INTERMEDIATE LAYER FILM FOR LAMINATED GLASS

专利摘要:
INTERMEDIATE LAYER FILM FOR LAMINATED GLASS AND LAMINATED GLASS. The present invention relates to an intermediate layer film for laminated glass including 2 or more resin layers laminated on top of each other, exhibits excellent deaeration properties in a laminated glass manufacturing process, and can prevent ghosting and refers to laminated glass that includes the interlayer film for laminated glass. The film in question has a large number of indentations and a large number of bulges on at least one surface thereof. Within the surface having the large number of recesses and the large number of protrusions, a groove depth (Rzg) of the recesses measured based on JIS B-0601(1994) is 10 ()m to 40 ()m, an average roughness of 10 points (Rz) of a surface of the resin layer and the large number of bulges measured based on JIS B 0601 (1994) is less than 2.7 ()m.
公开号:BR112016002064B1
申请号:R112016002064-2
申请日:2014-08-01
公开日:2022-01-04
发明作者:Hirofumi Kitano；Hiroaki Inui；Taiki Katayama；Manabu Matsumoto；Kazuhiko Nakayama
申请人:Sekisui Chemical Co., Ltd；
IPC主号:

专利说明:

FIELD OF TECHNIQUE
[0001] The present invention relates to an intermediate layer film for laminated glass that includes 2 or more layers of resin laminated on top of each other, exhibits excellent deaeration properties in the laminated glass manufacturing process, and can prevent the occurrence of ghost images. The present invention also relates to laminated glass which includes the interlayer film for laminated glass. BACKGROUND OF THE TECHNIQUE
[0002] Laminated glass, which is obtained by sandwiching an interlayer film for laminated glass that contains a thermoplastic resin, such as thermoplastic polyvinyl butyral, between two sheets of glass and bonding the interlayer film to the glass plates. glass, it is widely used in window glass for automobiles, aircraft, buildings and the like.
[0003] The intermediate layer film for laminated glass can consist not only of a single layer of resin, but also of a laminate composed of 2 or more layers of resin. If the 2 or more resin layers are composed of a first resin layer and a second resin layer and the properties of the first resin layer are different from the properties of the second resin layer, an intermediate layer film for laminated glass can be provided, which has various performances that are not easily accomplished with just a single layer.
[0004] For example, PTL 1 discloses an intermediate layer film for laminated glass that has a 3-layer structure composed of a soundproofing layer and 2 protective layers that interpose the soundproofing layer between them. PTL 1 laminated glass interlayer film includes the soundproofing layer which contains a polyvinyl acetal resin, which has excellent affinity for a plasticizer and a large amount of a plasticizer, and consequently the interlayer film exhibits excellent sound insulation. However, the protective layers prevent the adhesion between the intermediate layer film and the glass from deteriorating due to the bleeding of a large amount of the plasticizer contained in the soundproofing layer.
[0005] However, laminated glass using such an intermediate layer film for laminated glass that includes 2 or more resin layers laminated on top of each other has the following problem. That is, when external light rays are visually recognized through laminated glass, images are seen as ghost images in some cases or optical deformation is recognized in some cases. The occurrence of ghost images or optical deformation is markedly observed, particularly in the case of the interlayer film for laminated glass which has excellent sound insulation properties which is described in PTL 1. CITATION LIST
[0006] Patent Literature
[0007] PTL 1 JP-A-2007-331959 SUMMARY OF THE INVENTION TECHNIQUE PROBLEM
[0008] The present inventors have analyzed the cause of the occurrence of ghost images in the case of using the interlayer film for laminated glass that includes 2 or more layers of resin laminated one on top of the other. As a result, they found that indentations and bulges formed on a surface of the laminated glass interlayer film are the causes.
[0009] In general, when manufacturing laminated glass, a laminate, in which an intermediate layer film for laminated glass is laminated between at least 2 sheets of glass sheets, is passed through and passed through the throttling cylinders (a deaeration method). - pressing) or placed in a rubber bag and aspirated under reduced pressure (a vacuum deaeration method). In this way, while the air that remains between the glass plate and the interlayer film is being removed, the laminate is pressed together. Therefore, by pressure joining the laminate by means of heating and pressing it in, for example, an autoclave, laminated glass is manufactured. In the laminated glass manufacturing process, the deaeration properties at the time of laminating the glass with the laminated glass interlayer film are important. In order to obtain deaeration properties at the time of laminated glass fabrication, indentations and fine protrusions are formed on at least one surface of the interlayer film for laminated glass. Particularly, in the recesses and protrusions, if the recesses have a structure in which each recess has a groove shape with a continuous bottom (hereinafter, the shape will also be referred to as a "notched line shape") and the recesses adjacent to each other that are in the form of notched lines are parallel to each other and formed evenly, the laminated glass interlayer film can exhibit extremely excellent deaeration properties.
[0010] In general, the recesses and protrusions formed on the surface of the laminated glass interlayer film are destroyed at the time of pressure joining in the laminated glass manufacturing process. Therefore, recesses and protrusions rarely become a problem in the obtained laminated glass.
[0011] However, the present inventors have found that in the case of the interlayer film for laminated glass that includes 2 or more resin layers laminated on top of each other, the influence of the recesses and protrusions remains in the laminated glass obtained through the manufacturing process of laminated glass and causes ghosting to occur.
[0012] That is, it was considered that when indentations and protrusions are formed on a surface of laminated glass interlayer film that includes 2 or more layers of resin laminated on top of each other through the use of a cylinder of go- Fragment or similar, the indentations and bulges are formed on the surface of the intermediate layer film and are also transferred to the interface between the resin layers due to the pressure at the working time, and then the interface becomes non-smooth. In particular, it was considered that if recesses that are in the shape of a notched line are formed on the surface, the recesses that are in the shape of a notched line are also apparently transferred to the interface between the layers. Although the indentations and bulges on the surface of the interlayer film are destroyed at the time of pressure joining in the laminated glass manufacturing process, the indentations and bulges that were transferred to the interface between the layers remain. It was considered that due to the indentations and bulges formed at the interface between the layers, an optical interference phenomenon occurs and this causes the occurrence of ghost images. In particular, it has been found that in the interlayer film for laminated glass having excellent sound insulation properties described in PTL 1, when recesses and bulges are formed on a surface of a rigid protective layer, the recesses and bulges are easily transferred to the interface between the protective layer and the soft sound insulation layer, and so ghosting in particular occurs easily.
[0013] If indentations and bulges are not formed on the surface of the laminated glass interlayer film, ghosting can be prevented. However, if the indentations and bulges are not formed, the air cannot be sufficiently removed at the time of manufacturing the laminated glass. Consequently, air bubbles occur between the glass and the interlayer film and thus the external appearance of the laminated glass is degraded.
[0014] The present invention has been made in consideration of the aforementioned circumstances and the objects of the same are to provide an intermediate layer film for laminated glass that includes 2 or more layers of resin laminated one on top of the other, which exhibits excellent deaeration properties. in a laminated glass manufacturing process and can prevent ghosting and provide laminated glass that includes the laminated glass interlayer film. SOLUTION TO THE PROBLEM
[0015] In accordance with one aspect of the present invention, there is provided an intermediate layer film for laminated glass that includes 2 or more layers of resin laminated on top of each other that have a large number of recesses and a large number of protrusions at least least one surface thereof, each of the recesses has a groove shape with a continuous bottom, the recesses adjacent to each other are parallel to each other and regularly arranged in a line, within the surface which includes a large number of recesses and a large number of protrusions, a groove depth (Rzg) of the grooves measured based on JIS B-0601(1994) is 10 μm to 40 μm and an average roughness of 10 points (Rz) of a surface of a resin layer that has the surface that includes the large number of recesses and the large number of protrusions measured on the basis of JIS B 0601(1994) is less than 2.7 μm and the average roughness of 10 points (Rz) is obtained by removing the layer in resin having the surface that includes the large number of recesses and the large number of protrusions from another resin layer that comes into direct contact with the aforementioned resin layer and thereby measuring the surface of the removed layer in one side of another previously mentioned resin layer that came into direct contact with the removed resin layer based on JIS B 0601(1994).
[0016] In the aspect of the present invention, a state in which "the middle layer film has a large number of recesses and a large number of protrusions on at least one surface thereof" means that "a large number of recesses and a large number of of bulges were formed on at least one surface of the interlayer film". Furthermore, a state in which "each of the recesses has a groove shape with a continuous bottom and the recesses adjacent to each other are parallel to each other and arranged in a line" means that "each of the recesses has a groove with a continuous bottom and the recesses adjacent to each other are parallel to each other and formed regularly".
[0017] Hereinafter, the present invention will be specifically described.
[0018] As a result of intensive research, the present inventors have found the following fact. If the recesses and bulges are formed on a surface of the laminated glass interlayer film to such an extent that the interlayer film can exhibit sufficient deaeration properties in the laminated glass manufacturing process and the roughness of the recesses and ridges to be transferred to the interface between a layer of resin, which has the surface on which the indentations and protrusions are formed, and a layer of resin that comes into direct contact with the aforementioned resin layer, is maintained to be equal to or less than a certain level, even in an intermediate layer film for laminated glass that includes 2 or more layers of resin laminated on top of each other, both of excellent deaeration properties at the time of laminated glass manufacturing and the prevention of ghosting can be established. Based on these findings, the present inventors have carried out the present invention.
[0019] The laminated glass interlayer film of the present invention has a large number of recesses and a large number of protrusions on at least one surface thereof. Consequently, deaeration properties can be obtained at the time of laminated glass manufacturing.
[0020] The intermediate layer film of the present invention may have the indentations and bulges only on one surface thereof. However, the intermediate layer film preferentially has indentations and bulges on both surfaces of it, due to the fact that the deaeration properties are markedly improved.
[0021] The indentations and bulges can be at least shaped like a groove. For example, the recesses and protrusions may have a shape that is generally given to the surface of the laminated glass interlayer film, such as the shape of a notched line or the shape of a lattice. The recesses and protrusions may have a shape that has been transferred from an embossing cylinder.
[0022] Also, the top of the recesses can have a flat shape as shown in Figure 1 or it can have a non-flat shape as shown in Figure 2. When the top of the recesses have a flat shape, the recesses and thin protrusions can be additionally formed at the top.
[0023] In the recesses and bulges, the heights of the bulges can be the same or different from each other. Furthermore, the thicknesses of the recesses that correspond to the protrusions can be the same or different from each other, while the bottom side of the recesses is continuous.
[0024] In the laminated glass interlayer film of the present invention, among the recesses and protrusions that the interlayer film has on at least one surface thereof, each recess has a groove shape with a continuous bottom (a shape of notched lines) and the recesses adjacent to each other are parallel to each other and regularly arranged in a line. Generally, when a laminate in which an interlayer film for laminated glass has been laminated between 2 sheets of glass plates is pressure bonded, the ease with which air is removed is strictly related to the communication properties and smoothness of the bottom of the recesses. . If the indentations and protrusions on at least one surface of the intermediate layer film are shaped so that the indentations that are shaped like a notched line are parallel to each other and regularly arranged in a line, the communication properties of the background make it better and the deaeration properties are markedly improved.
[0025] In the present document, "evenly arranged in a line" means that recesses adjacent to each other that are in the shape of a notched line may be parallel to each other and arranged in a line at an equal interval. The phrase also means that although recesses adjacent to each other that are shaped like a notched line are parallel to each other and laid out in a line, the gap between all recesses adjacent to each other that are shaped like a notched line can not be an equal range.
[0026] Figures 1 and 2 are schematic views showing an example of an intermediate layer film for laminated glass in which the recesses that have the shape of a notched line are parallel to each other and arranged in a line at an equal interval.
[0027] Figure 3 is a schematic view showing an example of an intermediate layer film for laminated glass in which the recesses that have the shape of a notched line are parallel to each other and arranged in a line at an unequal interval. In Figure 3, an interval A between a groove 1 and a groove 2 is different from an interval B between groove 1 and a groove 3.
[0028] Within the surface which has the large number of recesses and the large number of bulges, a groove depth (Rzg) of the recesses is 10 μm to 40 μm. If the groove depth (Rzg) is equal to or greater than 10 μm, the intermediate layer film can exhibit extremely excellent deaeration properties and if it is equal to or less than 40 μm, the temperature at the time of laminated glass manufacture can be reduced. The lower limit of the groove depth (Rzg) is preferably 15 μm and the upper limit thereof is preferably 35 μm. The lower limit of the groove depth (Rzg) is more preferably 20 µm and the upper limit thereof is more preferably 30 µm.
[0029] In the present specification, the groove depth(Rzg) of the recesses refers to a value obtained by calculating a groove depth based on a midline of a roughness curve (a line defined so that the sum of squares of roughness curve deviation is less) by setting a reference length specified in JIS B-0601(1994) "Surface roughness-definition and expression" to be 2.5 mm and then calculating a average depths of the measured grooves. The number of grooves is an integer determined by rounding a value, which is obtained by dividing the reference length by the interval between the grooves, below the decimal point. When the number of grooves is equal to or greater than 5, the 5 groove depths shown in the reference length are calculated in order from the deepest groove of the grooves and the average of the grooves is taken as a groove depth per length of groove. reference. When the number of grooves is equal to or less than 4, the groove depths shown in the reference length are calculated in order from the shallowest groove and the average of them is taken as one groove depth per reference length. The groove depth per reference length is measured for at least 5 grooves of the grooves and their average is taken as the groove depth (Rzg) of the grooves. The groove depth (Rzg) can be easily obtained by running the data process on digital signals measured using, for example, a surface roughness meter (SE1700a manufactured by Kosaka Laboratory Ltd.).
[0030] In the aspect of the present invention, as a method for forming a large number of recesses and a large number of protrusions on at least one surface of the laminated glass interlayer film, for example, it is possible to use a cylinder embossing method. , a roll calendering method, a profile extrusion method, or an extrusion edge embossing method that utilizes melt fracture. Among these, a cylinder embossing method is preferred because the method facilitates obtaining the shape, in which the recesses adjacent to each other that are in the shape of a notched line are parallel to each other and regularly arranged in a line. .
[0031] Examples of the embossing cylinder used in the cylinder embossing method include an embossing cylinder that has embossing patterns (patterns of recesses and bulges) on the cylinder surface that are formed by performing the blasting process on the surface of a cylinder. metal cylinder by using a grinding material, such as aluminum oxide or silicon oxide, and thereby polishing the surface by vertical grinding or similar in order to reduce excessive peaks on the surface. Examples of the embossing cylinder also include an embossing cylinder that has embossing patterns (indentation and protrusion patterns) on the cylinder surface that are formed by transferring embossing patterns (indentation and protrusion patterns) from an engraving milling machine ( milling machine) to the surface of a metal cylinder, an embossing cylinder that has embossing patterns (patterns of recesses and bulges) on the cylinder surface that are formed by means of etching and the like.
[0032] In the laminated glass interlayer film of the present invention, an average roughness of 10 points (Rz) of the surface of the resin layer having the large number of recesses and the large number of protrusions (hereinafter, the resin layer will also be referred to as a "resin layer with the surface having indentations and bulges") measured based on JIS B 0601(1994) is less than 2.7 μm. The average roughness of 10 points (Rz) is obtained by removing the resin layer with the surface having indentations and bulges from another resin layer that comes into direct contact with the resin layer mentioned above, and thus measuring , the surface of the removed resin layer with the surface having indentations and bulges that came into contact with the other resin layer mentioned above based on JIS B 0601(1994).
[0033] As described above, although the indentations and bulges that have been transferred to the interface between the resin layers are the cause of the occurrence of ghost images and the like, it is extremely difficult to directly observe the indentations and bulges of the interface between the resin layers. . The indentations and bulges that have been transferred to the interface between the resin layers can be indirectly evaluated by removing the resin layer that comes into direct contact with another resin layer and measuring the 10-point average roughness of the surface of the resin. layer of resin removed, rather than directly observing the indentations and bulges of the interface between the resin layer. Furthermore, by adjusting the roughness of the recesses and bulges to be less than a certain level, the occurrence of ghost images caused by the transferred recesses and bulges can be inhibited.
[0034] The laminated glass interlayer film shown in Figure 4 is a laminated glass interlayer film that has a 2-layer structure in which the resin layer 20, which has a surface 21 that has a large number of recesses and a large number of protrusions and a resin layer 10 was laminated together. In the present invention, the resin layer 20 is removed from the resin layer 10 of the laminated glass interlayer film having the 2-layer structure, and then the 10-point average roughness (Rz) of a surface 22 of the layer of removed resin 20 on the side that came into contact with the resin layer 10 is measured.
[0035] The laminated glass interlayer film shown in Figure 5 is a laminated glass interlayer film that has a 3-layer structure in which the resin layer 20, which has the surface 21 that has the large number of recesses and the large number of protrusions, the resin layer 10 and a resin layer 30 were laminated on top of each other in that order. In the present invention, the resin layer 20 is removed from the resin layer 10 of the laminated glass interlayer film that has the 3-layer structure, and then the 10-point average roughness (Rz) of the surface 22 of the layer of removed resin 20 on the side that contacts the resin layer 10 is measured.
[0036] The removal of the resin layer that comes into direct contact with another resin layer is carried out under conditions of a rate of 10 cm/s to 15 cm/s in an environment with a temperature of 25 °C and a humidity of 30%. If the temperature, humidity and removal rate are kept constant, the variation of the measured value can be inhibited. Removal can be carried out through the use of a machine or it can be carried out manually through the use of a finger, as long as the above mentioned conditions are satisfied.
[0037] If the average roughness of 10 points is measured immediately after the removal of the resin layer that comes into direct contact with another resin layer is performed, variation may occur in the measured values. Consequently, the average roughness of 10 points is preferably measured after the removed resin layer is allowed to stand for 2 hours in an environment with a temperature of 25 °C and a humidity of 30%.
[0038] The resin layer with the surface that has recesses and bulges is removed under a certain condition described above and is left to rest and then the 10 point average roughness of the surface of the resin layer removed with the surface that has recesses and bulges on the side that came into contact with another layer of resin is measured.
[0039] In the present specification, the average roughness of 10 points is measured based on the method specified by JIS B 0601(1994) "Surface roughness-definition and expression". In addition, the 10-point average roughness can be easily measured using, for example, a high-precision profilometry system (manufactured by KEYENCE CORPORATION, "KS-1100" equipped with a "LT- 9510VM").
[0040] The 10-point average roughness of the resin layer removed with the surface that has indentations and bulges on the side that came into contact with another resin layer is less than 2.7 μm. If the average 10-point roughness is less than 2.7 μm, the occurrence of ghost images can be inhibited. The 10-point average roughness is preferably equal to or less than 2.3 µm, more preferably equal to or less than 1.9 µm, and even more preferably equal to or less than 1.7 µm. If the 10-point average roughness is equal to or less than the previously mentioned preferred upper limit, the occurrence of ghosting can be further inhibited. The lower limit of the 10-point average roughness is not particularly limited. However, it is preferably equal to or greater than 0.001 μm.
[0041] In order to make the 10 point average roughness of the surface of the removed resin layer with the surface that has indentations and bulges on the side that came in contact with another resin layer smaller than 2.7 μm, for example, (1) a method of increasing the thickness of the resin layer with the surface having indentations and bulges, (2) a method of decreasing the groove depth (Rzg) of the grooves present on the surface, (3) a method of dispersing pressure at the time of formation of the recesses by narrowing the gap between the recesses present in the surface that are adjacent to each other and have the shape of a notched line (hereinafter, the gap will also be referred to as a "gap between the recesses" ), (4) a method of reducing a press pressure or a linear press pressure at the time of formation of the indentations and protrusions on the surface and the like can be used in combination.
[0042] If the thickness of the resin layer with the surface having indentations and bulges has been increased, when the indentations and bulges are formed on the surface through the use of an embossing cylinder or similar, the pressure applied to the resin layer entering Direct contact with another layer of resin is reduced and therefore transfer from the recesses and bulges to the interface can be inhibited. That is, in order to make the 10-point average roughness of the surface of the removed resin layer with the surface that has indentations and bulges on the side that came in contact with another resin layer less than 2.7 μm, the thickness of resin layer with the surface having indentations and bulges is preferably increased as far as possible, within a range that does not detract from the purpose of establishing a multi-layer structure.
[0043] The thickness of the resin layer with the surface that has indentations and bulges, which is to produce the 10 point average roughness of the removed resin layer with the surface that has indentations and bulges on the side that came into contact with another layer of resin smaller than 2.7 μm, is not particularly limited and is determined according to the material or similar of the resin layer with the surface that has indentations and protrusions or the material of the resin layer that comes in direct contact with the layer of resin. resin mentioned above. However, in an intermediate layer film for general laminated glass, the thickness of the resin layer with the surface having indentations and bulges is preferably 100 μm to 500 μm and more preferably 300 μm to 500 μm. For example, when indentations and bulges are formed on a surface of a protective layer in a noise-insulating intermediate layer film that will be described later, the thickness of the protective layer is preferably equal to or greater than 100 μm. . If the thickness of the protective layer is equal to or greater than 100 μm, transfer from the recesses and bulges to the interface may be inhibited. The thickness of the protective layer is more preferably equal to or greater than 300 µm, even more preferably equal to or greater than 400 µm, and particularly preferably equal to or greater than 450 µm. The upper limit of the thickness of the protective layer is not particularly limited. However, in order to make the sound insulation layer so thick that the layer can obtain sufficient sound insulation properties, the upper limit is substantially 500 μm.
[0044] The 10 point average roughness of the surface of the removed resin layer with the surface that has indentations and bulges on the side that came in contact with another resin layer can be reduced by reducing the groove depth (Rzg) . In order to make the laminated glass interlayer film exhibit excellent deaeration properties at the time of pressure bonding as described above, the groove depth (Rzg) needs to be equal to or greater than 10 μm. However, if the groove depth is reduced as far as possible within a range that satisfies the aforementioned groove depth, the transfer of the recesses and bulges to the interface between the resin layers can be inhibited.
[0045] The 10-point average roughness of the surface of the removed resin layer with the surface having indentations and bulges on the side that came into contact with another resin layer can also be reduced by narrowing the gap between the indentations that have the notched line format.
[0046] The interval between indentations that are shaped like a notched line, which is to form the 10 point average roughness of the surface of the removed resin layer with the surface that has indentations and bulges on the side that came into contact with another resin layer smaller than 2.7 μm, is not particularly limited and is determined according to the material or similar of the resin layer with the surface that has indentations and protrusions or the material of the resin layer that comes in direct contact with the surface. resin layer mentioned above. However, in an intermediate layer film for general laminated glass, the gap between the recesses is preferably equal to or less than 500 μm. For example, when recesses and protrusions are formed on a surface of a protective layer in a noise-insulating intermediate layer film that will be described later, the interval between recesses that are in the form of a notched line is preferably equal to at or less than 500 μm. If the gap between the grooves that are shaped like a notched line is equal to or less than 500 μm, the transfer of the grooves and bulges to the interface between the resin layers can be inhibited. The gap between the grooves which are shaped like a notched line is more preferably equal to or less than 400 μm, even more preferably equal to or less than 300 μm, and even more preferably equal to or less than 250 μm. The lower limit of the gap between the recesses that are shaped like a notched line is not particularly limited. However, from the point of view of applicability at the time of laminated glass manufacture, the lower limit is substantially 10 μm.
[0047] In the present specification, the interval between recesses which are in the form of a notched line means the shortest distance between the very lower portions of two recesses which are adjacent to each other which are in the form of a notched line. Specifically, in order to determine the gap between the recesses, the surface (a 20 mm x 20 mm observation range) of the laminated glass interlayer film is observed with an optical microscope (e.g. BS-8000III manufactured by SONIC - GROUP) and all shortest distances between the very lower portions of the observed recesses adjacent to each other are measured. Subsequently, the average of the shortest measured distances is calculated and taken as the interval between the indentations. In the present document, the maximum value of the shortest measured distances can be taken as the interval between the recesses. The interval between indentations can be the average of the shortest distances or the maximum value of the shortest distances. However, if it is, preferably, the average of the shortest distances.
[0048] The 10 point average roughness of the surface of the layer of resin removed with the surface that has indentations and bulges on the side that came into contact with another layer of resin can also be reduced by setting the press pressure or the linear press pressure at the time of formation of indentations and bulges on the surface.
[0049] For example, when indentations and protrusions are formed on the surface through the use of an embossing cylinder, as a transfer condition, the temperature of the interlayer film for laminated glass, cylinder temperature, linear speed, press pressure or linear press pressure is set. At that time, if the transfer condition such as press pressure or linear press pressure is set, transfer from the recesses and bulges to the interface between the resin layers can also be inhibited.
[0050] In the laminated glass interlayer film of the present invention, 2 or more layers of resin have been laminated on top of each other. For example, if the intermediate layer film has a first resin layer and a second resin layer as the 2 or more resin layers and the properties of the first resin layer are different from the properties of the second resin layer, a Interlayer for laminated glass can be supplied which has various performances that are not easily realized with just a single layer. However, when 2 or more layers of resin are laminated on top of each other, the problem of ghosting occurs.
[0051] The resin layers preferably contain a thermoplastic resin.
[0052] Examples of the thermoplastic resin include polyvinylidene fluoride, polytetrafluoroethylene, a vinylidene fluoride-propylene hexafluoride copolymer, polyethylene trifluoride, an acrylonitrile-butadiene-styrene copolymer, polyester, polyether, polyamide, polycarbonate, polyacrylate, polymethacrylate, polyvinyl chloride, polyethylene, polypropylene, polystyrene, polyvinyl acetal, an ethylene-vinyl acetate copolymer, and the like. Of these, the resin layers preferably contain polyvinyl acetal or an ethylene-vinyl acetate copolymer, and more preferably contain polyvinyl acetal.
[0053] The resin layers preferably contain polyvinylacetal and a plasticizer.
[0054] The plasticizer is not particularly limited as it is a plasticizer generally used in an interlayer film for laminated glass. Examples thereof include organic plasticizers, such as a monobasic organic acid ester and a polybasic organic acid ester, phosphoric acid plasticizers, such as an organic phosphoric acid compound and an organic phosphoric acid compound, and the like.
[0055] Examples of organic plasticizers include triethylene glycol-di-2-ethyl hexanoate, triethylene glycol-di-2-ethyl butyrate, triethylene glycol-dn-heptanoate, tetraethylene glycol-di-2-ethyl hexanoate, tetraethylene glycol- di-2-ethyl butyrate, tetraethylene glycol-di-n-heptanoate, diethylene glycol-di-2-ethyl hexanoate, diethylene glycol-di-2-ethyl butyrate, diethylene glycol-di-n-heptanoate and the like. Of these, the resin layers preferably contain triethylene glycol-di-2-ethyl hexanoate, triethylene glycol-di-2-ethyl butyrate or triethylene glycol-di-n-heptanoate, and more preferably contain triethylene glycol-di- 2-ethyl hexanoate.
[0056] The resin layers preferably contain an adhesion adjustment age. Particularly, the resin layer, which comes into contact with the glass when laminated glass is manufactured, preferably contains the adhesion definer.
[0057] As *parag. adhesion adjustment agent, for example, an alkali metal salt or an alkaline earth metal salt is preferably used. Examples of the adhesion definer include a salt, such as sodium, potassium or magnesium.
[0058] Examples of an acid constituting the salt include an organic carboxylic acid, such as octyl acid, hexylic acid, 2-ethyl butyrate, butyric acid, acetic acid, or formic acid, and an inorganic acid, such as hydrochloric acid or nitric acid. The resin layer that comes into contact with the glass preferably contains a magnesium salt as the adhesion adjustment agent, since the adhesion between the glass and the resin layer can be easily defined when the laminated glass is manufactured.
[0059] If necessary, the resin layers may contain additives such as an antioxidant, a light stabilizer, modified silicone oil as an adhesion definer, a flame retardant, an antistatic agent, a moisture protection agent, a heat ray reflecting agent and a heat ray absorbing agent.
[0060] The laminated glass interlayer film of the present invention preferably has at least the first resin layer and the second resin layer as the 2 or more resin layers and the amount of polyvinyl hydroxyl groups acetal contained in the first resin layer (hereinafter polyvinyl acetal will be referred to as polyvinyl acetal A) is preferably different from the amount of hydroxyl groups of polyvinyl acetal contained in the second resin layer (hereinafter polyvinyl acetal will be referred to as polyvinyl acetal B).
[0061] Due to the fact that the properties of polyvinyl acetal A are different from the properties of polyvinyl acetal B, an intermediate layer film for laminated glass can be provided which has various performances that are not easily realized with just a single layer. For example, when the first resin layer is laminated between the 2 second resin layers described above and the amount of hydroxyl groups of polyvinyl acetal A is less than the amount of hydroxyl groups of polyvinyl acetal B, a glass transition temperature of the first resin layer tends to be less than that of the second resin layer. As a result, the first layer of resin becomes softer than the second layer of resin and the sound insulation properties of the laminated glass interlayer film are improved. Furthermore, when the first resin layer is laminated between the 2 second resin layers described above and the amount of hydroxyl groups of polyvinyl acetal A is greater than the amount of hydroxyl groups of polyvinyl acetal B, a glass transition temperature of the first resin layer tends to be greater than that of the second resin layer. As a result, the first layer of resin becomes more rigid than the second layer of resin, and so the penetration resistance of the laminated glass interlayer film is improved.
[0062] Furthermore, when the first resin layer and the second resin layer include a plasticizer, it is preferable that the plasticizer content in the first resin layer relative to 100 parts by mass of the polyvinyl acetal (hereinafter hereinafter document, the content will be referred to as a content A) is different from the content of the plasticizer in the second resin layer with respect to 100 parts of the polyvinyl acetal (hereinafter, the content will be referred to as a content B). For example, when the first resin layer is laminated between the 2 second resin layers described above and the A content is greater than the B content, the glass transition temperature of the first resin layer tends to be lower than that of the second layer of resin. resin. As a result, the first layer of resin becomes softer than the second layer of resin and the sound insulation properties of the laminated glass interlayer film are improved. Furthermore, when the first resin layer is laminated between the 2 second resin layers described above and the A content is lower than the B content, the glass transition temperature of the first resin layer tends to be higher than that of the second layer. of resin. As a result, the first layer of resin becomes more rigid than the second layer of resin and the penetration resistance of the laminated glass interlayer film is improved.
[0063] Examples of the combination of the 2 or more layers of resin that make up the laminated glass interlayer film of the aspect of the present invention include a combination of a soundproofing layer as the first resin layer and a protective layer as the second. resin layer, which is a combination to enhance the sound insulation properties of laminated glass. The soundproofing layer preferably contains polyvinyl acetal X and a plasticizer and the protective layer preferably contains polyvinyl acetal Y and a plasticizer, due to the fact that the soundproofing properties of laminated glass are enhanced. Furthermore, if the sound insulation layer is sandwiched between the 2 protective layers described above, an intermediate layer film for laminated glass which has excellent sound insulation properties can be obtained (hereinafter, the intermediate layer film will also be referred to as as a noise-insulating intermediate layer film). In the invention of the present application, even when resin layers having different properties, such as the soundproofing layer and the protective layer, are laminated on top of each other, it is possible to obtain an intermediate layer film for laminated glass that can prevent ghost images from occurring. Hereinafter, the noise insulating interlayer film will be more specifically described.
[0064] In the noise insulation intermediate layer film, sound insulation layer has a function of imparting sound insulation properties.
[0065] The sound insulation layer preferably contains polyvinyl acetal X and a plasticizer.
[0066] Polyvinyl acetal X can be prepared through the acetylation of polyvinyl alcohol through the use of aldehyde. In general, polyvinyl alcohol is obtained through the saponification of polyvinyl acetate.
[0067] The lower limit of an average degree of polymerization of polyvinyl alcohol is preferably 200 and the upper limit thereof is preferably 5,000. If the average degree of polymerization of polyvinyl alcohol is equal to or greater than 200, the penetration resistance of the obtained noise-insulating intermediate layer film can be improved, and if it is equal to or less than 5,000, the modability of the layer soundproofing can be guaranteed. The lower limit of the average degree of polymerization of the polyvinyl alcohol is more preferably 500 and the upper limit thereof is more preferably 4000.
[0068] In the present document, the average degree of polymerization of polyvinyl alcohol is determined by the method based on JIS K6726 "Testing methods for polyvinyl alcohol".
[0069] The lower limit of the number of aldehyde carbon atoms for acetylation of polyvinyl alcohol is preferably 4 and the upper limit thereof is preferably 6. If the number of carbon atoms of the aldehyde is equal to or greater that 4, enough of the plasticizer can be stably contained in the sound insulation layer, and then the noise insulation intermediate layer film can demonstrate excellent noise insulation performance. In addition, bleeding of the plasticizer can be avoided. If the number of carbon atoms of the aldehyde is equal to or less than 6, polyvinyl acetal X is easily synthesized and, therefore, productivity can be guaranteed.
[0070] The aldehyde having 4 to 6 carbon atoms can be linear or branched aldehyde and examples thereof include n-butyl aldehyde, n-valeraldehyde and the like.
[0071] The upper limit of the amount of hydroxyl groups of polyvinyl acetal X is preferably 30% by mol. If the amount of hydroxyl groups of polyvinyl acetal X is equal to or less than 30% by mol, the plasticizer can be contained in the sound insulation layer in an amount necessary for the noise insulation intermediate layer film to exhibit the insulation properties noise and plasticizer bleeding can be avoided. The upper limit of the amount of hydroxyl groups of polyvinyl acetal X is more preferably 28% by mol, even more preferably 26% by mol and particularly preferably 24% by mol. The lower limit of the amount of hydroxyl groups of polyvinyl acetal X is preferably 10% by mol, more preferably 15% by mol and most preferably 20% by mol.
[0072] The amount of hydroxyl groups of polyvinyl acetal X is a value determined through the expression of a molar fraction, which is obtained by dividing the amount of ethylene groups attached to the hydroxyl groups by the total amount of ethylene groups of a main chain, in percentage (% in mol). The amount of ethylene groups attached to the hydroxyl groups can be determined by measuring the amount of ethylene groups attached to the hydroxyl groups of polyvinyl acetal X using, for example, the method based on JIS K6728 "Testing methods for polyvinyl butyral ".
[0073] The lower limit of the amount of acetal groups of polyvinyl acetal X is preferably 60% by mol, and the upper limit thereof is preferably 85% by mol. If the amount of acetal groups of polyvinyl acetal X is equal to or greater than 60% by mol, the hydrophobicity of the soundproofing layer can be improved, the plasticizer can be contained in the soundproofing layer in an amount necessary for the Noise insulating intermediate layer film exhibit the sound insulation properties and the bleeding or bleaching of the plasticizer can be avoided. If the amount of acetal groups of polyvinyl acetal X is equal to or less than 85% by mol, polyvinyl acetal X can be easily synthesized and then productivity can be guaranteed. The lower limit of the amount of acetal groups of polyvinyl acetal X is, more preferably, 65% by mol, and even more preferably, equal to or greater than 68% by mol.
[0074] The amount of acetal groups can be determined by measuring the amount of ethylene groups attached to the acetal groups of polyvinyl acetal X by the method based on JIS K6728 "Testing methods for polyvinyl butyral".
[0075] The lower limit of the amount of acetyl groups of polyvinyl acetal X is preferably 0.1% by mol, and the upper limit thereof is preferably 30% by mol. If the amount of acetyl groups in polyvinyl acetal X is equal to or greater than 0.1% by mol, the plasticizer may be contained in the sound insulation layer in an amount necessary for the sound insulation intermediate layer film to exhibit the properties soundproofing and bleeding can be avoided. Furthermore, if the amount of acetyl groups in polyvinyl acetal X is equal to or less than 30% by mol, the hydrophobicity of the sound insulation layer can be improved and bleaching can be avoided. The lower limit of the amount of acetyl groups is more preferably 1% by mol, even more preferably 5% by mol, and particularly preferably 8% by mol. The upper limit of the amount of acetyl groups is more preferably 25% by mol, and even more preferably 20% by mol. The amount of acetyl groups is a value determined through the expression of a mole fraction, which is obtained by dividing a value obtained by subtracting the amount of ethylene groups attached to the acetal groups and the amount of ethylene groups attached to the hy- groups . droxyl from the total amount of ethylene groups of a main chain by the total amount of ethylene groups of the main chain, in percentage (% in mol).
[0076] Particularly, polyvinyl acetal X is preferably polyvinyl acetal in which the amount of acetyl groups is equal to or greater than 8% by mol, or polyvinyl acetal in which the amount of acetyl groups is less than 8% by mol and the amount of acetal groups is equal to or greater than 65% by mol, due to the fact that the plasticizer can be easily contained in the sound insulation layer in an amount necessary for the noise insulation intermediate layer film to exhibit insulating properties acoustic. Polyvinyl acetal X is more preferably polyvinyl acetal in which the amount of acetyl groups is equal to or greater than 8% by mol, or polyvinyl acetal in which the amount of acetyl groups is less than 8% by mol and the amount of acetal groups is equal to or greater than 68% by mol.
[0077] The lower limit of the plasticizer content in the acoustic insulation layer is preferably 45 parts by mass, and the upper limit of the same is preferably 80 parts by mass, in relation to 100 parts by mass, of polyvinyl acetal X. If the plasticizer content is equal to or greater than 45 parts by mass, the noise insulation intermediate layer film can exhibit a high degree of sound insulation properties and if the content is equal to or less than 80 parts by mass, it is possible to prevent the transparency or adhesion of the interlayer film for laminated glass from deteriorating due to plasticizer bleed. The lower limit of the plasticizer content is more preferably 50 parts by mass, and even more preferably 55 parts by mass. The upper limit of the plasticizer content is more preferably 75 parts by mass, and even more preferably 70 parts by mass.
[0078] The lower limit of the thickness of the acoustic insulation layer is preferably 50 μm. If the thickness of the sound insulation layer is equal to or greater than 50 μm, the noise insulation intermediate layer film can exhibit sufficient sound insulation properties. The lower limit of the thickness of the sound insulation layer is more preferably 80 μm. The upper limit of the same is not particularly limited. However, considering the thickness of the intermediate layer film for laminated glass, the upper limit is preferably 300 μm.
[0079] The protective layer has a function of preventing the adhesion between the intermediate layer film for laminated glass and the glass from deteriorating due to the bleeding of a large amount of the plasticizer contained in the sound insulation layer and providing resistance to penetration to the intermediate layer film for laminated glass.
[0080] The protective layer preferably contains, for example, polyvinyl acetal Y and a plasticizer and, more preferably, contains polyvinyl acetal Y, which contains more hydroxyl groups than polyvinyl acetal X and a plasticizer.
[0081] Polyvinyl acetal Y can be prepared through the acetylation of polyvinyl alcohol through the use of aldehyde.
[0082] In general, polyvinyl alcohol is obtained through the saponification of polyvinyl acetate.
[0083] The lower limit of an average degree of polymerization of polyvinyl alcohol is preferably 200 and the upper limit thereof is preferably 5,000. If the average degree of polymerization of polyvinyl alcohol is equal to or greater than 200, the penetration resistance of the intermediate layer film obtained for laminated glass can be improved, and if it is equal to or less than 5000, the modability of the protective layer can be improved. guaranteed. The lower limit of the average degree of polymerization of the polyvinyl alcohol is more preferably 500 and the upper limit thereof is more preferably 4000.
[0084] The lower limit of the number of aldehyde carbon atoms for acetylation of polyvinyl alcohol is preferably 3 and the upper limit thereof is preferably 4. If the number of carbon atoms of the aldehyde is equal to or greater than 3, the penetration resistance of the interlayer film for laminated glass is improved. If the number of carbon atoms of the aldehyde is equal to or less than 4, the productivity of polyvinyl acetal Y is improved.
[0085] The aldehyde having 3 to 4 carbon atoms can be linear or branched aldehyde and examples thereof include n-butyl aldehyde and the like.
[0086] The upper limit of the amount of hydroxyl groups of polyvinyl acetal Y is preferably 33% by mol, and the lower limit thereof is preferably 28% by mol. If the amount of hydroxyl groups of polyvinyl acetal Y is equal to or less than 33% by mol, bleaching of the interlayer film for laminated glass can be avoided. If the amount of hydroxyl groups of polyvinyl acetal Y is equal to or greater than 28% by mol, the penetration resistance of the laminated glass interlayer film is improved.
[0087] In polyvinyl acetal Y, the lower limit of the amount of acetal groups is preferably 60% by mol, and the upper limit thereof is preferably 80% by mol. If the amount of acetal groups is equal to or greater than 60% by mol, the plasticizer may be contained in the protective layer in an amount necessary for the laminated glass interlayer film to exhibit sufficient penetration resistance. If the amount of acetal groups is equal to or less than 80% by mol, adhesion between the protective layer and the glass can be guaranteed. The lower limit of the amount of acetal groups is more preferably 65% by mol, and the upper limit thereof is more preferably 69% by mol.
[0088] The upper limit of the amount of acetyl groups in polyvinyl acetal Y is preferably 7% by mol. If the amount of acetyl groups of polyvinyl acetal Y is equal to or less than 7% by mol, the hydrophobicity of the protective layer is improved and, therefore, bleaching can be avoided. The upper limit of the amount of acetyl groups is more preferably 2% by mol, and the lower limit thereof is preferably 0.1% by mol. In the present document, the amount of hydroxyl groups, the amount of acetal groups and the amount of acetyl groups in polyvinyl acetal A, B, and Y can be measured by the same method as polyvinyl acetal X.
[0089] The lower limit of the plasticizer content in the protective layer is preferably 20 parts by mass, and the upper limit of the same is preferably 45 parts by mass compared to 100 parts by mass of polyvinyl acetal Y. If the plasticizer content is equal to or greater than 20 parts by mass, penetration resistance can be guaranteed. If the plasticizer content is equal to or less than 45 parts by mass, bleeding of the plasticizer can be avoided and then deterioration of transparency or adhesion of the laminated glass interlayer film can be avoided. The lower limit of the plasticizer content is more preferably 30 parts by mass, and even more preferably 35 parts by mass. The upper limit thereof is more preferably 43 parts by mass, and even more preferably 41 parts by mass. The plasticizer content in the protective layer is preferably lower than the plasticizer content in the soundproofing layer, due to the fact that the soundproofing properties of laminated glass are further enhanced.
[0090] The amount of hydroxyl groups of polyvinyl acetal Y is preferably greater than the amount of hydroxyl groups of polyvinyl acetal X, due to the fact that the sound insulation properties of laminated glass are further improved. The amount of hydroxyl groups of polyvinyl acetal Y is greater than the amount of hydroxyl groups of polyvinyl acetal X, more preferably by not less than 1% by mol, even more preferably by not less than 5% by mol, and of particularly preferably, by not less than 8% by mol. If the amount of hydroxyl groups of polyvinyl acetal X and polyvinyl acetal Y is defined, the plasticizer content in the soundproofing layer and the protective layer can be controlled and the glass transition temperature of the soundproofing layer is reduced. As a result, the sound insulation properties of laminated glass are further enhanced.
[0091] The content (hereinafter also referred to as a content X) of the plasticizer in relation to 100 parts by mass of polyvinyl acetal X in the soundproofing layer is preferably greater than the content (hereinafter in this document , also referred to as a content Y) of the plasticizer relative to 100 parts by mass of polyvinyl acetal Y in the protective layer, due to the fact that the sound insulation properties of laminated glass are further enhanced. The X content is greater than the Y content, more preferably by not less than 5 parts by mass, even more preferably by not less than 15 parts by mass, and particularly preferably by not less than 20 parts , in large scale. If the content X and the content Y are defined, the glass transition temperature of the sound insulation layer is reduced. As a result, the sound insulation properties of laminated glass are further enhanced.
[0092] The thickness of the protective layer is not particularly limited and only needs to be defined within a range within which the protective layer can perform its function. In the present document, when the protective layer has indentations and protrusions on the surface thereof, it is preferable that the thickness of the protective layer is as good as possible, so that the indentations and protrusions are inhibited from being transferred to the interface between the protective layer. and the soundproofing layer that comes into direct contact with the protective layer. Specifically, the lower limit of the thickness of the protective layer is preferably 100 µm, more preferably 300 µm, even more preferably 400 µm and particularly preferably 450 µm. The upper limit of the thickness of the protective layer is not particularly limited. However, in order to make the soundproofing layer so thick that the layer can provide sufficient soundproofing properties, the upper limit of the thickness of the protective layer is substantially about 500 μm.
[0093] The method for manufacturing the noise-insulating interlayer film is not particularly limited. Examples of the method include a method of forming the sound-insulating layer and the protective layer in the form of a sheet by means of a general film-forming method, such as an extrusion method, a calendering method or a and laminating the soundproofing layer and the protective layer to each other.
[0094] In accordance with another aspect of the present invention, there is provided an intermediate layer film for laminated glass that includes 2 protective layers and a soundproofing layer laminated between the protective layers, wherein the soundproofing layer contains a plasticizer in an amount of 45 parts by mass to 80 parts by mass with respect to 100 parts by mass of polyvinyl acetal, the protective layers contain a plasticizer in an amount of 20 parts by mass to 45 parts by mass, relative to 100 parts by mass of polyvinyl acetal, the protective layers have a large number of recesses and a large number of protrusions on at least one surface thereof, each recess has a groove shape with a bottom continuous, the recesses adjacent to each other are parallel to each other and regularly arranged in a line, within the surface of the protective layer which has the large number of recesses and the large number that of bulges, a groove depth (Rzg) of the recesses measured based on JIS B-0601(1994) is 10 μm to 40 μm, an average roughness of 10 points (Rz) of a surface of the protective layer that has the surface which includes the large number of recesses and the large number of bulges measured based on JIS B 0601(1994) is less than 2.7 μm and the average roughness of 10 points (Rz) is obtained by removing the protective layer that has the surface that includes the large number of recesses and the large number of bulges of the soundproofing layer and thereby measuring the surface of the protective layer removed on one side of the soundproofing layer based on JIS B 0601(1994) .
[0095] In the present invention, the state in which "the protective layer has a large number of recesses and a large number of protrusions on at least one surface of the table" refers to a state in which "a large number of recesses and a large numbers of bulges were formed on at least one surface of the protective layer". Furthermore, the state in which "each of the recesses has a groove shape with a continuous bottom, and the recesses adjacent to each other are parallel to each other and regularly arranged in a line" refers to a state in which "each one of the recesses has a groove shape with a continuous bottom and the recesses adjacent to each other are parallel to each other and formed regularly".
[0096] In accordance with yet another aspect of the present invention, laminated glass is provided in which the laminated glass interlayer film of the present invention is laminated between a pair of glass plates.
[0097] Like the glass plates, it is possible to generally use used clear glass plate. Examples thereof include flat glass plate, polished glass plate, printed glass, wire reinforced glass, wired glass plate, colored glass plate, heat ray absorbing glass, heat ray reflecting glass and inorganic glass, such as green glass. Furthermore, it is possible to use UV shielding glass in which a UV shielding coating is provided on the glass surface. In addition, organic plastic sheets such as polyethylene terephthalate, polycarbonate and polyacrylate can be used.
[0098] Like the glass plates mentioned earlier, two or more types of glass plates can be used. Examples thereof include laminated glass in which the laminated glass interlayer film of the present invention is laminated between a plate of clear glass and a plate of colored glass, such as green glass. Also, like glass plates, two or more types of glass plates that have different thicknesses can be used.
[0099] The method for making laminated glass of the aspect of the present invention is not particularly limited and methods known in the related art can be used. ADVANTAGEOUS EFFECTS OF THE INVENTION
[00100] According to the aspect of the present invention, it is possible to provide an intermediate layer film for laminated glass that includes 2 or more resin layers laminated on top of each other, exhibit excellent deaeration properties in a glass making process. laminate and can prevent ghosting from occurring and provide the laminated glass that includes the laminated glass interlayer film. BRIEF DESCRIPTION OF THE DRAWINGS
[00101] Figure 1 is a schematic view showing an example of an intermediate layer film for laminated glass, in which each of the recesses having a groove shape with a continuous bottom is formed on the surface thereof at an equal interval. and the recesses adjacent to each other are parallel to each other and arranged in a line.
[00102] Figure 2 is a schematic view showing an example of an intermediate layer film for laminated glass, in which each of the recesses that has a groove shape with a continuous bottom is formed on the surface of the same at an equal interval and the recesses adjacent to each other are parallel to each other and arranged in a line.
[00103] Figure 3 is a schematic view showing an example of an intermediate layer film for laminated glass, in which each of the recesses that has a groove shape with a continuous bottom is formed on the surface thereof at an unequal interval and the recesses adjacent to each other are parallel to each other and arranged in a line.
[00104] Figure 4 is a schematic view illustrating the intermediate layer film for laminated glass that has a 2-layer structure and a surface thereof on which an average roughness of 10 points (Rz) is measured.
[00105] Figure 5 is a schematic view illustrating the intermediate layer film for laminated glass which has a 3-layer structure and a surface thereof on which an average roughness of 10 points (Rz) is measured. DESCRIPTION OF MODALITIES
[00106] Hereinafter, embodiments of the present invention will be more specifically described based on the examples, but the present invention is not limited to the examples. (EXAMPLE 1)(1) Preparation of resin composition for sound insulation layer
[00107] As a plasticizer, 60 parts by mass of triethylene glycol-di-2-ethyl hexanoate (3GO) was added to 100 parts by mass of polyvinyl butyral (an amount of acetyl groups: 12% by mol, an amount of butyral groups: 66% in mol, an amount of hydroxyl groups: 22% in mol) which was obtained through the acetylation of polyvinyl alcohol which has an average degree of polymerization of 2,400 through the use of n-butyl aldehyde and the resulting was thoroughly mixed using a mixing cylinder, thereby obtaining a resin composition for a soundproofing layer.(2) Preparation of resin composition for a protective layer
[00108] As a plasticizer, 40 parts by mass of triethylene glycol-di-2-ethyl hexanoate (3GO) were added to 100 parts by mass of polyvinyl butyral (an amount of acetyl groups: 1% by mol, an amount of butyral groups: 69% in mol, an amount of hydroxyl groups: 30% in mol) which was obtained through the acetylation of polyvinyl alcohol which has an average degree of polymerization of 1,700 through the use of n-butyl aldehyde and the resulting was thoroughly mixed using a mixing cylinder, thereby obtaining a resin composition for a protective layer.(3) Interlayer film preparation for laminated glass
[00109] The resin composition obtained for a soundproofing layer and resin composition for a protective layer was co-extruded through the use of a co-extruder, thereby obtaining an intermediate layer film for laminated glass (interlayer film of noise insulation) which has a 3-layer structure in which a layer A (protective layer) formed from the resin composition to a protective layer and which has a thickness of 450 μm, a layer B (sound insulation layer) formed from the composition of resin for a soundproofing layer and having a thickness of 100 μm and a layer C (protective layer) formed from the resin composition for a protective layer and having a thickness of 450 μm were laminated over each other in that order. (4) Formation of indentations and bulges
[00110] As a first step, the shape of random recesses and protrusions was transferred to both surfaces of the laminated interlayer film according to the following procedure. First, through the use of a blasting agent, random recesses and bulges were formed on the surface of an iron cylinder, and then vertical grinding was performed on the iron cylinder. Furthermore, through the use of a finer blasting agent, the fine indentations and protrusions were formed into a flat portion formed after grinding. As a result, a pair of cylinders of the same shape having both rough main embossing and fine sub-embossing was obtained. By using the pair of cylinders as a device to transfer the shape of recesses and protrusions, the shape of random recesses and protrusions was transferred to both surfaces of the obtained intermediate layer film for laminated glass. At that time, as the transfer conditions, the temperature of the interlayer film for laminated glass was set to be 80 °C, the temperature of the cylinders was set to be 145 °C, the linear velocity was set to be 10 m/min and the linear press pressure was set to be 10 kN/m to 200 kN/m. The surface roughness of the shaped interlayer film for laminated glass was measured as the 10 point average roughness (Rz) described in JIS B 0601(1994). As a result, it was confirmed that the surface roughness should be 16 μm. Surface roughness was obtained by processing data into digital signals measured using a surface roughness meter (SE1700a manufactured by Kosaka Laboratory Ltd.). The surface roughness was measured in a direction perpendicular to the notched line, under conditions of a cut value = 2.5 mm, a reference length = 2.5 mm, an evaluation length = 12.5 mm, a radius of the probe tip = 2 μm, a tip angle = 60°, and a measurement rate = 0.5 mm/s.
[00111] As a second step, each of the recesses and protrusions that have a groove shape with a continuous bottom (a notched line shape) was formed on a surface of the laminated glass interlayer film according to the procedure Next. As a device for transferring the shape of recesses and protrusions, a pair of cylinders composed of a metal cylinder whose surface had undergone the milling process through the use of an inclined triangular milling machine and a rubber cylinder having a hardness of JIS 45 to 75 was used. The intermediate layer film for laminated glass, to which the shape of random recesses and protrusions was transferred in the first step, was passed through the device to transfer the format of recesses and protrusions. As a result, on a surface of layer A of the laminated glass interlayer film, recesses and protrusions were formed, in which the recesses each have a groove shape with a continuous bottom (a one-line shape). notched) are parallel to each other and arranged in a line at an equal interval. At that time, as the transfer conditions, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130 °C, the linear velocity was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 500 kPa.
[00112] Subsequently, a C-layer surface of the laminated glass interlayer film was subjected to the same operation as described above, except that a metal cylinder having a different shape of recesses and protrusions was used, and hence In this way, the indentations, each of which have a groove shape with a continuous bottom (a notched line shape) were formed on the surface. At this time, the recesses were formed so that a crossing angle between each of the recesses which has a groove shape with a continuous bottom (a notched line shape) was formed on the surface of layer A and where each one of the recesses has a groove shape with a continuous bottom (a notched line shape) that was formed on the surface of layer C becomes 10°.(5) Measurement of the recesses and protrusions of the surface of layer A and layer C
[00113] Through the use of an optical microscope (BS-8000III manufactured by SONIC-GROUP), the surface (a 20 mm x 20 mm observation range) of layer A and layer C of the obtained intermediate layer film for glass laminate was observed. Furthermore, an interval between the recesses adjacent to each other was measured and then the average of the shortest distances between the very lower portions of the recesses adjacent to each other was calculated, thereby obtaining an interval between the recesses. An interval between recesses on the surface of layer A was 500 μm and an interval between recesses on the surface of layer C was 750 μm. In the present document, the mean and maximum value of the shortest distance were the same for layer A and layer C.
[00114] In order to obtain the groove depth (Rzg) of the indentations on the surface of layer A and layer C of the intermediate layer film obtained for laminated glass, a groove depth based on a midline of a roughness curve (a line configured so that the sum of squares of roughness curve deviation is minimized) was calculated by setting a reference length specified in JIS B-0601(1994) "Surface roughness-definition and expression" to be 2, 5 mm; an average of the measured groove depths was taken as a groove depth per reference length; and an average of the groove depth per reference length of 5 grooves was taken as the groove depth (Rzg). The number of grooves of layer A was 5 and the number of grooves of layer C was 4. In addition, the groove depth (Rzg) of the surface indentations of layer A and layer C was obtained by performing the data process on digital signals measured using a surface roughness meter (SE1700a manufactured by Kosaka Laboratory Ltd.). Surface roughness was measured in a direction perpendicular to the notched line, under conditions of a probe tip radius = 2 μm, a tip angle = 60° and a measurement rate = 0.5 mm/s.
[00115] The groove depth (Rzg) of the surface recesses of layer A was 21 μm and the groove depth (Rzg) of the surface recesses of layer C was 19 μm.
[00116] In addition, the surface of layer A and layer C of the intermediate layer film obtained for laminated glass was measured using a surface roughness meter (SE1700a manufactured by Kosaka Laboratory Ltd.), thereby obtaining the average roughness of 10 points (Rz) of the same. The average 10-point roughness (Rz) of the surface of layer A was 51 μm and the average 10-point roughness (Rz) of the surface of layer C was 50 μm.(6) Measurement of interface recesses and protrusions
[00117] The intermediate layer film obtained for laminated glass was cut to 5 cm (length) x 5 cm (width) and left to rest for 2 hours in an environment with a temperature of 25 °C and a humidity of 30%.
[00118] By inserting a finger between layer A and layer B, the layers were removed from each other at a rate of 10 cm/s to 15 cm/s. After removal, they were left for 2 hours in an environment with a temperature of 25°C and a humidity of 30%. Subsequently, the surface of layer A removed on the layer B side was measured using a high-precision profilometry system (manufactured by KEYENCE CORPORATION, "KS-1100" equipped with a "LT-9510VM" model nose head). based on JIS B 0601(1994), thereby obtaining an average roughness of 10 points (Rz). The 10-point average roughness (Rz) of the surface of layer A removed on the side of layer B was 1.7 μm. Regarding the measurement conditions, a moving stage rate was defined to be 100.0 μm/s, a measurement step of an X axis axis was defined to be 2.0 μm and a measurement step of an axis axis. Y was set to be 2.0 μm.
[00119] Layer B and layer C were also removed from each other in the same method as described above and the 10 point average roughness (Rz) of the surface of layer C removed on the side of layer B was obtained. The 10-point average roughness (Rz) of the surface of layer C removed on the side of layer B was 1.9 μm. (EXAMPLES 2 TO 5, COMPARATIVE EXAMPLE 1)
[00120] Interlayer films for laminated glass were prepared by the same method as in Example 1, except that the thickness of each layer, the interval between the indentations in the surface of layer A and layer C, the groove depth (Rzg) of the indentations, the 10-point average roughness (Rz), the 10-point average roughness (Rz) of the surface of layer A removed on the layer B side, and the 10-point average roughness (Rz) of the layer surface C removed on the side of layer B were defined as shown in Table 1.
[00121] In Example 2, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 200 kPa.
[00122] In Example 3, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 400 kPa.
[00123] In Example 4, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130° C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 500 kPa.
[00124] In Example 5, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 500 kPa.
[00125] In Comparative Example 1, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130 °C , the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 200 kPa.
[00126] In the present document, in the step of measuring the gap between the recesses in Examples 2 to 5 and comparative example 1, the average and the maximum value of the shortest distance between the recesses were the same for all Examples. (EXAMPLES 6 and 7, COMPARATIVE EXAMPLE 2)
[00127] The interlayer films for laminated glass were prepared by the same method as in Example 1, except that the thickness of each layer, the interval between the surface indentations of layer A and layer C, the groove depth (Rzg) of the recesses, the 10-point average roughness (Rz), the 10-point average roughness (Rz) of the surface of layer A removed on the layer B side, and the 10-point average roughness (Rz) of the surface of layer C removed on the side of layer B were defined as shown in Table 1 and the transfer conditions at the time of formation of the indentations and bulges were changed.
[00128] In Example 6, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 700 kPa.
[00129] In Example 7, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 200 kPa.
[00130] In Comparative Example 2, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130 °C , the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 100 kPa.
[00131] In the present document, in the step of measuring the gap between the recesses in Examples 6 and 7 and comparative example 2, the mean and maximum value of the shortest distance between the recesses were the same for all Examples. (COMPARATIVE EXAMPLES 3 and 4)
[00132] As a device to transfer embossing similar to orange peel, a pair of cylinders was used that had undergone the sandblasting process in which a sandblasting material formed from aluminum oxide (#36: which has a roughness of 65 μm under a saturation condition) was discharged into the cylinders at a discharge pressure of 50 x 104 Pa. The laminated glass interlayer film obtained in Example 1 was passed through the device to transfer embossments similar to orange peel and, as a result, embossing similar to orange peel was formed on the surface of layer A and layer C of the laminated glass interlayer film.
[00133] At that time, as the transfer conditions, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130 °C, the linear velocity was set to be 10 m /min, the film width was set to be 1.5 m and the press pressure was set to be 500 kPa.
[00134] In the present document, in the intermediate layer film for laminated glass obtained in Comparative Examples 3 and 4, the groove depth (Rzg) could be measured. (EXAMPLES 8 TO 10)
[00135] The intermediate layer films for laminated glass were prepared by the same method as in Example 1, except that the thickness of each layer, the interval between the surface indentations of layer A and layer C, the groove depth (Rzg) of the indentations, the 10-point average roughness (Rz), the 10-point average roughness (Rz) of the surface of layer A removed on the layer B side, and the 10-point average roughness (Rz) of the layer surface C removed on the side of layer B were defined as shown in Table 1.
[00136] In Example 8, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 200 kPa.
[00137] In Example 9, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 500 kPa.
[00138] In Example 10, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the press pressure was set to be 500 kPa.
[00139] In the present document, in the step of measuring the gap between the recesses in Examples 8 to 10, the average and the maximum value of the shortest distance between the recesses were the same as in all Examples. (EXAMPLES 11 TO 14)
[00140] Interlayer films for laminated glass were prepared by the same method as in Example 1, except that the amount of acetyl groups, the amount of butyral groups and the amount of hydroxyl groups of polyvinyl butyral used in the protective layer and in the sound insulation layer as well as the plasticizer content were changed as shown in Table 1; the thickness of each layer, the interval between the surface recesses of layer A and layer B, the groove depth (Rzg) of the recesses, the average roughness of 10 points (Rz), the average roughness of 10 points (Rz) of the surface of layer A removed on the side of layer B and the 10 point average roughness (Rz) of the surface of layer C removed on the side of layer B were defined as shown in Table 1; and the transfer conditions at the time of formation of the indentations and bulges were changed. In the present document, the polyvinyl butyral used in the protective layer and in the sound insulation layer was obtained through the acetylation of polyvinyl alcohol which has an average degree of polymerization of 1700 through the use of n-butyl aldehyde.
[00141] In Example 11, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the linear press pressure was set to be 200 kPa.
[00142] In Example 12, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the linear press pressure was set to be 500 kPa.
[00143] In Example 13, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear speed was set to be 10 m/min, the film width was set to be 1.5 m and the linear press pressure was set to be 500 kPa.
[00144] In Example 14, as the transfer conditions at the time of formation of the indentations and bulges, the temperature of the interlayer film for laminated glass was set to be room temperature, the cylinder temperature was set to be 130°C, the linear velocity was set to be 10 m/min, the film width was set to be 1.5 m and the linear press pressure was set to be 550 kPa.
[00145] In the present document, in the step of measuring the gap between the recesses in Examples 11 to 14, the average and the maximum value of the shortest distance between the recesses were the same for all Examples. (ASSESSMENT)
[00146] The intermediate layer films for laminated glass obtained in Examples and Comparative Examples were evaluated by the following method.
[00147] The results are shown in Table 1. In the Table, "Degree of butylation" represents the amount of butyral groups, "Degree of hydroxylation" represents the amount of hydroxyl groups, "Degree of acetylation" represents the amount of acetyl groups and "Plasticizer (parts)" represents the content of plasticizer in relation to 100 parts, by mass, of polyvinyl butyral.(1) Assessment of deaeration properties
[00148] The intermediate layer film obtained for laminated glass that has the recesses and protrusions on one surface of the glass was initially pressure bonded and then pressure bonded completely by means of a vacuum deaeration method, preparing, thus, laminated glass. (VACUUM DEAERATION METHOD)
[00149] The intermediate layer film was sandwiched between 2 sheets of clean glass plates (30 cm (length) x 30 cm (width) x 2.5 mm (thickness)) and the portion that protrudes the glass plates was cut . The laminated (laminated) glass structure obtained in this way was moved in a rubber bag and the rubber bag was connected to a suction decompressor. The laminated glass structure was then heated and held under reduced pressure at -60 kPa (an absolute pressure of 16 kPa) for 10 minutes. The laminated (laminated) glass structure was kept heated until the temperature (pre-pressure bonding temperature) of the same became 70 °C, and then the pressure was returned to atmospheric pressure to complete the preliminary pressure bonding. In the present document, at the time of preliminary pressure joining, deaeration was initiated at a temperature of 40 °C, 50 °C, and 60 °C. (TOTAL PRESSURE JOIN)
[00150] The laminated (laminated) glass structure that was completely pressure joined by the aforementioned method was placed in an autoclave and kept under conditions of a temperature of 140 °C and a pressure of 1,300 kPa for 10 minutes. The laminated glass was then cooled to 50 °C and the pressure was returned to atmospheric pressure to complete the full pressure bond. In this way, laminated glass was prepared. (LAMINATED GLASS COOKING TEST)
[00151] The laminated glass obtained was heated for 2 hours in an oven at 140 °C. Therefore, the laminated glass was taken out of the oven and allowed to cool for 3 hours and then the external appearance of the laminated glass was visually observed. For 20 sheets of laminated glass, the number of laminated glass in which bubbles (air bubbles) occurred between the glass plate and the laminated glass interlayer film was counted. A case where the number of laminated glass on which bubbles occurred under all conditions was equal to or less than 5 was assessed as "O" and a case where the number of laminated glass on which the bubbles bubbles occurred was equal to or greater than 6 or "X". (2) Optical deformation evaluation
[00152] A fluorescent lamp (FL32S.D manufactured by Panasonic Corporation) was placed at a point 7 m away from an observer and the laminated glass obtained was placed at a point 40 cm away from the observer in a straight line connecting the fluorescent lamp to the viewer, such as laminated glass inclined by 20° to a horizontal plane. A case where the fluorescent lamp was seen to be distorted through laminated glass was rated to be "X" and a case where the fluorescent lamp was seen to be undistorted through laminated glass was rated to be "O". (3) Evaluation of the occurrence of ghost image
[00153] Through the use of two types of light sources 1 and 2 that have different brightness, whether a ghost image occurred was evaluated or not. A light source 1 was a 10 W silica light bulb (manufactured by Kyokko Ins., PS55 E 26 110 V-10 W, a total luminous flux of 70 lm) which was considered to be a light source having general glare that can enter the window panes of automobiles, aircraft, buildings and the like. Light source 2 was a 40 W silica light bulb (manufactured by ASAHI ELECTRIC CO., LTD., LW 100 V 38 W-W, a total luminous flux of 440 lm) that was considered to be a light source. light that has particularly high brightness among the lights that can enter the window panes of automobiles, aircraft, buildings, and the like. Using the method based on JIS R 3212(2008), it was evaluated whether or not a ghost image occurred in the laminated glass obtained. As a result, a case where only a single image was observed when either light source 1 and light source 2 were used or a case where 15 minutes of double arc image was evaluated to be "OO" . Also, a case where a ghost image occurred when light source 2 was used but a single image was observed when light source 1 was used or a case where 15 minutes of double arc image was evaluated to be "THE". Also, a case where a triple image occurred when either light source 1 and light source 2 were used was evaluated to be "X".
[00154] In the present document, laminated glass was measured considering that the angle of the same actually mounted on a car is 30°. Furthermore, layer A was arranged so that an angle formed between the recess which is shaped like a notched line formed on the surface of layer A and a horizontal direction becomes 5° and layer B was arranged so that an angle formed between the indentation which is shaped like a notched line formed on the surface of layer C and a horizontal direction becomes -5°.
[00155] Furthermore, 15 minutes double arc image was not an image that results from the interlayer film, but an image that results from the glass.

INDUSTRIAL APPLICABILITY
[00156] According to the present invention, it is possible to provide an intermediate layer film for laminated glass that includes 2 or more resin layers laminated on top of each other, exhibit excellent deaeration properties in a laminated glass manufacturing process, and can display the occurrence of ghost images and provide laminated glass that includes the interlayer film for laminated glass. NUMERICAL REFERENCE LIST1 a randomly selected recess2 recess adjacent to a randomly selected recess3 recess adjacent to a randomly selected recess4 range between recess 1 and recess 2B gap between recess 1 and recess 310 resin layer 20 resin layer having a surface that includes a large number of recesses and a large number of protrusions 21 resin layer surface 20 having a large number of recesses and a large number of protrusions22 super resin layer surface 20 on the side that came into contact with resin layer 1030 resin layer

权利要求:
Claims (6)
[0001]
1. Interlayer film for laminated glass comprising 2 or more layers of resin (30) laminated on top of each other, wherein the interlayer film has a large number of recesses and a large number of protrusions on at least one surface of the same, each of the recesses (1,2,3) has a groove shape with a continuous bottom, the recesses adjacent to each other are parallel to each other and regularly arranged in a line, characterized by the fact that inside the surface ( 21) which includes the large number of recesses and the large number of protrusions, a groove depth (Rzg) of the recesses measured based on JIS B-0601(1994) is 10 μm to 40 μm, the range (A, B) between grooves having a groove shape with a continuous bottom is not more than 500 μm, and an average roughness of 10 points (Rz) of a surface of a resin layer (20) which has the surface that includes the large number of grooves and the large number of bulges the measurement based on JIS B 0601(1994) is less than 2.7 μm, and the average roughness of 10 points (Rz) is obtained by removing the resin layer (20) that has the surface that includes the large number of recesses and the large number of bulges from another resin layer that comes into direct contact with the aforementioned resin layer (20) and then measuring the surface (22) of the resin removed on one side of the other layer of resin mentioned above (20) that came into direct contact with the removed resin layer (20) based on JIS B 0601(1994).
[0002]
2. Interlayer film for laminated glass, according to claim 1, characterized in that the recesses adjacent to each other are parallel to each other and arranged in a line at an equal interval.
[0003]
3. Interlayer film for laminated glass, according to claim 1 or 2, characterized in that the resin layers contain polyvinyl acetal and a plasticizer.
[0004]
4. Intermediate layer film for laminated glass, according to claim 3, characterized in that it comprises at least: a first layer of resin; and a second resin layer, wherein the amount of hydroxyl groups of the polyvinyl acetal contained in the first resin layer is different from the amount of hydroxyl groups of the polyvinyl acetal contained in the second resin layer.
[0005]
5. Intermediate layer film for laminated glass, according to claim 3, characterized by the fact that the plasticizer content in the first resin layer in relation to 100 parts by mass of polyvinyl acetal is different from the plasticizer content in the second layer of resin in relation to 100 parts of polyvinyl acetal.
[0006]
6. Intermediate layer film for laminated glass according to claim 1, characterized in that it comprises: 2 protective layers; and a soundproofing layer laminated between the protective layers, wherein the soundproofing layer contains a plasticizer in an amount of 45 parts by mass to 80 parts by mass with respect to 100 parts by mass of polyvinyl acetal, the protective layers contain a plasticizer in an amount of 20 parts by mass to 45 parts by mass with respect to 100 parts by mass of polyvinyl acetal, the protective layers have a large number of recesses and a large number of protrusions on at least one surface thereof, each of the recesses has a groove shape with a continuous bottom, the recesses adjacent to each other are parallel to each other and regularly arranged in a line, within the surface of the protective layers which have the large number of recesses and the large number of bulges, a groove depth (Rzg) of the grooves measured based on JIS B-0601(1994) is 10 μm to 40 μm, the gap between the grooves having a groove with a continuous bottom is less than 500 μm, and an average roughness of 10 points (Rz) of a surface of the protective layer having the surface including the large number of recesses and the large number of bulges measured based on JIS B 0601 (1994) is less than 2.7 μm, and the average roughness of 10 points (Rz) is obtained by removing the protective layer that has the surface that includes the large number of recesses and the large number of protrusions of the acoustic insulation layer. and then measuring the surface of the protective layer removed on one side of the sound insulation layer based on JIS B 0601(1994).

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法律状态:
2019-11-12| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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2021-08-10| B06A| Patent application procedure suspended [chapter 6.1 patent gazette]|

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2021-11-09| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

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2022-01-04| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 01/08/2014, OBSERVADAS AS CONDICOES LEGAIS. |

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2022-02-22| B16D| Grant of patent or certificate of addition of invention cancelled|Free format text: ANULADA A PUBLICACAO CODIGO 16.1 NA RPI NO 2661 DE 04/01/2022 POR TER SIDO INDEVIDA. |

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2022-03-03| B09X| Republication of the decision to grant [chapter 9.1.3 patent gazette]|

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