JP4992806B2 - Laminated glass manufacturing method and laminated glass - Google Patents

Description

  The present invention relates to a method for producing laminated glass that prevents occurrence of optical defects in laminated glass and has good impact resistance and sound insulation performance, and laminated glass obtained by the production method.

  Transparent glass plates are used for many windows in the building. The glass plate is a highly durable transparent plate and excellent in daylighting performance, but is a material with very low damping performance, so the sound insulation performance is significantly reduced due to the coincidence effect. Therefore, laminated glass made by laminating two or more glass plates with an intermediate film has been used for windows that require sound insulation performance. This is to improve the sound insulation performance of the window glass by using an intermediate film having a damping performance. In other words, the intermediate film is used because it has the ability to convert vibration energy into thermal energy and absorb vibration energy, “damping performance”.

  Conventionally, as an interlayer film for architectural laminated glass, polyvinyl butyral (hereinafter abbreviated as PVB) resin or ethylene vinyl acetate resin (hereinafter abbreviated as EVA), which is excellent in transparency, adhesiveness, and impact resistance, has been used. ing.

However, laminated glass used for window glass for buildings is required to have high sound insulation and excellent sound insulation against sound inside and outside the building in addition to preventing scattering when broken. In general, the glass composition that minimizes the thickness of the window glass satisfying the sound insulation performance of T-3 grade defined in JIS A 4706 is a laminated structure in which two glass plates having a thickness of 6 mm are laminated with an interlayer film of PVB. It is glass. The laminated glass using two glass plates having a thickness of 6 mm has a weight of 30 kg / m ² , and the sash into which the laminated glass is fitted needs to have rigidity corresponding to the weight of the window glass. The weight of the entire opening is very heavy compared to a normal window glass. For this reason, workability | operativity was bad, and not only material cost but construction cost also became high, and the weight reduction of the window glass with a favorable sound-insulation characteristic was desired.

  As a means to reduce the weight of the window glass with good sound insulation performance, there are methods such as thickening the interlayer film or using a glass plate with a different thickness, etc., but increase in manufacturing cost, target sound insulation performance cannot be obtained, etc. Realization as a sound insulation window is difficult.

  There is also a method of reducing the weight of a window glass having good sound insulation by improving the interlayer film. For example, Patent Document 1 discloses a method for improving the sound insulation performance by changing the molecular arrangement of polyvinyl acetal resin. Furthermore, Patent Document 2 discloses an intermediate film having a three-layer configuration of a polyvinyl acetal resin containing a plasticizer.

  Further, Patent Document 3 discloses an interlayer film that makes it possible to provide a window glass having a light-weight and high-performance sound insulation performance on a building window, and improves the sound insulation performance of the laminated glass. For this purpose, a laminated glass having a high sound insulating property is produced by using a resin multilayer intermediate film in which a resin film formed by block copolymerization of polystyrene and a rubber-based resin is sandwiched between two transparent resins.

  When the structure of the interlayer film is multilayered as in Patent Document 3, an optical defect that looks like a rainbow color may occur in the laminated glass manufacturing stage. Furthermore, the impact resistance performance was mechanically lower than that of a conventional laminated glass made of only polyvinyl butyral without passing L2-2 of the shot bag test described in JIS R 3205.

Regarding the production of laminated glass that is characterized by the structure of the interlayer film, for example, Patent Document 4 describes that a vacuum is leaked while being heated.
JP-A-6-926 JP 2004-2108 A JP 2007-014991 A JP 2003-146710 A

  It is an object to provide a method for producing a laminated glass having excellent transparency and high impact resistance, and a laminated glass in the production of laminated glass produced using an interlayer film obtained by laminating resins having different interlayer films. And

  The method for producing a laminated glass of the present invention is a method for producing a laminated glass in which two or more sheets of glass are laminated using an intermediate film. Using an intermediate film having a three-layer structure sandwiched between two layers and two or more glasses, the intermediate film is inserted between the glasses to form a laminate, (Step 2) above the melting point of the resin B, the resin A pretreatment for heat-adhesion is performed while degassing in a temperature range of B melting point + 10 ° C. or lower, and then (step 3) the laminate obtained in step 2 is melted from resin B melting point + 10 ° C. to resin B melting point + 15 ° C. It is a method for producing a laminated glass, characterized in that heat-pressure bonding is performed under a temperature range of 0.25 MPa to 1.3 MPa.

  The laminated glass manufacturing method of the present invention is the above laminated glass manufacturing method, wherein the laminate obtained in step 2 is selected from those having a haze of 40% or less. It is a method for producing a laminated glass, which is bonded by heating and pressing.

  Moreover, the method for producing laminated glass of the present invention is a method for producing laminated glass, wherein the resin A is a copolymer of styrene and a rubber-based resin monomer in the method for producing laminated glass.

A method of manufacturing a laminated glass of the present invention is the manufacturing method of the laminated glass, 1 to claim thickness of a film of heat-adhesive resin B is characterized in that it is 0.01mm or more 0.1mm or less It is a manufacturing method of the laminated glass in any one of Claim 3.

  The method for producing a laminated glass of the present invention is a method for producing a laminated glass, wherein the degassing in step 2 is performed using a rubber vacuum bag or tube in the method for producing a laminated glass. is there.

Moreover, the manufacturing method of the laminated glass of this invention WHEREIN: Deaeration of the process 2 is performed in the range of 1 * 10 < ⁰ > -4 * 10 < ³ > Pa in the manufacturing method of the said laminated glass, The manufacturing of the laminated glass characterized by the above-mentioned. Is the method.

  In addition, the laminated glass of the present invention uses two glasses each having a glass thickness of 3 to 5 mm and a total thickness of two glasses of 8 to 10 mm. The laminated glass is characterized by having a sound insulation performance of 2 to 1 mm and a sound insulation performance of T-3 or higher as defined in JIS A 4706.

  The case where the laminated glass manufacturing method of the present invention is manufactured using two sheets of glass will be described.

  As the intermediate film used in the method for producing laminated glass of FIG. 1, a three-layer structure in which a resin A film is sandwiched between resin B films as shown in FIG.

  The method for producing a laminated glass of the present invention can be applied to a laminated glass produced using at least one intermediate film having a three-layer structure shown in FIG. 2 and using at least two or more glasses.

  When three or more glasses are used, EVA or PVB may be used in addition to the intermediate film shown in FIG.

  For the resin A, a resin selected from resins obtained by copolymerizing styrene and a rubber-based resin monomer can be suitably used. For the resin B film, a PVB-based interlayer resin for laminated glass (for example, Sekisui Chemical Co., Ltd. (trade name) S-LEC film), EVA (for example, Sekisui Chemical Co., Ltd. (trade name) S-LEC EN film, Tosoh Corporation (trade name) Mersen G), ethylene- One or more resins selected from (meth) acrylic ester, urethane and vinyl chloride are preferably used.

  In particular, the resin A is preferably a resin obtained by copolymerizing styrene and a rubber-based resin monomer, and more preferably a resin obtained by hydrogenating a styrene / isoprene / butadiene block copolymer.

  As the rubber resin, isoprene rubber, butadiene rubber, styrene-butadiene rubber (SBR), acrylonitrile-butadiene rubber, chloroprene rubber, butyl rubber, urethane rubber, acrylic rubber, or the like can be used.

  In the multilayer intermediate film in which the resin A film is sandwiched between the resin B films, the thickness of the resin B film is in the range of 0.1 to 1.0, where the thickness of the resin A film is 1. It is also desirable that the thickness of the multilayer intermediate film in which the resin A film is sandwiched between the resin B films is 0.2 mm or more.

  This is because the sound insulation performance of the laminated glass produced by sandwiching the multilayer intermediate film between two glass plates is effective. Moreover, it is preferable that thickness is 0.2 mm or more and 2 mm or less from handling of the intermediate film when producing laminated glass.

  In the laminated glass 1 formed by laminating the glass plates 2 and 4 of FIG. 1 with the multilayer intermediate film 3 shown in FIG. 2, the damping effect increases as the loss factor (loss factor) η of the multilayer intermediate film 3 used for lamination increases. It is expected to be large and have high sound insulation performance.

  The loss factor η is obtained by η = E ′ / 2πE, where E is vibration energy applied to the member and E ′ is energy converted into heat during one cycle, and indicates the degree of vibration energy absorption.

  The loss factor η at 1 kHz of the polyvinyl butyral (PVB) film conventionally used for laminated glass is 0.06, and the loss factor η of the resin A is about 0.1.

  Further, when the temperature dependency of the sound insulation performance is viewed in terms of tan delta (tan δ), the tan delta (tan δ) of the resin A is 0.4 to 0.4 compared to the tan delta (tan δ) of PVB of 0.1 to 0.2. 2.0 shows a larger value than that of the PVB film although it varies depending on the temperature.

  The tan delta (tan δ) is obtained in a dynamic viscoelasticity test and is defined as a ratio of a loss elastic modulus to a storage elastic modulus, and can be measured by an apparatus suitable for measuring the viscoelasticity of a solid material. Examples of this device include RHEOVibron DDV-III manufactured by Orientec. The value of tan delta (tan δ) between the PVB and the resin A was obtained by measuring the storage elastic modulus and elastic modulus under the conditions of the tensile mode, the vibration frequency 11 Hz, and the temperature rising rate 2 ° C./min. It is a value in the range of ° C., and the tan delta (tan δ) 2.0 of the resin A is a peak value indicated at a temperature of −15 ° C.

  Both loss factor η and tan delta (tan δ) are larger in resin A than PVB, and if laminated glass is made using resin A, the sound insulation performance is superior to laminated glass produced using a PVB film. .

  Further, by producing a laminated glass using a resin A film having a loss factor η of 0.07 or more and a tan delta (tan δ) of 0.2 or more, a sound insulation rating T-3 or more defined in JIS A 4706 is obtained. A laminated glass having sound insulation performance is obtained.

  When the laminated glass 1 is produced using the multilayer interlayer film of FIG. 2, the multilayer interlayer film 3 is laminated between a pair of glasses 2 and 4 (step 1), and the temperature is higher than the melting point of the resin A and lower than the melting point + 10 ° C. A pretreatment for heat bonding is performed while deaeration within a range (step 2).

  Deaeration is performed by, for example, placing a multilayer interlayer film 3 sandwiched between a pair of glasses 2 and 4 in a rubber vacuum bag, and pulling the air in the rubber vacuum bag with a vacuum pump, Preferably it is done.

It is preferable to start deaeration at room temperature, and after the pressure in the vacuum bag reaches 4 × 10 ³ Pa or less, heat treatment is performed. Moreover, it is preferable to perform heat processing in the range whose pressure in a vacuum bag is 1 * 10 < ⁰ > -4 * 10 < ³ > Pa.

When the pressure is larger than 4 × 10 ³ Pa, sufficient degassing becomes difficult and air remains, so it is desirable that the deaeration be 4 × 10 ³ Pa or less. Further, if the deaeration pressure is smaller than 1 × 10 ⁰ Pa, it takes time to reach the pressure and the productivity deteriorates. Therefore, the pressure in the reduced pressure state is 1 × 10 ⁰ to 4 × 10 ³ Pa. It is desirable to do.

  Heating may be performed immediately after reaching the pressure, but more preferably, holding at room temperature for about 10 minutes after reaching the pressure is preferable because degassing can be performed more sufficiently.

  In addition to using the rubber vacuum bag, the deaeration may be performed by a ring method in which the peripheral portion is covered with a rubber tube and vacuumed, or a roll method in which pressure is applied using a roll.

  Heating is performed in a temperature range from (melting point of resin B) to (melting point of resin B + 10 ° C., and heating temperature in step 3 described later) while keeping the degassed state, for example, with the rubber vacuum bag closed. However, although not particularly specified, it is preferably performed for about 10 minutes to 40 minutes.

  If the heating temperature is lower than the melting point of the resin B, the transparency of the laminated glass tends to be impaired due to poor deaeration of the laminated glass. Therefore, it is preferable that the heating temperature of the pretreatment in step 2 is not less than the melting point of the resin B and not more than the heating temperature of the step 3 described later, more preferably not more than the melting point of the resin B + 10 ° C.

  The laminate obtained by the pretreatment in step 2 may be brought into an atmospheric pressure state by, for example, opening a rubber vacuum bag from a state where it is immediately deaerated. Since air bubbles easily enter the interlayer film, it is preferable to set the pressure to atmospheric pressure after the laminate has cooled to near room temperature.

  The appearance of the laminate obtained by the pretreatment in step 2 does not necessarily need to be colorless and transparent, and remains undissolved on the surface irregularities of the intermediate film in contact with the glass, or a part that appears entirely or partially white If the haze of the laminated body after cooling is 40% or less even if it remains, it can be dissolved in the subsequent step 3, and a transparent laminated glass is obtained.

  If the haze is 40% or more, a laminated glass having a good appearance cannot be obtained even if it is finished and bonded in Step 3.

  Therefore, it is preferable to select a laminate having a haze of 40% or less from the laminate obtained in step 2 and perform the heat and pressure bonding in the next step 3. This heat and pressure bonding can be performed using an autoclave furnace.

  The heating time is not particularly defined but is preferably about 20 to 90 minutes. The pressurizing pressure is about 0.25 to 1.3 MPa, and the higher the pressurizing pressure, the shorter the heating time.

  When laminated glass is produced by the process as described above, laminated glass having no optical defects, high impact resistance, and almost no undissolved surface irregularities on the intermediate film in contact with the glass is obtained. Can do.

Example 1
For the resin A film, a styrene / isoprene / butadiene block copolymer containing 12% by weight of styrene and 88% by weight of isoprene / butadiene and having a melt flow rate of 2 g / 10 min in accordance with ASTM D1238 is water. An accompanying resin was used. The thickness of the resin A film 26 was 0.20 mm.

  For the resin B film, an EVA-based resin (trade name Mersen G7055, manufactured by Tosoh Corporation) was used.

  A film of resin A was formed between films of resin B having a thickness of 0.05 mm to produce a multilayer intermediate film 3 having a thickness of 0.30 mm having a three-layer structure as shown in FIG.

  The loss factor η of the multilayer film 3 was 0.13, and the tan delta (tan δ) was 0.8 (value at 0 ° C.).

The multilayer intermediate film 3 is inserted between two sheets of float sheet glass having a thickness of 4 mm and a size of 1930 mm × 864 mm, and the multilayer interlayer film 3 stacked between the glasses 2 and 4 is put in a rubber vacuum bag, After the air in the rubber vacuum bag was drawn to reach a pressure of 4 × 10 ³ Pa, the reduced pressure state was maintained for 10 minutes.

  While maintaining the pressure of the rubber vacuum bag, the rubber vacuum bag having the laminated body of the glass 2 and 4 and the multilayer intermediate film 3 placed therein is transferred to an oven, and the melting point of the resin B + 80 ° C. of 5 ° C. Heat at 40 ° C. for 40 minutes.

  Next, the rubber vacuum bag was opened, and the produced laminate was cooled to room temperature and taken out from the rubber vacuum bag. The haze of this laminate was about 0.3 to 40%.

  Next, using an autoclave, the heating temperature was 90 ° C. of the melting point of the resin B + 15 ° C., the pressure was 0.25 MPa, the pressure was maintained for 20 minutes, and heat and pressure bonding was performed to obtain a laminated glass.

Example 2
A laminated glass was produced in the same procedure as in Example 1 except that the autoclave holding time was 40 minutes and the pressure was 1.3 MPa.

Comparative Example 1
A laminated glass was produced in the same procedure as in Example 1 except that the heating temperature of the autoclave was 130 ° C., the holding time was 30 minutes, and the pressing pressure was 1.3 MPa.

Comparative Example 2
A laminated glass was produced in the same procedure as in Example 1 except that the heating temperature of the autoclave was 75 ° C., the holding time was 30 minutes, and the pressing pressure was 1.3 MPa.

Comparative Example 3
The laminated body obtained in Example 1 was put in a rubber vacuum bag, depressurized to 1 × 10 ⁰ to 4 × 10 ³ Pa for 10 minutes, then transferred to an oven, and the temperature of the resin B film reached 130 ° C. Then, heating was performed for 20 minutes. Thereafter, the rubber vacuum bag was opened, the laminate was cooled to room temperature, and a laminated glass was produced.

Comparative Example 4
The laminated body obtained in Example 1 is put in a rubber vacuum bag, depressurized to 1 × 10 ⁰ to 4 × 10 ³ Pa for 10 minutes, then transferred to an oven, and the temperature of the resin B film reaches 90 ° C. Thus, heating was performed for 20 minutes. Thereafter, the rubber vacuum bag was opened and the laminate was cooled to room temperature to produce a laminated glass.

Comparative Example 5
The laminated body obtained in Example 1 is put in a rubber vacuum bag, depressurized to 1 × 10 ⁰ to 4 × 10 ³ Pa for 10 minutes, then transferred to an oven, and the temperature of the resin B film reaches 75 ° C. Thus, heating was performed for 20 minutes. Thereafter, the rubber vacuum bag was opened, and the laminate was cooled to room temperature to produce a laminated glass.
[Characteristic evaluation of laminated glass]
By evaluating the following items, the characteristics of the laminated glasses produced in Examples 1-2 and Comparative Examples 1-5 were evaluated. The evaluation results are shown in Table 1. In Table 1, evaluation items 2 to 4 were not evaluated for comparative examples in which evaluation item 1 was defective.

  Evaluation item 1: Appearance inspection was performed according to JIS R 3205 to determine whether haze was good or bad.

  Evaluation item 2: When the laminated glass is illuminated with a halogen lamp, and the light transmitted through the laminated glass has an optical defect that is observed by coloring the laminated glass while changing the incident angle of the light of the halogen lamp and the observation direction. Was evaluated as x, and the case where there was no was evaluated as ○.

  Evaluation item 3; A shot bag test (L2-2) was conducted in accordance with JIS R 3205 to determine pass / fail.

  Evaluation item 4: The sound insulation performance was inspected according to JIS A 4706, and the pass / fail of the sound insulation grade T-3 was determined.

It is a schematic sectional drawing which shows the structure of a laminated glass. It is a schematic sectional drawing which shows the structure of the intermediate film used for a laminated glass.

Explanation of symbols

1 Laminated Glass 2 Glass 3 Intermediate Film 4 Glass 31 Resin B Film 32 Resin A Film 33 Resin B Film

Claims (7)

  In the method for producing a laminated glass in which two or more glasses are laminated using an intermediate film, (Step 1) having a three-layer structure in which a layer made of resin A exhibiting rubber elasticity is sandwiched between layers of thermal adhesive resin B Using an intermediate film and two or more glasses, the intermediate film is inserted between the glasses to form a laminate. (Step 2) In a temperature range from the melting point of the resin B to the melting point of the resin B + 10 ° C. A pretreatment for heat bonding is performed while degassing, and then (step 3) the laminate obtained in step 2 is 0.25 MPa to 1. ° C. in a temperature range of melting point of resin B + 10 ° C. to melting point of resin B + 15 ° C. A method for producing a laminated glass, characterized in that heat-pressure bonding is performed under a pressure of 3 MPa.   2. The laminated glass according to claim 1, wherein a laminate having a haze of 40% or less is selected from the laminate obtained in step 2, and the selected laminate is bonded by heating and pressing in step 3. Method.   Resin A consists of a copolymer of styrene and a rubber-type resin monomer, The manufacturing method of the laminated glass in any one of Claim 1 or 2 characterized by the above-mentioned. Method for producing a laminated glass according to any one of claims 1 to 3 film thickness of the film of the heat-adhesive resin B is characterized in that it is 0.01mm or more 0.1mm or less.   The method for producing a laminated glass according to any one of claims 1 to 4, wherein the deaeration in step 2 is performed using a rubber vacuum bag or tube. The method for producing a laminated glass according to any one of claims 1 to 5, wherein the deaeration in step 2 is performed in a range of 1 x 10 ⁰ to 4 x 10 ³ Pa.   The thickness of one glass is 3 to 5 mm, the total thickness of the two glasses is 8 to 10 mm, and the intermediate film has a thickness of 0.2 to 1 mm. A laminated glass produced by the manufacturing method according to claim 6 and having a sound insulation performance of sound insulation grade T-3 or higher as defined in JIS A 4706.

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