KR102071793B1 - Film for laminating glasses, and laminated glasses comprising of the same - Google Patents

Abstract

The present invention relates to a film for glass bonding and laminated glass including the same, comprising: a first layer comprising a first resin and a plasticizer comprising polyvinyl acetal resin A; And a second layer in contact with one surface of the first layer, the second resin including a polyvinyl acetal resin B and a plasticizer. And a third layer in contact with one surface of the second layer and including a third resin including polyvinyl acetal resin C and a plasticizer, wherein the amount of hydroxyl groups in the first resin is 18% by weight or more. The amount of hydroxyl groups of the third resin is 9% by weight or less, the amount of hydroxyl groups of the second resin is 9-18% by weight, and the amount of hydroxyl groups of the second resin is different from the amount of hydroxyl groups of the first resin or the third resin. will be.

Description

Glass bonding film, and laminated glass including the same {FILM FOR LAMINATING GLASSES, AND LAMINATED GLASSES COMPRISING OF THE SAME}

The present invention relates to a glass bonding film and a laminated glass including the same, which exhibits excellent sound insulation performance in a wide temperature range but does not exhibit foaming phenomenon in the laminated glass.

Plasticized polyvinyl acetals are used in the manufacture of films applied as intermediate layers in light-transmitting laminates such as laminated glass (tempered glass, safety glass), polymer laminates, and the like.

Laminated glass refers to a transparent laminate produced by placing a polyvinyl butyral sheet between two sheets of glass. Laminated glass is mainly used to provide transparent barriers in building railings, exterior materials and automotive windshields.

The main function of laminated glass is to minimize the damage or injury to objects or people in the transparent barrier by absorbing the energy caused by the blow without allowing penetration through the laminated glass (penetration resistance) (impact resistance). . In addition, interlayer sheets applied to laminated glass may impart additional functionality to the laminated glass, such as reducing acoustic noise and reducing UV and / or IR light transmission.

In particular, the film used for glass of automobiles, buildings, and the like has a great demand for improving sound insulation. The sound insulation can be evaluated as the transmission loss according to the frequency change. Especially, the range of 1,000 to 6,000 Hz, which belongs to the range of the loudness curve, has a high sensitivity in human hearing, so it is above the sound insulation performance in other areas. Sound insulation performance at is important.

Laminated glass using a conventional interlayer film, the anti-scattering effect is sufficient, but it is difficult to sufficiently reduce the coincidence effect (coincidence effect) which is a resonance effect by the glass plate around 2,000 Hz, it is difficult to have sufficient sound insulation performance.

For example, Japanese Patent No. 3,335,436 discloses a laminated glass exhibiting scattering prevention performance and sound insulation performance by interposing an interlayer film between a pair of glass plates. However, since the interlayer film interposed between the laminated glass is specialized in sound insulation performance only at room temperature, the effect of sound insulation performance is limited in an actual field where temperature changes occur in the morning / evening or season.

Japanese Patent No. 3,224,436 Domestic Patent No. 10-1354439

An object of the present invention is to provide a film for glass bonding, and a laminated glass including the same, which exhibits excellent sound insulation performance in a wide temperature range but does not exhibit foaming on the laminated glass.

In order to achieve the above object, the glass bonding film according to an embodiment of the present invention comprises a first layer comprising a first resin and a plasticizer comprising a polyvinyl acetal resin A; And a second layer in contact with one surface of the first layer, the second resin including a polyvinyl acetal resin B and a plasticizer. And a third layer in contact with one surface of the second layer and including a third resin including polyvinyl acetal resin C and a plasticizer, wherein the amount of hydroxyl groups in the first resin is 18% by weight or more. The amount of hydroxyl groups of the third resin is 9% by weight or less, the amount of hydroxyl groups of the second resin is 9-18% by weight, and the amount of hydroxyl groups of the second resin is different from the amount of hydroxyl groups of the first resin or the third resin. will be.

The thickness ratio of the first layer and the second layer may be 1: 0.01 to 0.35.

The thickness of the second layer may be 10% or less of the total thickness of the glass bonding film.

The ratio of the thickness of the first layer and the thickness of the third layer may be 1: 0.15 to 0.35.

The glass bonding film may have a loss factor value of 0.32 or more measured at 20 ° C. and a loss factor value of 10 ° C. or more measured at 10 ° C.

The second resin included in the second layer may have a hydroxyl content of 13.5 to 18 wt% or less.

The difference between the plasticizer content (G2) of the second layer and the plasticizer content (G3) of the third layer may range from -8 to + 8% by weight.

The difference between the plasticizer content (G1) of the first layer and the plasticizer content (G3) of the third layer may range from -15 to -5 wt%.

The content of the plasticizer included in the second layer may be 26 to 42% by weight based on the entire second layer.

Laminated glass according to another embodiment of the present invention includes a laminate in which the glass bonding film according to claim 1 is positioned between a pair of glass.

The glass bonding film of the present invention, and the laminated glass including the same have excellent penetration resistance and impact resistance even at a thin thickness of less than a certain level, and in particular, sound insulation at low temperature while maintaining sound insulation properties at room temperature and high temperature at the same level. It can have excellent sound insulation in a wide temperature range, such as to improve the characteristics. The foaming phenomenon that can occur after the glass bonding, which is a problem of the existing sound insulation film, does not occur or is insufficient so that it cannot be visually confirmed.

Figure 1 (a) and (b) is a conceptual diagram illustrating a cross section of the film for glass bonding according to an embodiment of the present invention, respectively.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art may easily implement the present invention. As those skilled in the art would realize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention. Like parts are designated by like reference numerals throughout the specification.

Throughout this specification, the term "combination of these" included in the expression of the makushi form means one or more mixtures or combinations selected from the group consisting of constituents described in the expression of the makushi form, wherein the constituents It means to include one or more selected from the group consisting of.

Throughout this specification, description of "A and / or B" means "A, B, or A and B".

Throughout this specification, terms such as “first”, “second” or “A”, “B” are used to distinguish the same terms from each other unless otherwise specified.

In the present specification, that B is located on A means that B is located on A, or that B may be positioned on A while another layer is located therebetween and B is in contact with the surface of A. It is limited to what does and is not interpreted.

In the present specification, the singular forms “a,” “an” and “the” are intended to be interpreted in the context of the singular or plural forms, unless the context describes them otherwise.

In the present specification, the size of each component in the drawings may be exaggerated for the purpose of explanation, and may differ from the size actually applied.

In this invention, evaluation of the amount of hydroxyl groups measured and evaluated the amount of ethylene groups which the hydroxyl group of the said polyvinyl acetal resin couple | bonded with the method based on JISK6728.

In the present specification, the weight average molecular weight or the number average molecular weight is expressed by omitting Dalton (Da) as a unit. The measurement of the weight average molecular weight, etc. has been described based on values measured using gel permeation chromatography (GPC) -evaporative light scattering detector (ELSD), but the measuring method is not limited thereto.

The inventors of the present invention confirmed that the foaming phenomenon may occur more easily when the film with improved sound insulation is produced in laminated glass, and during the development of a film without such a foaming phenomenon, a certain kind of layer The present invention was completed by confirming that it was possible to manufacture a film having excellent sound insulation in a wider temperature range and no foaming phenomenon by laminating.

1A and 1B are conceptual views illustrating cross sections of a film for glass bonding according to an embodiment of the present invention, respectively. Hereinafter, the present invention will be described in detail with reference to the drawings. In order to achieve the above object, the glass bonding film 900 according to an embodiment of the present invention includes a first layer 100 including a first resin and a plasticizer containing a polyvinyl acetal resin A; And a second layer 200 in contact with one surface of the first layer and including a second resin and a plasticizer including polyvinyl acetal resin B; And a third layer 300 contacting one surface of the second layer and including a third resin and a plasticizer including polyvinyl acetal resin C.

The polyvinyl acetal resin may be a polyvinyl acetal resin obtained by acetalizing polyvinyl alcohol having a degree of polymerization of 1,600 to 3,000 with aldehyde. The aldehyde is not particularly limited. For example, it may be selected from the group consisting of n-butyl aldehyde, isobutyl aldehyde, n-barrel aldehyde, 2-ethyl butyl aldehyde, n-hexyl aldehyde and blend resins thereof. Specifically, the resin produced using n-butyl aldehyde is good in that the refractive index difference with glass is small and the bonding strength with glass is excellent.

The first resin is a polyvinyl acetal resin having an amount of hydroxyl groups of 18% by weight or more.

The first resin may be a polyvinyl acetal resin having a hydroxyl group amount of 18 to 30% by weight.

The first resin may contain 0.1 to 3% by weight of an acetyl group.

The third resin is a polyvinyl acetal resin having a hydroxyl amount of 9% by weight or less.

The third resin may be a polyvinyl acetal resin having a hydroxyl group amount of 1 to 9 wt%.

The third resin may contain 3 to 15% by weight of an acetyl group.

The second resin is a polyvinyl acetal resin having a hydroxyl amount of 9 to 18% by weight.

The second resin may contain 3 to 15% by weight of an acetyl group.

The second resin may be applied to polyvinyl acetal resin of 9 to 18% by weight alone (single resin), and may be applied by mixing two or more polyvinyl acetal resins having different amounts of hydroxyl groups from each other (mixed resins). ).

When applying a resin having such characteristics to the first to third layers it can be produced a multilayer film having both mechanical strength and sound insulation properties.

The amount of hydroxyl groups of the second resin is different from the amount of hydroxyl groups of the first resin or the third resin. That is, the second layer 200 positioned between the first layer 100 and the third layer 300 so as to be in direct contact with one surface of each of the two layers may have different characteristics from each other. It serves as a bridge between the layer 100 and the third layer 300 and also serves to suppress the occurrence of phenomena such as bubble formation at the interface between the two layers, which may occur due to the heterogeneous properties of the two layers.

The second resin, which is a resin included in the second layer 200, may have a characteristic corresponding to that between the first resin and the third resin, and specifically, the value of the hydroxyl device of the second resin is the first resin. It may have a value between the hydroxyl value of the resin and the hydroxyl value of the third resin.

The second resin included in the second layer 200 may have a hydroxyl content of 13.5 to 18 wt%. In such a case, the low temperature (10 ° C) sound insulation and the high temperature (30 ° C) sound insulation may be maintained or improved while maintaining the sound insulation at 20 ° C. or more.

The first resin may have a weight average molecular weight value of 200,000 to 300,000. The first resin may have a weight average molecular weight value of 240,000 to 280,000, and may be 250,000 to 270,000.

The third resin may have a weight average molecular weight value of 490,000 to 850,000, 610,000 to 820,000, and 690,000 to 790,000. The weight average molecular weight value of the third resin is significantly higher than the weight average molecular weight value of the first resin, and co-extrusion workability is applied even when a large amount of plasticizer is applied to the third resin 300. Improved process convenience and can improve the mechanical properties of the multilayer film produced.

The same plasticizer applied to the first layer 100, the second layer 200, and the third layer 300 may be applied to the same one, or may be different from each other.

The plasticizer is specifically triethylene glycol bis 2-ethylhexanoate (3G8), tetraethylene glycol diheptanoate (4G7), triethylene glycol bis 2-ethylbutyrate (3GH), triethylene glycol bis 2-heptanoate (3G7), dibutoxyethoxyethyl adipate (DBEA), butyl carbitol adipate (DBEEA), dibutyl sebacate (DBS), bis 2-hexyl adipate (DHA) and mixtures thereof Can be. The plasticizers are each independently composed of triethylene glycol bis 2-ethylhexanoate (3G8), triethylene glycol bis2-ethylbutyrate (3GH), triethylene glycol bis 2-heptanoate (3G7), and combinations thereof. Any one selected from the group may be applied, and in this case, it is good in compatibility with the resin, maintaining the mechanical strength of the film, and the like.

The content of the plasticizer included in the first layer 100 may be 24 to 30% by weight based on the entire first layer. Specifically, the first layer 100 may include 70 to 76% by weight of the first resin, and 24 to 30% by weight of the plasticizer. In addition, if necessary, it may include 0 to 2% by weight of the additive described below. In this case, the first layer 100 may form a film for glass bonding having excellent mechanical properties while having an appropriate bonding strength with the glass and the second layer 200.

The content of the plasticizer included in the second layer 200 may be 26 to 42 wt% based on the entire second layer. Specifically, the second layer 200 may include 58 to 72 wt% of the second resin and 26 to 42 wt% of the plasticizer. The second layer 200 may include 58 to 68 wt% of the second resin and 30 to 42 wt% of the plasticizer. In addition, if necessary, it may include 0 to 2% by weight of the additive described below. In this case, the second layer 200 has a proper bonding force with the first layer 100 and the third layer 300, to mitigate the heterogeneous characteristics of both layers to stabilize the physical properties of the entire film, in particular to generate bubbles It acts as a deterrent.

The amount of the plasticizer included in the third layer 300 may be 32 to 42 wt% based on the entire third layer. Specifically, the third layer 300 may include 58 to 68 wt% of the third resin and 32 to 42 wt% of the plasticizer. In addition, if necessary, it may include 0 to 2% by weight of the additive described below. In this case, the third layer 300 may serve as a sound insulation layer while having an appropriate bonding force with the second layer 200.

Wherein the content of plasticizer may be a (G ₂₎ and said second range of -8 to + 8% by weight The difference between the content of the plasticizer (G ₃₎ of the third layer 300 of the second layer 200, -6 to +6 weight It may be in the range of%.

Wherein the content of plasticizer may be a (G ₁₎ and wherein the range of -15 to -5% by weight, the difference in plasticizer content (G ₃₎ of the third layer 300 of the first layer 100, -13 to -7 by weight It may be in the range of%.

When the film is configured to have a difference between the plasticizer contents of each of these layers, it is possible to provide a film for glass bonding having excellent sound insulation properties in a wider temperature range.

In particular, when the other conditions are the same, when the value obtained by subtracting the plasticizer content of the third layer from the plasticizer content of the second layer has a negative value, the low temperature sound insulation property may be further improved.

The thickness ratio of the first layer 100 and the second layer 200 may be 1: 0.01 to 0.35, 1: 1: may be 0.02 to 0.3. In the case of having such a thickness ratio, the effect of alleviating the interfacial heterogeneity with the third layer, which will be described later, by the second layer and the mechanical strength improvement effect by the first layer can be better exhibited.

The thickness ratio of the first layer 100 and the second layer 200 may be 1: 0.02 to 0.15, 1: 1: may be from 0.02 to 0.1. In this case, the sound insulation characteristics at room temperature and high temperature can be further improved while having an interlayer heterogeneity alleviation effect.

The ratio of the thickness of the first layer and the thickness of the third layer may be 1: 0.15 to 0.35, and 1: 0.18 to 0.35. In addition, the ratio of the thickness of the first layer and the thickness of the third layer may be 1: 0.22 to 0.35, 1: 1: may be 0.27 to 0.34. When the glass bonding film is constituted by such a ratio of the thickness, a wider range of sound insulating properties can be realized with a thinner thickness, and the mechanical properties of the film can be maintained well.

The thickness of the second layer may be 10% or less of the total thickness of the glass bonding film, 0.1 to 10%, thickness may be 9.5% or less, and 0.5 to 9.5%. In addition, the thickness of the second layer may be 0.5 to 5% of the total thickness of the glass bonding film, may be 0.8 to 3%. In the case of forming the thickness of the second layer in such a range, it is possible to implement a thin glass-bonding film as a whole, to reduce interfacial heterogeneity between layers, and to further improve sound insulation characteristics.

The thickness of the first layer may be 30% or more of the total thickness of the glass bonding film, the thickness may be 30 to 45% or less, and may be 33 to 43% or less. When the first layer is formed at such a thickness ratio, sufficient and stable mechanical strength may be given to the glass bonding film.

The thickness of the third layer may be 10 to 15% of the total thickness of the glass bonding film. When the third layer is formed at such a thickness ratio, stable sound insulating properties may be imparted to the glass bonding film.

The glass bonding film 900 may further include a fourth layer 400 in contact with one surface of the third layer 300 and positioned to face the second layer 200.

Detailed descriptions of the composition, content, and thickness of the fourth layer 400 overlap with descriptions of the composition, content, and thickness of the second layer 200, and thus description thereof is omitted.

In addition, the glass bonding film 900 may further include a fifth layer 500 in contact with one surface of the fourth layer 400 and positioned to face the third layer 300. .

Detailed descriptions of the composition, content, thickness, and the like constituting the fifth layer 500 overlap with descriptions of the composition, content, thickness, etc. constituting the first layer 100, and thus description thereof is omitted.

The entire thickness of the glass bonding film 900 may be 400 to 1300 um, may be 600 to 900 um. When forming the glass bonding film in the range of such a thickness it can be provided a multilayer film that satisfies the sound insulation properties and mechanical properties requirements at the same time.

Each layer may further contain an additive selected from the group consisting of an antioxidant, a heat stabilizer, a UV absorber, a UV stabilizer, an IR absorber, a glass bonding force regulator, and a combination thereof, as necessary.

The antioxidant may be used hindered amine or hindered phenol (hindered phenol). Specifically, a hindered phenol-based antioxidant is more preferable in the polyvinyl butyral (PVB) manufacturing process requiring a process temperature of 150 ° C or higher. A hindered phenolic antioxidant can use, for example, BARG's IRGANOX 1076, 1010, etc.

The thermal stabilizer may be a phosphite-based thermal stabilizer when considering compatibility with the antioxidant. For example, IRSF's IRGAFOS 168 may be used.

The UV absorber may be used Chemisorb 12, Chemisorb 79, Chemisolve 74, Chemisolve 102, Tinuvin 328, Tinuvin 329, Tinuvin 326 from BASF. The UV stabilizer may be used such as BASF Tinuvin. ITO, ATO, AZO, etc. may be used as the IR absorber, and the glass bonding force modifier may be a metal salt such as Mg, K, Na, epoxy-modified Si oil, or a mixture thereof, but the present invention is limited thereto. It doesn't happen.

The glass bonding film 900 may have a loss factor value measured at 10 ° C. of at least 0.18 and a loss factor value measured at 20 ° C. of at least 0.32.

The glass bonding film 900 may have a loss coefficient value measured at 10 ° C. of 0.20 or more and a loss coefficient value measured at 20 ° C. of 0.32 or more.

The glass bonding film 900 may have a loss coefficient value measured at 10 ° C. of 0.20 or more, a loss coefficient value measured at 20 ° C. of 0.32 or more, and a loss coefficient value measured at 30 ° C. of 0.20 or more.

The loss factor evaluation is based on the results measured with a film having a thickness of 800 to 900 um.

Laminated glass according to another embodiment of the present invention includes a laminate in which the film for glass bonding described above is positioned between a pair of glass.

The laminated glass may be utilized as a windshield or building interior and exterior materials of automobiles as safety glass. Glass of the laminated glass can be applied to replace the transparent plastic material if necessary.

Hereinafter, specific laboratory examples of the present invention will be described in more detail.

Experimental Example 1: Evaluation of Resin and Composition

Manufacture of film for glass bonding

Polyvinyl acetal resins having the properties shown in Table 1 below were obtained by butyrating the polyvinyl alcohol resins having a degree of polymerization of 1700 and 2400 from n-butylaldehyde:

Production Example Degree of polymerization Safflower Acetalization degree Fisheries Acetyl group amount mol% wt% First floor Resin A 1700 99 78.2 20.6 1.2 2nd layer Resin B 2400 92 75.1 14.3 10.6 3rd floor Resin C 2400 92 82.2 8.8 9

When the mixed resin was applied to the second layer, the resin A and the resin B were mixed 1: 1 and applied as the second resin. At this time, the amount of hydroxyl groups was found to be 17.45% by weight.

The polyvinyl acetal resin and the plasticizer triethylene glycol di-2-ethylhexanoate (3G8, obtained from PROVIRON, PROVIST 1766) are each added in the amounts shown in Table 2 below, and thoroughly kneaded with a mixing roll for forming each layer. The resin composition was obtained.

By coextrusion with an extruder using the obtained resin composition for each layer, a film for glass bonding as shown in Fig. 1 (b) (total thickness of about 800 um, five layers of 300-50-100-50-300 um Structure), and the fourth layer was prepared in the same manner as the second layer, and the fifth layer was prepared in the same manner as the first layer. In Comparative Example 1, a total thickness of about 800 um was produced as a three-layer film having a first layer-second layer-first layer (340-120-340 um).

Sample Layer structure Suzy Hydroxyl group of resin
content
(weight%) On each floor
Plasticizer content
(weight%) G ₂ -G ₃ * G ₁ -G ₂ * G ₁ -G ₃ * Example 1 First floor Resin A 20.6 27 3 -10 -7 The second layer Resin B 14.3 37 3rd floor Resin C 8.8 34 Example 2 First floor Resin A 20.6 27 0 -10 -10 The second layer Resin B 14.3 37 3rd floor Resin C 8.8 37 Example 3 First floor Resin A 20.6 27 -3 -10 -13 The second layer Resin B 14.3 37 3rd floor Resin C 8.8 40 Example 4 First floor Resin A 20.6 27 3 -10 -7 The second layer Resin A + Resin B 17.45 37 3rd floor Resin C 8.8 34 Example 5 First floor Resin A 20.6 27 6 -13 -7 The second layer Resin A + Resin B 17.45 40 3rd floor Resin 2 8.8 34 Comparative Example 1 First floor Resin A 20.6 27 - - - 3rd floor Resin C 8.8 37

* G ₁ , G ₂ and G ₃ are the plasticizer contents of the first layer, the second layer and the third layer, respectively, and are weight percent values based on the total composition of each layer.

Evaluation of physical properties

(Sound insulation evaluation)

Each of the films was cut to a size of 30 cm in length and 2.5 cm in width, and sandwiched between two transparent float glasses (30 cm in length, 2.5 cm in width and 2.1 T in thickness) to obtain a laminate. The laminate was placed in a rubber bag and degassed with a vacuum of 2.6 KPa for 20 minutes, then degassed and placed in an oven for 30 minutes at 90 ° C., and the laminate was pre-pressed by vacuum press. The laminated body preliminarily crimped in the autoclave at the temperature of 140 degreeC, and the pressure conditions of 1.2 MPa was crimped for 20 minutes, and the laminated glass used for sound insulation measurement was obtained.

The laminated glass was subjected to vibration by a vibration generator for dumping test, the vibration characteristics obtained therefrom were amplified by a mechanical impedance measuring device, and the vibration spectrum was analyzed by an FFT spectrum analyzer to obtain L / F (loss factor) values. Indicated.

(Evaluation degree of foaming)

Five laminated glass were used for each film for each foaming test. Specifically, the foaming test was carried out in the same manner as the laminated glass used for the above acoustic test except that laminated films were sandwiched between two transparent float glass (10 cm wide, 10 cm wide, and 2.1 T thick). The laminated glass used for was obtained.

The laminated glass thus prepared was left for 100 hours in an oven at 50 ° C., and then observed whether foaming occurred in the laminated glass. From the observation result, the state of foaming was determined by the following criteria.

The foam size generated in the five laminated glass was approximated to an ellipse in plan view, and its elliptical area was made into the foam area. The average value of the elliptic area observed in the five laminated glass was obtained, and the ratio (percentage) of the average value (foamed area) of the elliptic area to the area of the laminated glass (10 cm wide and 10 cm long) was calculated. Table 3 shows.

(Circle): Foaming is not observed in all the laminated glass.

(Circle): The ratio of the average value (foam area) of an ellipse area is less than 5%.

(Triangle | delta): The ratio of the average value (foam area) of an ellipse area is 5% or more and less than 10%.

X: The ratio of the average value (foam area) of an ellipse area is 10% or more.

Penetration Assessment

The penetration resistance of the laminated glass was evaluated based on KS L 2007.

Each of the Examples and the films, 300 mm × 300 mm, 2.1 T thick glass, and each of the Examples and films were prepared in a laminated structure of glass-film-glass, and pre-bonded by vacuum to degas and edge seal. Thereafter, the specimen was prepared by bonding the specimen at 150 ° C. for 2 hours using an autoclave. Thereafter, 2.26 kg of steel balls were dropped on the specimen, and the height (MBH) through which the specimen was penetrated was measured. In this case, when penetrating at a height of less than 4 m, it is marked as fail, and when penetrating at a height of more than 4 m, it is marked as a pass.

(Impact resistance evaluation)

Based on KS L 2007: 2008, the absence or absence of the laminated glass in which the polyvinyl acetal film was laminated was evaluated.

2.1 The process of manufacturing and bonding each of the T-thickness glass and the film into the laminated structure of the glass-film-glass proceeded in the same manner as the above penetration resistance evaluation.

The low temperature test was to drop 227 g of steel balls at a temperature of minus 20 ° C for 4 hours and then drop them at a height of 9 m and fail if the impacted specimens were broken and the glass was scattered or the amount of glass falling from the sheet was more than 15 g. When the received specimen is not broken or the glass is scattered and the amount of glass falling from the sheet is less than 15 g, it is marked as pass.

The room temperature evaluation is a failure of the glass when it is stored at 40 ° C for 4 hours and then impacted at 10 m. If the amount of glass falling from the sheet which is not broken or the glass is scattered is less than 15 g, it is marked as pass.

In the case of evaluating the pass in both the low temperature evaluation and the room temperature evaluation, it is indicated as a pass in Table 3 below.

Sample L / F In unit area
Firing
(/0.01m ² ) Penetration Tolerance Impact resistance 10 ℃ 20 ℃ 30 ℃ Example 1 0.21 0.34 0.2 OO pass pass Example 2 0.23 0.32 0.2 OO pass pass Example 3 0.24 0.31 0.18 OO pass pass Example 4 0.23 0.32 0.17 OO pass pass Example 5 0.29 0.32 0.16 OO pass pass Comparative Example 1 0.19 0.32 0.16 X pass pass

Referring to Table 3, it was confirmed that the foaming phenomenon does not appear in the foam evaluation while maintaining the basic physical properties of the shock resistance and impact resistance of the samples. In particular, the films were found to have a significant improvement in low temperature sound insulation properties (10 ° C.) while having high temperature sound insulation properties (30 ° C.) and room temperature sound insulation properties (20 ° C.). Along with this, it was also confirmed that the foaming decision result was very good and showed a very good effect in terms of interlayer stability.

Experimental Example 2: Evaluation of Physical Properties According to Thickness Change

Manufacture of film for glass bonding

In the same manner as in Experimental Example 1 above to prepare a glass bonding film of a multi-layer structure, by adjusting the layer ratio of each layer as shown in Table 4 below to prepare a sample.

Sample apply
Suzy Hydroxyl
content
weight% Plasticizer content
weight% G ₂ -G ₃ * G ₁ -G ₂ * G ₁ -G ₃ * thickness
um First floor
prepare
Each floor
Thickness ratio all
In film
thickness
ratio film
Total thickness Example Layer structure Example 6 First floor Resin A 20.6 27 -6 -4 -10 350 1.0000 42.68% 820 The second layer Resin B 14.3 31 10 0.0286 1.22% 3rd floor Resin C 8.8 37 100 0.2857 12.20% Example 7 First floor Resin A 20.6 27 0 -10 -10 350 1.0000 42.68% 820 The second layer Resin B 14.3 37 10 0.0286 1.22% 3rd floor Resin C 8.8 37 100 0.2857 12.20% Example 8 First floor Resin A 20.6 27 0 -10 -10 300 1.0000 34.88% 860 The second layer Resin B 14.3 37 80 0.2667 9.30% 3rd floor Resin C 8.8 37 100 0.3333 11.63%

* G ₁ , G ₂ and G ₃ are the plasticizer contents of the first layer, the second layer and the third layer, respectively, and are weight percent values based on the total composition of each layer.

Films thus prepared were evaluated for physical properties in the same manner as the above-described physical properties evaluation, and the results are shown in Table 5 below.

Sample L / F Foam determination in unit area
(/0.01 m ² ) Penetration Tolerance Impact resistance 10 ℃ 20 ℃ 30 ℃ Example 6 0.21 0.37 0.25 OO pass pass Example 7 0.21 0.35 0.23 O pass pass Example 8 0.23 0.32 0.2 OO pass pass

Referring to the results of Table 5, the samples of Examples 6 to 8 have excellent sound insulation characteristics in a wider range, and in particular, while maintaining or improving the room temperature sound insulation characteristics and the high temperature sound insulation characteristics at the same level, the low sound insulation characteristics were simultaneously improved. . Particularly, in terms of low sound insulation characteristics, the best results were obtained in Example 8, and the results of Example 6 were the best when both room temperature sound insulation characteristics and high temperature sound insulation characteristics were considered. In terms of overall physical properties, when the thickness of the second layer was slightly thinner, the result was better.

Although the preferred embodiments of the present invention have been described in detail above, the scope of the present invention is not limited thereto, and various modifications and improvements of those skilled in the art using the basic concepts of the present invention defined in the following claims are also provided. It belongs to the scope of rights.

100: first layer 200: second layer
300: third layer 400: fourth layer
500: fifth layer 900: film for glass bonding

Claims (10)

A first layer comprising a first resin containing polyvinyl acetal resin A and a plasticizer; And a second layer in contact with one surface of the first layer and including a second resin and a plasticizer including polyvinyl acetal resin B; And a third layer in contact with one surface of the second layer and including a third resin containing a polyvinyl acetal resin C and a plasticizer.
The amount of hydroxyl groups in the first resin is 18% by weight or more, the amount of hydroxyl groups in the third resin is 9% by weight or less, the amount of hydroxyl groups in the second resin is 9-18% by weight, and the amount of hydroxyl groups in the second resin. Is different from the amount of hydroxyl of the first resin or the third resin,
The value obtained by subtracting the plasticizer content (G ₃ ) of the third layer from the plasticizer content (G ₂ ) of the second layer has a negative value in the range of -8 to +8 wt%,
A film for glass bonding, wherein the loss factor value measured at 20 ° C. is 0.32 or more and the loss factor value measured at 10 ° C. is 0.18 or more.
The method of claim 1,
The thickness ratio of the said 1st layer and said 2nd layer is 1: 0.01 to 0.35, the film for glass bonding.
The method of claim 1,
The thickness of the said 2nd layer is a glass bonding film which is 10% or less of the total thickness of the said glass bonding film.
The method of claim 1,
The ratio of the thickness of the first layer and the thickness of the third layer is 1: 0.15 to 0.35, the film for glass bonding.
delete The method of claim 1,
The second resin included in the second layer has a hydroxyl content of 13.5 to 18% by weight or less, glass bonding film.
delete The method of claim 1,
The plasticizer content (G ₁ ) of the first layer minus the plasticizer content (G ₃ ) of the third layer is in the range of -15 to -5% by weight, glass bonding film.
The method of claim 1,
The amount of plasticizer included in the second layer is 26 to 42% by weight based on the entire second layer, the glass bonding film.
Laminated glass including the laminated body in which the film for glass bonding of Claim 1 is located between a pair of glass.

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