JPH0158139B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a method for manufacturing laminated glass. The conventional manufacturing method for laminated glass, especially heat-reflecting laminated glass, is to first coat a resin film such as polyethylene terephthalate or nylon-6 with a film of 1×10 ^-5 to 5×10 ^-5 .
At least one selected from metals and metal oxides, such as gold, silver, TiO ₂ , tungsten oxide, etc., by continuous vacuum evaporation or continuous sputtering while continuously feeding the film in a mmHg (Torr) vacuum chamber. A heat ray reflective film is created by continuously depositing metals or metal oxides of Furthermore, two sheets of inorganic glass or organic glass were superimposed on the outer surface of the film-like adhesive, and then they were laminated by thermocompression bonding in an autoclave.
However, this method of manufacturing laminated glass has the problem that wrinkles occur in the heat ray reflective film of the completed laminated glass. The inventors of the present invention conducted various studies on the cause of this problem, and as a result, they confirmed that the water content in the heat ray reflective film greatly influences the occurrence of wrinkles when pressurizing the glass to form laminated glass. In other words, during the manufacturing process, the heat ray reflective film is placed under high vacuum during vacuum deposition or sputtering, and in a bath with a temperature of 40 to 90°C, so that most of the water originally contained in the film evaporates. At the time of completion, the moisture content is 0.1~
It becomes 0.5% by weight. Moreover, if the heat ray reflective film is continuously wound up in the same tank and immediately packaged, almost no moisture is absorbed by the heat ray reflective film.
When such a heat ray reflective film with a low water content is laminated as it is on inorganic glass or organic glass via two film-like adhesive layers, that is, a layer of polyvinyl butyral, and is laminated by thermocompression bonding in an autoclave, it is possible to It has been found that during pressing, the heat ray reflective film absorbs moisture from the adjacent adhesive, ie, polyvinyl butyral, and as a result, the heat ray reflective film stretches and wrinkles. This invention was made in view of these conventional problems, and it is possible to improve the moisture content of a heat ray reflective film made of a resin film, particularly a nylon-6 film, to which a metal or metal oxide is attached as a base material, from 1.0 to 1.0. 7.5
% by weight, and stack the heat ray reflective film in this state in the following order: organic glass or inorganic glass/adhesive layer/humidity controlled heat ray reflective film/adhesive/organic glass or inorganic glass. The object of the present invention is to solve the above-mentioned problems by thermocompression bonding and laminating to form a laminated glass. Therefore, the method for manufacturing laminated glass of the present invention is characterized by controlling the humidity before laminating the heat ray reflective film so that the moisture content immediately before lamination is 1.0 to 7.5% by weight. If the moisture content of the heat ray reflective film immediately before lamination is less than 1.0% by weight, wrinkles will occur too much, which is inappropriate; if it exceeds 7.5% by weight, the heat ray reflective film will turn bluish and the visible light transmittance will decrease. This is not preferable because it significantly reduces the Hereinafter, this invention will be explained based on examples. FIG. 1 is an explanatory cross-sectional view of laminated glass produced by the manufacturing method of the present invention. 1 and 1' are inorganic glass, 2 and 2' are adhesives, ie, polyvinyl butyral, and 3 is a heat ray reflective film made of a resin film to which metal or metal oxide is attached. Example 1 A nylon-6 film with a width of 1000 mm and a thickness of 37 μm was taken up in a vapor deposition device at a film winding speed of 2.0 m/min.
sec, vacuum level 1×10 ^-5 mmHg (Torr), gold and silver
0.018-0.027g/ ^m2 , Ag 0.045-0.073g/ ^m2
A heat ray reflective film was prepared by vapor depositing at a ratio of 200 Å to a thickness of 200 Å. As a preliminary experiment, we determined the relationship between humidity control conditions and moisture content of a heat ray reflective film. First, six sheets of heat ray reflective film prepared by the above method were held in a vacuum dryer in a state where they were separated from each other so as not to come into contact with each other, and heated to 50°C.
Dry for an hour. The weight W ₀ of this dried heat ray reflective film was measured. Next, the five dried heat-reflecting films were placed in a constant temperature and humidity chamber at a temperature of 20°C and a relative humidity of 20% for 40 minutes.
%, 60%, 80%, and 95% after holding each for 24 hours.
The weight was measured using a balance, and the weight was defined as _W1 . The moisture content was calculated as W ₁ −W ₀ /W ₀ ×100 (%), and the results are shown in FIG. Next, seven heat ray reflective films were deposited with gold and silver under the conditions described above, and a nylon-6 film was prepared without changing the deposition conditions.
Three heat ray reflective films with a diameter of 25 μm were used, and 20%, 30%, and 40% for a 37 μm heat ray reflective film.
%, 50%, 60%, 70%, 95%, and 25 μm heat ray reflective films are heated at 20°C for 24 hours with the front and back sides of the film in contact with the above atmosphere for 20%, 30%, and 60%. Immediately after adjusting the humidity under the conditions, measuring the weight and measuring the moisture content, inorganic glass (thickness 2.0
mm) / Polyvinyl butyral as adhesive layer (thickness 0.76 mm) / Humidity-controlled heat ray reflective film / Polyvinyl butyral as adhesive layer (thickness 0.38 mm)
mm)/inorganic glass (thickness 2.0 mm),
After vacuum degassing, they were thermally compressed and laminated at a temperature of 120° C. and a pressure of 12.5 kg/cm ² for 30 minutes to produce 10 laminated glasses A to J having the cross-sectional shapes shown in FIG. The size of the completed laminated glass was 50m x 150mm.
The occurrence of wrinkles in the heat ray reflective films of these 10 laminated glasses A to J was investigated, and the results are shown in Table 1 along with the moisture content. The wrinkles are 1 inch square, or 25.4 mm x
Expressed by the number of wrinkles of 25.4 mm. Comparative Example 1 Example 1 is based on two humidity control conditions: 37 μm and 25 μm.
Relative humidity of 0% and 10% for heat reflective film of seeds
Four types of laminated glass, K to N, were created under the same conditions except for the change in %. The moisture content and the incidence of wrinkles in the heat ray reflective film were measured and are listed in Table 1.

【table】

[Table]
Example 2 Two types of heat ray reflective films with thicknesses of 37 μm and 25 μm created in the same manner as the heat ray reflective film created in Example 1 were immersed in water for 60 minutes, and then the thickness
For 37μm films, dry in a drying oven at 60°C.
The film with a thickness of 25 μm was kept in a drying oven at 60° C. for 10 minutes to control the humidity, and two types of humidity-controlled heat ray reflective films were prepared. After humidity conditioning, measure the moisture content and immediately apply inorganic glass (thickness 2.0mm) / polyvinyl butyral as adhesive layer (thickness 0.38mm) / heat ray reflective film for humidity conditioning /
Polyvinyl butyral as adhesive layer (thickness
0.38mm) / inorganic glass (thickness 2.0mm), and after vacuum degassing, the temperature was 120℃ and the pressure was 12.5Kg/ ^cm2.
Laminated glasses O and P were created by thermocompression bonding for 30 minutes. The degree of wrinkling of the heat ray reflective film of these laminated glasses was investigated, and the results are shown in Table 2 along with the moisture content. Comparative Example 2 Thickness 37μm and 25μm created in the same manner as Example 1
Two kinds of heat ray reflective films were immersed in water for 60 minutes. Next, three types of heat-reflecting films with a diameter of 37 μm were created: one that was simply drained, one that was kept in a drying oven maintained at 60°C for 5 minutes, and one that was kept for 10 minutes under different humidity control conditions. In addition, for heat ray reflective films with a thickness of 25 μm, those that are simply soaked in water and then drained, and
Heat-reflecting films were created using different humidity control conditions, including one in a drying oven maintained at 60°C and the other in a drying oven held for 5 minutes.
Immediately after measuring the moisture content of these five types of heat ray reflective films, five types of laminated glasses Q, R, S, T, and U were created in the same manner as in Example 2. The degree of wrinkle occurrence was investigated in the same manner as in Example 2 and is shown in Table 2 along with the moisture content.

[Table] Expressed by numbers.
Comparative Example 3 A nylon-6 film with a thickness of 37 μm, a width of 1000 mm, and a length of 100 m was placed in a vapor deposition tank at a vacuum level of 1×10 ^-5 mmHg.
Silver was continuously deposited to a thickness of 200 Å while winding the film at a film winding speed of 2.0 m/sec (Torr). The wound roll of the heat ray reflective film prepared in this way was stored in a constant temperature and humidity chamber at a temperature of 20°C and a relative humidity of 60%, and the central part (X part) of the roll and 80% of the outside diameter of the roll were Part (Y part) and outside (Z part)
In addition, in the width direction, the initial moisture content of the center portion and the moisture content over time were measured. The results are shown in FIG. After 100 days, measure the length of each part of X, Y, and Z.
Cut to 1500mm, inorganic glass (thickness 2.0mm) / polyvinyl butyral as adhesive layer (thickness 0.37mm)
mm) / X, Y or Z / Polyvinyl butyral as adhesive layer (thickness 2.0 mm) / Inorganic glass (thickness
2.0mm), and after vacuum degassing,
Three types of laminated glass were produced by thermocompression bonding and lamination in an autoclave for about 40 minutes at a temperature of 120° C. and a pressure of 13.0 Kg/cm ² . When we investigated the occurrence of wrinkles in the heat ray reflective film of these laminated glasses, we found that
The one using heat ray reflective film in the X part is 25.4mm×
Number of wrinkles per 25.4mm: 20, same for Y: 19, Z: 0
Therefore, sufficient humidity control could only be achieved in the outer area. In other words, it can be seen that the external atmosphere has no effect on the moisture content inside the roll when it is wound onto a roll. From Tables 1 and 2 showing the results of the above Examples and Comparative Examples, the moisture content of the heat ray reflective film is
By adjusting the humidity to 1.0% by weight or more before laminating it with adhesives, glass, etc., it is possible to prevent the generation of wrinkles in the heat ray reflective film of laminated glass, and also to control the humidity to a moisture content of 7.5% by weight or less. It can be seen that discoloration of the heat ray reflective film can be prevented by laminating the heat ray reflective film. Further, as shown in FIG. 1, the humidity control conditions are preferably to maintain the relative humidity at 20° C. and about 20% or more for 24 hours. Also, to control humidity in a single hour, from Table 2, after immersing the film in water for 60 minutes, if the film thickness is about 25 μm, it will take more than 10 minutes, and if it is about 37 μm, it will take more than 10 minutes to dry in a drying oven at 60℃. A method such as putting it in a container is preferable. Furthermore, as is clear from Comparative Example 3, when controlling the humidity, it is necessary to expose both the front and back sides of the heat ray reflective film to a predetermined atmosphere. Therefore, it is not necessary to adjust the humidity while the heat ray reflective film is rolled up. Instead, it is necessary to cut it into a predetermined size and hold it so that both sides are exposed to the atmosphere while controlling the humidity, or to adjust the humidity with a gap between the heat ray reflective films. It is preferable to adjust the humidity by opening the container and winding it up with a spacer interposed therebetween. As explained above, according to this invention,
A resin film to which a metal or metal oxide is attached, that is, a heat ray reflective film, is bonded through an adhesive layer.
In the method of manufacturing laminated glass by laminating sheets of inorganic or organic glass, the humidity of the heat ray reflective film is adjusted before lamination to bring the moisture content to 1.0 to 7.5% by weight just before lamination. , the effect that the heat ray reflective film installed in the manufactured laminated glass is free from wrinkles and discoloration can be obtained.

[Brief explanation of drawings]

Fig. 1 is a cross-sectional view of laminated glass manufactured by the manufacturing method of the present invention, Fig. 2 is a graph showing the relationship between the equilibrium water content (wt%) and relative humidity of a heat ray reflective film, and Fig. 3 is a graph showing the relationship between the equilibrium moisture content (wt%) and relative humidity of a heat ray reflective film. It is a graph showing the relationship between the position of the heat ray reflective film and the moisture content. 1, 1'... Inorganic glass, 2, 2'... Adhesive layer, 3... Heat ray reflective film.

Claims (1)

[Claims] 1. A resin film to which at least one metal or metal oxide selected from the group consisting of metals and metal oxides is attached is laminated so as to be sandwiched between two sheets of inorganic glass or organic glass via an adhesive layer. In the method for manufacturing laminated glass, the humidity is controlled before laminating the resin film, and the moisture content is adjusted to 1.0 just before lamination.
7.5% by weight.