 to 2 carbon atoms.
It is characterized by containing a magnesium salt of 10 carboxylic acids.

The invention according to claim 4 (hereinafter referred to as “fourth
The interlayer film for laminated glass according to the present invention is characterized in that the composition for an interlayer film according to any one of the first to third inventions is formed.

Further, the invention according to claim 5 (hereinafter referred to as "the invention")
The laminated glass according to the "fifth invention" is characterized in that the interlayer film for a laminated glass according to the fourth invention is interposed between at least a pair of glasses and integrated.

The polyvinyl butyral resin (hereinafter referred to as “P”) contained as a main component in the composition for an intermediate film according to the first invention.
VB ") is not particularly limited, and examples thereof include polyvinyl alcohol (hereinafter, referred to as polyvinyl alcohol).
"PVA") is dissolved in warm water, and the resulting aqueous solution is kept at a predetermined temperature, for example, 0 to 95 ° C., an acid catalyst and butyraldehyde are added, and the butyralization reaction is allowed to proceed with stirring. Then, the reaction is completed by raising the reaction temperature and aging, and thereafter, a so-called precipitation method or the like, in which neutralization, washing and drying are performed to obtain a PVB powder, is preferably employed.

The average degree of polymerization of PVA used for the production of PVB is not particularly limited, but is 500 to 500.
It is preferably 3000, more preferably 100
0 to 2500. When the average degree of polymerization of PVA is less than 500, the penetration resistance of the obtained laminated glass may be insufficient. Conversely, when the average degree of polymerization of PVA exceeds 3000, the production of the interlayer becomes difficult. There is. or,
The saponification degree of the PVA is not particularly limited, but is preferably 70 mol% or more. If the degree of saponification of PVA is less than 70 mol%, the resulting interlayer film or laminated glass may have insufficient transparency, heat resistance, and the like.

The average degree of polymerization and the degree of saponification of the PVA can be measured according to JIS K-6726 "Testing method for polyvinyl alcohol".

The average degree of butyralization of the PVB obtained above is not particularly limited, but is preferably 40 to 75 mol%, more preferably 65 to 72 mol%.

If the average degree of butyralization of the PVB is less than 40 mol%, the compatibility with triethylene glycol di-2-ethylhexanoate used as a plasticizer may be deteriorated. Those having a butyralization degree of more than 75 mol% are not preferred because the process of producing PVB may take a very long time.

The average degree of butyralization of PVB is as follows:
It can be measured in accordance with JIS K-6728 "Polyvinyl butyral test method".

Triethylene glycol di-2-ethylhexanoate (hereinafter referred to as “3GO”) contained as a plasticizer in the composition for an intermediate film according to the first invention is a mixture of triethylene glycol and 2-ethylhexanoic acid. It can be manufactured as a raw material. Specifically, for example, 2-ethylhexanoic acid 2 to 2 moles of triethylene glycol is used.
2.5 mol was added, and if necessary, sulfuric acid, hydrochloric acid,
A catalyst such as an inorganic acid such as phosphoric acid or an organic acid such as p-toluenesulfonic acid or methanesulfonic acid may be used in an amount of 0.01 to 5% of the total reactants.
The desired 3GO can be obtained by adding ester by weight and performing an esterification reaction. The esterification reaction may be performed by diluting the reaction system with an organic solvent such as toluene or xylene, or may be performed using 2-ethylhexanoic acid itself as a catalyst, or may be performed at normal temperature and normal pressure. However, considering the promotion of the reaction and the removal of generated water, etc., 50 to 300
It is preferable to carry out the reaction under heating at about ° C.

Since the 3GO obtained above has a relatively high boiling point (219 ° C./5 mmHg), evaporation during the production of the interlayer film and evaporation from the trim portion after forming the laminated glass are small, so that good workability is obtained. And excellent trim cut properties can be obtained. It also has the advantage of being excellent in hydrolysis resistance.

In the composition for an intermediate film according to the first invention, 3GO20 to 3GO20 to 100 parts by weight of the PBV is used.
It is necessary to contain 60 parts by weight.

If the content of 3GO relative to 100 parts by weight of PVB is less than 20 parts by weight, the resulting laminated glass will have insufficient penetration resistance, and if the content of 3GO relative to 100 parts by weight of PVB exceeds 60 parts by weight. 3) The bleed-out phenomenon of 3GO occurs, and the transparency of the interlayer film and the laminated glass deteriorates.

In the first invention, a solution obtained by dissolving 8 parts by weight of the PVB in 100 parts by weight of the above 3GO (hereinafter referred to as “PVB-3GO solution”) has a cloud point of 9%.
It needs to be 0 to 130 ° C.

The cloud point of the PVB-3GO solution is defined as
It is a cloud point measured in accordance with IS K-2269 “Pour point of crude oil and petroleum products and cloud point test method of petroleum products”. Specifically, after heating a PVB-3GO solution to 150 ° C. or more, It means the temperature at which clouding begins to occur in a part of the solution when the temperature is lowered by leaving it in an atmosphere of 10 to 30 ° C.

As a method of measuring the temperature (cloud point) at which clouding begins to occur in a part of the solution, for example, a method of visually observing the appearance of the solution, a method of measuring the haze of the solution with a haze meter, For example, there is a method in which a limit sample of a plurality of stages is prepared, and clouding is determined in comparison with the limit sample.

The above cloud point of the PVB-3GO solution is 90 ° C.
If it is less than 3, the plasticizing effect of 3GO on PVB will be too large, and the blocking resistance of the obtained interlayer film will be reduced, and the mechanical properties and penetration resistance of the obtained laminated glass will be insufficient. .

Conversely, the above cloud point of the PVB-3GO solution is 1
When the temperature exceeds 30 ° C., the compatibility between PVB and 3GO becomes poor, and the bleed-out phenomenon of 3GO on the surface of the obtained intermediate film becomes extremely intense, resulting in lack of practicality.

Next, the composition for an intermediate film according to the second invention is
In the composition for an intermediate film according to the first invention described above, PV
B has an average degree of butyralization of 65 to 72 mol%.

If the average degree of butyralization of PVB is less than 65 mol%, the compatibility between PVB and 3GO becomes insufficient, and the bleed-out phenomenon of 3GO tends to occur when an intermediate film is formed. When PVB has an average degree of butyralization of more than 72 mol%, the process for producing PVB takes a long time, which is not economically preferable.

Next, the composition for an intermediate film according to the third invention is
The composition for an intermediate film according to the first invention or the second invention, wherein a magnesium salt of a carboxylic acid having 2 to 10 carbon atoms is contained as an adhesion regulator.

By containing the magnesium salt of a carboxylic acid having 2 to 10 carbon atoms in the composition for an intermediate film, the adhesive strength between the obtained intermediate film and the glass is within an appropriate range both in the initial stage and after the elapse of time. Thus, it is possible to obtain a laminated glass having excellent shock absorption and penetration resistance.

The magnesium salt of a carboxylic acid having 2 to 10 carbon atoms is not particularly limited. For example, formic acid, acetic acid, propionic acid, butyric acid, pentanoic acid,
Examples thereof include magnesium salts such as 2-ethylbutanoic acid, heptanoic acid, octanoic acid, and 2-ethylhexanoic acid, which are preferably used. Among them, magnesium acetate, magnesium propionate, magnesium 2-ethylbutanoate,
-Magnesium ethylhexanoate and the like are more preferably used.

The magnesium salts of carboxylic acids having 2 to 10 carbon atoms may be used alone or in combination of two or more.

C 2 to C 10 in the intermediate film composition
The content of the magnesium salt of the carboxylic acid is not particularly limited, but is preferably 0.01 to 0.5 part by weight, more preferably 0.02 part by weight, based on 100 parts by weight of PVB. ０．２0.2 parts by weight.

If the content of the magnesium salt is less than 0.01 part by weight with respect to 100 parts by weight of PVB, a sufficient adhesive force adjusting effect may not be obtained.
The content of the magnesium salt is 0. 00 parts by weight.
If the amount exceeds 5 parts by weight, the adhesive strength of the obtained interlayer film to glass may be too low, or water resistance and transparency may be impaired.

In the composition for an intermediate film according to the first to third inventions, PVB, 3GO and C2-C2 which are essential components are contained.
In addition to the magnesium salt of the carboxylic acid of 10, a plasticizer other than 3GO, an adhesion regulator other than the magnesium salt of the carboxylic acid having 2 to 10 carbon atoms, an ultraviolet absorber, a light stabilizer, an antioxidant, a surfactant, One or more of various additives generally used in interlayer films for laminated glass, such as inorganic fillers such as finely divided silica and coloring agents, may be contained.

Examples of the plasticizer other than 3GO include, but are not particularly limited to, triethylene glycol-di-2-ethylbutyrate (3GH), triethylene glycol-di-n-heptanoate (3G7), and the like. Triethylene glycol dicaprylate, triethylene glycol di-n-octoate, tetraethylene glycol di-2-ethyl butyrate (4GH), tetraethylene glycol di-2-ethylhexanoate (4
GO), tetraethylene glycol-di-n-heptanoate (4G7), dihexyl adipate (DHA),
Examples thereof include dibenzyl phthalate, and one or more of these are suitably used.

The adhesion regulator other than the magnesium salt of a carboxylic acid having 2 to 10 carbon atoms is not particularly limited. For example, a metal salt of a carboxylic acid such as a potassium salt or a sodium salt of the carboxylic acid is used. Modified silicone oils such as salts, ether-modified silicone oils, ester-modified silicone oils, epoxy-modified silicone oils, amine-modified silicone oils and the like are mentioned, and one or more of these are preferably used.

The ultraviolet absorber is not particularly limited. For example, trade names “Tinuvin P”, “Tinuvin 320” and “Tinuvin 32” manufactured by Ciba-Geigy, Inc.
And benzotriazole-based ultraviolet absorbers such as "6" and "tinuvin 328", and one or more of these are suitably used.

The light stabilizer is not particularly restricted but includes, for example, hindered amine light stabilizers such as "ADEKA STAB LA-57" (trade name, manufactured by Asahi Denka Kogyo Co., Ltd.). One or more kinds are suitably used.

Examples of the antioxidant include, but are not particularly limited to, phenol-based antioxidants such as "Sumilyzer BHT" manufactured by Sumitomo Chemical Co., Ltd. and "Irganox 1010" manufactured by Ciba Geigy. Antioxidants and the like are mentioned, and one or more of these are suitably used.

The surfactant is not particularly restricted but includes, for example, sodium lauryl sulfate and sodium alkylbenzenesulfonate, and one or more of these are preferably used.

Next, the interlayer film for laminated glass according to the fourth invention is characterized in that the composition for an interlayer film according to any of the first to third inventions described above is formed.

The method for producing the interlayer film for laminated glass is as follows.
It is not particularly limited, and for example, the first invention to the third invention
After uniformly kneading the composition for an intermediate film according to any of the inventions, a film is formed into a sheet by an extrusion method, a calendar method, a pressing method, a casting method, an inflation method, etc. to form a resin film of the composition for an intermediate film. Then, this may be used as an intermediate film.

The resin film of the composition for an intermediate film may be a single layer or an intermediate film in a state where two or more sheets are laminated. The intermediate film may be used as a single layer, or may be used in a state where two or more sheets are stacked.

The total thickness of the above-mentioned intermediate film is not particularly limited. However, in consideration of shock absorption, penetration resistance, weather resistance, and the like required for a laminated glass, a practical laminated glass is practically used. 0.3 as in the case of
It is preferably about 2 mm.

Next, the laminated glass according to the fifth invention is characterized in that the interlayer film for laminated glass according to the fourth invention is interposed between at least a pair of glasses and integrated.

The above glass includes not only ordinary inorganic transparent glass but also organic transparent glass such as polycarbonate plate and polymethyl methacrylate plate.

The type of the above glass is not particularly limited. For example, various types of inorganic glass such as float glass, polished glass, template glass, mesh glass, wire glass, heat absorbing glass, and colored glass. Glass or organic glass is mentioned, and one or more of these are suitably used. The thickness of the glass may be appropriately selected depending on the application, and is not particularly limited.

The manufacturing method of the laminated glass according to the fifth invention is not special, and the same manufacturing method as in the case of ordinary laminated glass is employed. For example, an interlayer film for laminated glass according to the fourth invention is interposed between two transparent glass plates, placed in a rubber bag, pre-adhered at a temperature of about 70 to 110 ° C. while suctioning under reduced pressure, and then autoclaving. Or using a press, about 120-150 ° C
A desired laminated glass can be obtained by performing the actual bonding at a temperature of about 10 to 15 kg / cm ² and integrating them.

[0060]

The composition for an intermediate film according to the first and second inventions is characterized in that a specific amount of triethylene glycol di-2-ethylhexanoate having a relatively high boiling point is used as a plasticizer with respect to polyvinyl butyral resin as a main component. Contained
In addition, since the cloud point of a solution obtained by dissolving a specific amount of the polyvinyl butyral resin with respect to the triethylene glycol di-2-ethylhexanoate is defined in a specific range, the bleed out of the plasticizer to the surface of the intermediate film is performed. It is suitable for obtaining an interlayer film for laminated glass, which can prevent a decrease in blocking resistance of the interlayer film and a whitening phenomenon of the interlayer film, etc., and also has an excellent trim cut property.

The composition for an intermediate film according to the third invention is the composition for an intermediate film according to the first or second invention, wherein the composition for an intermediate film contains a magnesium salt of a carboxylic acid having 2 to 10 carbon atoms as an adhesion regulator. Therefore, in addition to the above-mentioned advantages of the composition for an intermediate film according to the first and second aspects of the present invention, the adhesive strength to glass is maintained within an appropriate range both at an initial stage and after a lapse of time. Suitable for obtaining an interlayer film for laminated glass.

The interlayer film for laminated glass according to the fourth invention comprises:
Since the composition for an intermediate film according to any one of the first to third inventions is formed into a film, the composition has excellent blocking resistance at the time of storage, transportation, and the like, as well as bleed-out and whitening of the plasticizer. It is suitable for obtaining a laminated glass having almost no occurrence or the like, and having an adhesive strength to glass within an appropriate range both at an initial stage and after a lapse of time, and having an excellent trim cut property.

The laminated glass according to the fifth invention is characterized in that
Since it is manufactured using the interlayer film for laminated glass according to the invention, it is excellent in basic performance required for laminated glass such as transparency, shock absorption, penetration resistance, etc., hardly causes whitening phenomenon, and has trim cutability. Is also excellent.

[0064]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples. In the examples, “parts” means “parts by weight”.

(Example 1)

(1) Preparation of Composition for Intermediate Film An average degree of butyralization of 68.5 synthesized by a precipitation method using polyvinyl alcohol (PVA) having an average degree of polymerization of 1700 and a saponification degree of 99 mol% and butyraldehyde as raw materials. For 100 parts by mol of polyvinyl butyral resin (PVB), 40 parts of triethylene glycol di-2-ethylhexanoate (3GO) as a plasticizer and 0.13 part of magnesium 2-ethylbutanoate (Mg
(Concentration: 90 ppm) and uniformly stirred and mixed to obtain a composition for an intermediate film.

(2) Measurement of cloud point 100 parts of the above 3GO and PVB8 were placed in a glass test tube.
Part, and heated to 170 ° C. to dissolve PVB, PV
A B-3GO solution was obtained. Next, the solution was stirred and cooled while measuring the temperature of the solution with a thermocouple, and the temperature at which part of the solution began to cloud (cloud point) was measured. The cloud point was 113 ° C.

(3) Production of interlayer film for laminated glass A small die extruder (trade name “Laboplast Mill”, manufactured by Toyo Seiki Co., Ltd.) was equipped with a T-die, and the extrusion temperature was 80 to 180 ° C. and the mold outlet temperature was 200 ° C. The composition for an intermediate film obtained in (1) was extruded and formed into a film under the conditions described in (1) to obtain an intermediate film for a laminated glass having a thickness of 800 μm.

(4) Production of Laminated Glass The interlayer film for laminated glass obtained above was sandwiched between two pieces of float glass (thickness: 2.4 mm), placed in a rubber vacuum bag, and vacuumed at 20 torr. After holding for 20 minutes, the substrate was kept in an oven at 90 ° C. for 30 minutes and preliminarily bonded. Next, the preliminarily bonded laminate was heated in an autoclave at a temperature of 150 ° C. and a pressure of 13 kg / c.
It was hot-pressed under the conditions of m ² and permanently bonded to obtain a laminated glass.

(5) Evaluation The performance (compatibility and blocking resistance) of the interlayer film for laminated glass obtained above, and the performance of the laminated glass obtained above ｛Trim cut property, adhesive strength (Pummel value) And moisture resistance｝ were evaluated by the following methods. The results were as shown in Table 2.

Compatibility: The interlayer film for laminated glass is 23 ° C.
After being left in an atmosphere of -25% RH for 3 days, the plasticizer bleed out to the surface of the intermediate film with a blotting paper was blotted, and the presence or absence of stains was visually observed, and the compatibility was evaluated according to the following criteria. [Evaluation criteria] ○ ‥‥ No stain was observed and compatibility was good × ‥‥ A large amount of stain was observed and compatibility was poor

Blocking resistance: The interlayer film for laminated glass was cut into a rectangle of 10 mm × 25 mm, and two layers were laminated.
After a load of 2 kg was placed thereon and allowed to stand for 25 hours, the 180-degree square peel strength was measured using a tensile tester, and the blocking resistance was evaluated according to the following criteria. The peel strength was an average value of n = 3. [Judgment Criteria] ○ ‥‥ peel strength less than 100 (g / cm), good blocking resistance × ‥‥ peel strength 100 (g / cm) or more, poor blocking resistance

Trim-cutting property: The work of cutting the intermediate film (trim) protruding from the edge of the laminated glass with a cutter knife was performed, and the trim-cutting property was evaluated according to the following criteria. [Judgment criteria] ○ ‥‥ Easily cut × ‥‥ Interlayer was hard and difficult to cut

Adhesive strength (Pummel value): -18 ± 0.6
The laminated glass, which had been left standing at a temperature of 16 ° C. for 16 hours, was beaten with a hammer having a head of 0.45 Kg, and crushed 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 by a preliminarily graded limit sample, and the result was expressed as a Pummel value according to the criterion shown in Table 1 below, and was defined as an adhesive force. 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.

[0075]

[Table 1]

Moisture resistance: Laminated glass at 50 ° C.-95%
After being left in an RH atmosphere for 4 weeks, it was taken out, and the distance of the whitened portion (whitening distance (mm)) was measured from the peripheral edge of the laminated glass.

(Example 2) In the preparation of the composition for an intermediate film, 0.05 g of magnesium acetate was used instead of 0.13 part of magnesium 2-ethylbutanoate as an adhesion regulator.
An intermediate film composition was obtained in the same manner as in Example 1 except that 2 parts (Mg concentration: 60 ppm) was added.

Example 3 In the preparation of the composition for an intermediate film, the average butyralization degree was 68.5 mol% as PVB.
Instead of 100 parts of PVB, the average degree of butyralization is 7
A composition for an intermediate film was obtained in the same manner as in Example 1 except that 100 parts of PVB of 1.0 mol% was used. In addition, 3GO
PVB-3G obtained by dissolving 8 parts of PVB per 100 parts
When the cloud point of the O solution was measured in the same manner as in Example 1, the cloud point was 101 ° C.

Example 4 In the preparation of the composition for an intermediate film, the average degree of butyralization was 68.5 mol% as PVB.
Average butyralization degree of 6 instead of 100 parts of PVB
A composition for an intermediate film was obtained in the same manner as in Example 1, except that 100 parts of 7.0 mol% of PVB was used. In addition, 3GO
PVB-3G obtained by dissolving 8 parts of PVB per 100 parts
When the cloud point of the O solution was measured in the same manner as in Example 1, the cloud point was 123 ° C.

(Comparative Example 1) In the preparation of the composition for an intermediate film, the average degree of butyralization was 68.5 mol% as PVB.
Average butyralization degree of 6 instead of 100 parts of PVB
A composition for an intermediate film was obtained in the same manner as in Example 1, except that 100 parts of PVB of 4.1 mol% was used. In addition, 3GO
PVB-3G obtained by dissolving 8 parts of PVB per 100 parts
When the cloud point of the O solution was measured in the same manner as in Example 1, the cloud point was 137 ° C.

(Comparative Example 2) In the preparation of the composition for an intermediate film, a boiling point of 19 parts was used instead of 40 parts of 3GO as a plasticizer.
A composition for an intermediate film was obtained in the same manner as in Example 1, except that 40 parts of triethylene glycol di-2-ethylbutyrate (3GH) at 6 ° C / 5 mmHg was used. The above 3
PVB-3G in which 8 parts of PVB are dissolved in 100 parts of GH
When the cloud point of the H solution was measured in the same manner as in Example 1, the cloud point was 68 ° C.

(Comparative Example 3) In the preparation of the composition for an intermediate film, 0.106 part of potassium acetate (K concentration: 300 ppm) was added as an adhesive force regulator instead of 0.13 part of magnesium 2-ethylbutanoate. Comparative Example 2 except that
In the same manner as in the above, a composition for an intermediate film was obtained.

(Comparative Example 4) In the preparation of the composition for an intermediate film, the average degree of butyralization was 68.5 mol% as PVB.
Instead of 100 parts of PVB, the average degree of butyralization is 7
A composition for an intermediate film was obtained in the same manner as in Example 1 except that 100 parts of 5.6 mol% of PVB was used. In addition, 3GO
3GO-PV in which 8 parts of the PVB was dissolved in 100 parts
The cloud point of Solution B was measured in the same manner as in Example 1, and the cloud point was 84 ° C.

Using the compositions for interlayer films obtained in Examples 2 to 4 and Comparative Examples 1 to 4, production of interlayer films for laminated glass and laminated glass was performed in the same manner as in Example 1. Was. However, in the interlayer film for a laminated glass manufactured using the composition for an interlayer film of Comparative Example 1, the plasticizer (3GO) bleed out violently, so that no laminated glass was manufactured.

The performances of the interlayer films for laminated glass and laminated glass obtained in Examples 2 to 4 and Comparative Examples 2 to 4 were evaluated in the same manner as in Example 1. The results were as shown in Table 2. In the interlayer film for laminated glass obtained in Comparative Example 1, since the plasticizer (3GO) bleed out violently, the evaluation of blocking resistance was not performed.

[0086]

[Table 2]

As is clear from Table 2, the interlayer films for laminated glass of Examples 1 to 4 produced using the compositions for interlayer films of Examples 1 to 4 according to the present invention are polyvinyl butyral resins (PVB). ) And the plasticizer (3GO) were excellent in compatibility, and exhibited excellent blocking resistance.

The laminated glasses of Examples 1 to 4 produced using the interlayer films for laminated glass of Examples 1 to 4 described above had trim cut properties, adhesive strength (Pummel value), and moisture resistance (whitening resistance). Sex).

On the other hand, the interlayer for laminated glass of Comparative Example 1 produced using the composition for interlayer of Comparative Example 1 in which the cloud point of the PVB-3GO solution exceeded 130 ° C. was P
Due to the poor compatibility between VB and 3GO, bleeding out of 3GO to the surface of the intermediate film was extremely severe and lacked practicality.

Further, in place of 3GO, a comparative example 2 was produced using an interlayer film for laminated glass comprising the composition for an interlayer film of comparative example 2 using a plasticizer (3GH) having a relatively low boiling point. The laminated glass had poor trim cut properties.

Further, the intermediate of Comparative Example 3 using 3GH as a plasticizer and a potassium salt of carboxylic acid (potassium acetate) in place of the magnesium salt of carboxylic acid having 2 to 10 carbon atoms as an adhesion regulator was used. The laminated glass of Comparative Example 3 produced using the interlayer film for a laminated glass composed of the film composition had poor trim cut properties and severe occurrence of whitening due to moisture absorption.

Further, the interlayer film for laminated glass of Comparative Example 4 produced using the composition for interlayer film of Comparative Example 4 in which the cloud point of the PVB-3GO solution was less than 90 ° C. Was bad.

[0093]

As described above, the interlayer for laminated glass produced using the composition for interlayer according to the present invention is:
Since the compatibility between the polyvinyl butyral resin and the plasticizer is good, there is almost no bleed-out of the plasticizer on the surface of the intermediate film, and the anti-blocking property during storage or transportation is excellent.

Further, the laminated glass of the present invention produced using the interlayer film for laminated glass is excellent in trim cutability, so that the workability is good, and the adhesive strength between the interlayer film and the glass is within an appropriate range. It is excellent in basic performance as a laminated glass, such as shock absorption and penetration resistance, and excellent in moisture resistance (whitening resistance), so that it is suitably used for automobiles and buildings.

Claims (5)

[Claims] 1. An intermediate film composition comprising 20 to 60 parts by weight of triethylene glycol di-2-ethylhexanoate with respect to 100 parts by weight of a polyvinyl butyral resin, wherein A composition for an intermediate film, wherein a solution obtained by dissolving 8 parts by weight of the polyvinyl butyral resin per 100 parts by weight of ethyl hexanoate has a cloud point of 90 to 130 ° C. 2. The composition for an intermediate film according to claim 1, wherein the polyvinyl butyral resin has an average degree of butyralization of 65 to 72 mol%. 3. The composition for an intermediate film according to claim 1, further comprising a magnesium salt of a carboxylic acid having 2 to 10 carbon atoms. 4. An interlayer for laminated glass, wherein the composition for an interlayer according to any one of claims 1 to 3 is formed. 5. The method according to claim 4, wherein at least between the pair of glasses.
A laminated glass characterized by being integrated with an interlayer film for laminated glass as described in 1 above.