JP2018168013A - Interlayer for laminated glass, laminated glass, and method for producing interlayer for laminated glass - Google Patents
Interlayer for laminated glass, laminated glass, and method for producing interlayer for laminated glass Download PDFInfo
- Publication number
- JP2018168013A JP2018168013A JP2017066005A JP2017066005A JP2018168013A JP 2018168013 A JP2018168013 A JP 2018168013A JP 2017066005 A JP2017066005 A JP 2017066005A JP 2017066005 A JP2017066005 A JP 2017066005A JP 2018168013 A JP2018168013 A JP 2018168013A
- Authority
- JP
- Japan
- Prior art keywords
- layer
- laminated glass
- light control
- transparent conductive
- interlayer film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000005340 laminated glass Substances 0.000 title claims abstract description 87
- 239000011229 interlayer Substances 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 13
- 239000010410 layer Substances 0.000 claims abstract description 139
- 239000012790 adhesive layer Substances 0.000 claims description 59
- 229920005989 resin Polymers 0.000 claims description 25
- 239000011347 resin Substances 0.000 claims description 25
- 239000011521 glass Substances 0.000 claims description 20
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- 239000000463 material Substances 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- 239000000565 sealant Substances 0.000 claims description 12
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 11
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 claims description 11
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- 238000000034 method Methods 0.000 claims description 9
- 229920001187 thermosetting polymer Polymers 0.000 claims description 7
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- 238000011156 evaluation Methods 0.000 description 7
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- 239000005357 flat glass Substances 0.000 description 6
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- 125000004432 carbon atom Chemical group C* 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 125000006850 spacer group Chemical group 0.000 description 5
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- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 description 3
- OJXOOFXUHZAXLO-UHFFFAOYSA-M magnesium;1-bromo-3-methanidylbenzene;bromide Chemical compound [Mg+2].[Br-].[CH2-]C1=CC=CC(Br)=C1 OJXOOFXUHZAXLO-UHFFFAOYSA-M 0.000 description 3
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- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 description 2
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- KZVBBTZJMSWGTK-UHFFFAOYSA-N 1-[2-(2-butoxyethoxy)ethoxy]butane Chemical compound CCCCOCCOCCOCCCC KZVBBTZJMSWGTK-UHFFFAOYSA-N 0.000 description 1
- DLZBUNUDESZERL-UHFFFAOYSA-N 1-o-heptyl 6-o-nonyl hexanedioate Chemical compound CCCCCCCCCOC(=O)CCCCC(=O)OCCCCCCC DLZBUNUDESZERL-UHFFFAOYSA-N 0.000 description 1
- UNNGUFMVYQJGTD-UHFFFAOYSA-N 2-Ethylbutanal Chemical compound CCC(CC)C=O UNNGUFMVYQJGTD-UHFFFAOYSA-N 0.000 description 1
- GCDUWJFWXVRGSM-UHFFFAOYSA-N 2-[2-(2-heptanoyloxyethoxy)ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCC GCDUWJFWXVRGSM-UHFFFAOYSA-N 0.000 description 1
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- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 description 1
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- SXKCDRRSQHPBOI-UHFFFAOYSA-N 6-o-cyclohexyl 1-o-hexyl hexanedioate Chemical compound CCCCCCOC(=O)CCCCC(=O)OC1CCCCC1 SXKCDRRSQHPBOI-UHFFFAOYSA-N 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
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- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
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- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10165—Functional features of the laminated safety glass or glazing
- B32B17/10174—Coatings of a metallic or dielectric material on a constituent layer of glass or polymer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10165—Functional features of the laminated safety glass or glazing
- B32B17/10431—Specific parts for the modulation of light incorporated into the laminated safety glass or glazing
- B32B17/10467—Variable transmission
- B32B17/10495—Variable transmission optoelectronic, i.e. optical valve
- B32B17/10504—Liquid crystal layer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10788—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing ethylene vinylacetate
Landscapes
- Liquid Crystal (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
Description
本発明は、調光体層を有しながら、周辺部に調光体の染み出しがない合わせガラス用中間膜、該合わせガラス用中間膜を用いた合わせガラス、及び、該合わせガラス用中間膜の製造方法に関する。 The present invention relates to an interlayer film for laminated glass that has a light control layer and does not bleed out the light control body in the peripheral portion, a laminated glass using the interlayer film for laminated glass, and the interlayer film for laminated glass It relates to the manufacturing method.
電圧を印加することにより光の透過率が変化する調光体は、広く知られている。上記調光体は、液晶材料を用いた調光体と、エレクトロクロミック化合物を用いた調光体とに大別される。なかでも、液晶材料を用いた調光体は、電光板等の表示装置に応用することを目的とする検討が重ねられてきた。 A dimmer whose light transmittance is changed by applying a voltage is widely known. The dimmer is roughly classified into a dimmer using a liquid crystal material and a dimmer using an electrochromic compound. In particular, dimming bodies using a liquid crystal material have been repeatedly studied for the purpose of being applied to display devices such as lightning plates.
近年、自動車等の車内や建築物等の室内の温度を制御するために、調光体を合わせガラス用中間膜として用いた合わせガラスが提案されている(例えば、特許文献1等)。具体的には、厚み方向に接着層、調光体層、接着層の順に積層された構造を有する合わせガラス用中間膜が提案されている。このような合わせガラス用中間膜を用いることにより、合わせガラスの光線透過率を制御することができると考えられている。
しかしながら、このような調光体層を有する合わせガラス用中間膜では、周辺部に調光体の一部が染み出し、汚染してしまうことがあるという問題があった。とりわけ、調光体として液晶材料を用いた場合にこの問題が顕著であった。
In recent years, a laminated glass using a dimmer as an interlayer film for laminated glass has been proposed in order to control the temperature in the interior of a vehicle such as an automobile or a building (for example, Patent Document 1). Specifically, an interlayer film for laminated glass having a structure in which an adhesive layer, a light control layer, and an adhesive layer are laminated in this order in the thickness direction has been proposed. It is considered that the light transmittance of the laminated glass can be controlled by using such an interlayer film for laminated glass.
However, in the interlayer film for laminated glass having such a light control layer, there is a problem that a part of the light control body oozes out to the periphery and may be contaminated. In particular, this problem is remarkable when a liquid crystal material is used as the light control member.
本発明は、上記現状に鑑み、調光体層を有しながら、周辺部に調光体の染み出しがない合わせガラス用中間膜、該合わせガラス用中間膜を用いた合わせガラス、及び、該合わせガラス用中間膜の製造方法を提供することを目的とする。 In view of the above situation, the present invention has an interlayer film for laminated glass that has a light control layer and does not bleed out the light control body in the periphery, laminated glass using the interlayer film for laminated glass, and the It aims at providing the manufacturing method of the intermediate film for laminated glasses.
本発明は、厚み方向に接着層、調光体層、接着層の順に積層された構造を有する合わせガラス用中間膜であって、前記調光体層は、周縁部がシール層により封止されている合わせガラス用中間膜である。
以下に本発明を詳述する。
The present invention is an interlayer film for laminated glass having a structure in which an adhesive layer, a light control layer, and an adhesive layer are laminated in this order in the thickness direction, and the light control layer is sealed at its periphery by a sealing layer. It is an interlayer film for laminated glass.
The present invention is described in detail below.
厚み方向に接着層、調光体層、接着層の順に積層された構造を有する合わせガラス用中間膜は、通常は、まず接着層、調光体層、接着層の順に積層された積層体を調製し、これを100〜150℃程度の温度をかけながらオートクレーブによって圧着するラミネート工程を経て製造される。本発明者らは、該ラミネート工程において熱圧着したときに、合わせガラス用中間膜の調光体層から調光体の一部が染み出してしまうことを見出した。
本発明者らは、鋭意検討の結果、調光体層の周縁部をシール層により封止することにより、ラミネート工程時に調光体層から調光体が染み出してしまうのを防止できることを見出し、本発明を完成した。
An interlayer film for laminated glass having a structure in which an adhesive layer, a light control layer, and an adhesive layer are laminated in the thickness direction is usually a laminate in which an adhesive layer, a light control layer, and an adhesive layer are first laminated in this order. It is manufactured through a laminating process in which it is prepared and pressure-bonded by an autoclave while applying a temperature of about 100 to 150 ° C. The inventors of the present invention have found that when the thermocompression bonding is performed in the laminating step, a part of the light control body exudes from the light control material layer of the interlayer film for laminated glass.
As a result of intensive studies, the present inventors have found that the light control body can be prevented from oozing out of the light control material layer during the laminating process by sealing the periphery of the light control material layer with a seal layer. The present invention has been completed.
本発明の合わせガラス用中間膜は、厚み方向に接着層、調光体層、接着層の順に積層された構造を有する。上記調光体層を有することにより、本発明の合わせガラス用中間膜に電圧を印加することにより光の透過率を変化させることができる。 The interlayer film for laminated glass of the present invention has a structure in which an adhesive layer, a light control layer, and an adhesive layer are laminated in this order in the thickness direction. By having the said light control body layer, the transmittance | permeability of light can be changed by applying a voltage to the intermediate film for laminated glasses of this invention.
上記調光体層に含まれる調光体としては特に限定されず、液晶材料を用いた調光体、エレクトロクロミック化合物を用いた調光体等の従来公知の調光体を用いることができる。なかでも、液晶材料を用いた調光体や、SPD(Suspended Particle Device)等の比較的流動性の高い調光体を用いた場合に、本願発明は特に有効である。 It does not specifically limit as a light control body contained in the said light control body layer, Conventionally known light control bodies, such as a light control body using a liquid-crystal material, a light control body using an electrochromic compound, can be used. In particular, the present invention is particularly effective when a light control body using a liquid crystal material or a light control body with relatively high fluidity such as SPD (Suspended Particle Device) is used.
上記液晶材料からなる調光体としては、例えば、TN液晶、STN液晶、TFT液晶、及びこれらの液晶を高分子マトリックスに含浸させた材料等が挙げられる。 Examples of the light modulator made of the liquid crystal material include TN liquid crystal, STN liquid crystal, TFT liquid crystal, and a material obtained by impregnating these liquid crystals into a polymer matrix.
上記調光体が比較的流動性の高い調光体である場合には、上記調光体層は、スペーサ粒子を含有することが好ましい。上記スペーサ粒子を含有することにより、調光体層の厚みを安定化させることができる。上記スペーサ粒子としては特に限定されず、無機粒子や有機粒子を用いることができる。
また、上記調光体として液晶に高分子架橋体を配合したゲル状の調光体(例えば、九州ナノテック社製、商品名「MIYO−フィルム」)等を用いる場合には、スペーサ粒子を用いなくとも、調光体層の厚みを安定化させることができる。
When the light control body is a light control body having a relatively high fluidity, the light control body layer preferably contains spacer particles. By containing the spacer particles, it is possible to stabilize the thickness of the light control layer. The spacer particles are not particularly limited, and inorganic particles and organic particles can be used.
In addition, when using a gel-like light-adjusting material (for example, trade name “MIYO-film” manufactured by Kyushu Nanotech Co., Ltd.), which is a liquid crystal blended with a polymer cross-linked material, the spacer particles are not used. In both cases, the thickness of the light control layer can be stabilized.
上記調光体層の厚みは特に限定されないが、好ましい下限は80μm、好ましい上限は500μmである。上記調光体層の厚みがこの範囲内であると、電圧を印加することにより光の透過率を充分に変化させることができる。上記調光体層の厚さのより好ましい下限は100μm、より好ましい上限は400μmである。 Although the thickness of the said light control body layer is not specifically limited, A preferable minimum is 80 micrometers and a preferable upper limit is 500 micrometers. When the thickness of the light control layer is within this range, the light transmittance can be sufficiently changed by applying a voltage. The minimum with more preferable thickness of the said light control body layer is 100 micrometers, and a more preferable upper limit is 400 micrometers.
上記接着層は、上記調光体層を挟持して、ガラスに対する密着性を発揮させる役割を有する。
上記接着層は、熱可塑性樹脂を含有することが好ましい。
上記熱可塑性樹脂としては、例えば、ポリフッ化ビニリデン、ポリテトラフルオロエチレン、フッ化ビニリデン−六フッ化プロピレン共重合体、ポリ三フッ化エチレン、アクリロニトリル−ブタジエン−スチレン共重合体、ポリエステル、ポリエーテル、ポリアミド、ポリカーボネート、ポリアクリレート、ポリメタクリレート、ポリ塩化ビニル、ポリエチレン、ポリプロピレン、ポリスチレン、ポリビニルアセタール、エチレン−酢酸ビニル共重合体等が挙げられる。なかでも、上記接着層はポリビニルアセタール又はエチレン−酢酸ビニル共重合体を含有することが好ましく、ポリビニルアセタールを含有することがより好ましい。
The said adhesive layer has the role which pinches | interposes the said light control body layer and exhibits the adhesiveness with respect to glass.
The adhesive layer preferably contains a thermoplastic resin.
Examples of the thermoplastic resin include polyvinylidene fluoride, polytetrafluoroethylene, vinylidene fluoride-hexafluoropropylene copolymer, polytrifluoride ethylene, acrylonitrile-butadiene-styrene copolymer, polyester, polyether, Examples thereof include polyamide, polycarbonate, polyacrylate, polymethacrylate, polyvinyl chloride, polyethylene, polypropylene, polystyrene, polyvinyl acetal, and ethylene-vinyl acetate copolymer. Especially, it is preferable that the said contact bonding layer contains a polyvinyl acetal or an ethylene-vinyl acetate copolymer, and it is more preferable to contain a polyvinyl acetal.
上記ポリビニルアセタールは、ポリビニルアルコールをアルデヒドでアセタール化して得られるポリビニルアセタールであれば特に限定されないが、ポリビニルブチラールが好適である。また、必要に応じて2種以上のポリビニルアセタールを併用してもよい。 The polyvinyl acetal is not particularly limited as long as it is a polyvinyl acetal obtained by acetalizing polyvinyl alcohol with an aldehyde, but polyvinyl butyral is preferable. Moreover, you may use together 2 or more types of polyvinyl acetal as needed.
上記ポリビニルアセタールのアセタール化度の好ましい下限は40モル%、好ましい上限は85モル%であり、より好ましい下限は60モル%、より好ましい上限は75モル%である。
上記ポリビニルアセタールは、水酸基量の好ましい下限が15モル%、好ましい上限が35モル%である。水酸基量が15モル%以上であると、合わせガラス用中間膜とガラスとの接着性が高くなる。水酸基量が35モル%以下であると、合わせガラス用中間膜の取り扱いが容易になる。
なお、上記アセタール化度及び水酸基量は、例えば、JIS K6728「ポリビニルブチラール試験方法」に準拠して測定できる。
The preferable lower limit of the degree of acetalization of the polyvinyl acetal is 40 mol%, the preferable upper limit is 85 mol%, the more preferable lower limit is 60 mol%, and the more preferable upper limit is 75 mol%.
The polyvinyl acetal has a preferred lower limit of the hydroxyl group content of 15 mol% and a preferred upper limit of 35 mol%. Adhesiveness between the interlayer film for laminated glass and the glass is increased when the amount of the hydroxyl group is 15 mol% or more. When the hydroxyl group amount is 35 mol% or less, handling of the interlayer film for laminated glass becomes easy.
The degree of acetalization and the amount of hydroxyl groups can be measured in accordance with, for example, JIS K6728 “Testing method for polyvinyl butyral”.
上記ポリビニルアセタールは、ポリビニルアルコールをアルデヒドでアセタール化することにより調製することができる。
上記ポリビニルアルコールは、通常、ポリ酢酸ビニルを鹸化することにより得られ、鹸化度70〜99.8モル%のポリビニルアルコールが一般的に用いられる。上記ポリビニルアルコールの鹸化度は、80〜99.8モル%であることが好ましい。
上記ポリビニルアルコールの重合度の好ましい下限は500、好ましい上限は4000である。上記ポリビニルアルコールの重合度が500以上であると、得られる合わせガラスの耐貫通性が高くなる。上記ポリビニルアルコールの重合度が4000以下であると、合わせガラス用中間膜の成形が容易になる。上記ポリビニルアルコールの重合度のより好ましい下限は1000、より好ましい上限は3600である。
The polyvinyl acetal can be prepared by acetalizing polyvinyl alcohol with an aldehyde.
The polyvinyl alcohol is usually obtained by saponifying polyvinyl acetate, and polyvinyl alcohol having a saponification degree of 70 to 99.8 mol% is generally used. The saponification degree of the polyvinyl alcohol is preferably 80 to 99.8 mol%.
The preferable lower limit of the polymerization degree of the polyvinyl alcohol is 500, and the preferable upper limit is 4000. When the polymerization degree of the polyvinyl alcohol is 500 or more, the penetration resistance of the obtained laminated glass is increased. When the polymerization degree of the polyvinyl alcohol is 4000 or less, the interlayer film for laminated glass can be easily molded. The minimum with a more preferable polymerization degree of the said polyvinyl alcohol is 1000, and a more preferable upper limit is 3600.
上記アルデヒドは特に限定されないが、一般には、炭素数が1〜10のアルデヒドが好適に用いられる。上記炭素数が1〜10のアルデヒドは特に限定されず、例えば、n−ブチルアルデヒド、イソブチルアルデヒド、n−バレルアルデヒド、2−エチルブチルアルデヒド、n−ヘキシルアルデヒド、n−オクチルアルデヒド、n−ノニルアルデヒド、n−デシルアルデヒド、ホルムアルデヒド、アセトアルデヒド、ベンズアルデヒド等が挙げられる。なかでも、n−ブチルアルデヒド、n−ヘキシルアルデヒド、n−バレルアルデヒドが好ましく、n−ブチルアルデヒドがより好ましい。これらのアルデヒドは単独で用いられてもよく、2種以上を併用してもよい。 The aldehyde is not particularly limited, but generally an aldehyde having 1 to 10 carbon atoms is preferably used. The aldehyde having 1 to 10 carbon atoms is not particularly limited. For example, n-butyraldehyde, isobutyraldehyde, n-valeraldehyde, 2-ethylbutyraldehyde, n-hexylaldehyde, n-octylaldehyde, n-nonylaldehyde N-decylaldehyde, formaldehyde, acetaldehyde, benzaldehyde and the like. Of these, n-butyraldehyde, n-hexylaldehyde, and n-valeraldehyde are preferable, and n-butyraldehyde is more preferable. These aldehydes may be used alone or in combination of two or more.
上記接着層は、可塑剤を含有することが好ましい。上記可塑剤は特に限定されず、例えば、一塩基性有機酸エステル、多塩基性有機酸エステル等の有機エステル可塑剤、有機リン酸可塑剤、有機亜リン酸可塑剤等のリン酸可塑剤等が挙げられる。上記可塑剤は液状可塑剤であることが好ましい。 The adhesive layer preferably contains a plasticizer. The plasticizer is not particularly limited, and examples thereof include organic ester plasticizers such as monobasic organic acid esters and polybasic organic acid esters, phosphoric acid plasticizers such as organic phosphoric acid plasticizers and organic phosphorous acid plasticizers, and the like. Is mentioned. The plasticizer is preferably a liquid plasticizer.
上記一塩基性有機酸エステルは特に限定されないが、例えば、トリエチレングリコール、テトラエチレングリコール、トリプロピレングリコール等のグリコールと、酪酸、イソ酪酸、カプロン酸、2−エチル酪酸、ヘプチル酸、n−オクチル酸、2−エチルヘキシル酸、ペラルゴン酸(n−ノニル酸)、デシル酸等の一塩基性有機酸との反応によって得られたグリコールエステル等が挙げられる。なかでも、トリエチレングリコールジカプロン酸エステル、トリエチレングリコールジ−2−エチル酪酸エステル、トリエチレングリコールジ−n−オクチル酸エステル、トリエチレングリコールジ−2−エチルヘキシル酸エステル等が好適である。 The monobasic organic acid ester is not particularly limited. For example, glycols such as triethylene glycol, tetraethylene glycol, and tripropylene glycol, butyric acid, isobutyric acid, caproic acid, 2-ethylbutyric acid, heptylic acid, and n-octyl Examples thereof include glycol esters obtained by reaction with monobasic organic acids such as acid, 2-ethylhexyl acid, pelargonic acid (n-nonyl acid), and decyl acid. Of these, triethylene glycol dicaproate, triethylene glycol di-2-ethylbutyrate, triethylene glycol di-n-octylate, triethylene glycol di-2-ethylhexylate and the like are preferable.
上記多塩基性有機酸エステルは特に限定されないが、例えば、アジピン酸、セバシン酸、アゼライン酸等の多塩基性有機酸と、炭素数4〜8の直鎖又は分岐構造を有するアルコールとのエステル化合物が挙げられる。なかでも、ジブチルセバシン酸エステル、ジオクチルアゼライン酸エステル、ジブチルカルビトールアジピン酸エステル等が好適である。 Although the said polybasic organic acid ester is not specifically limited, For example, ester compound of polybasic organic acid, such as adipic acid, sebacic acid, azelaic acid, and the alcohol which has a C4-C8 linear or branched structure Is mentioned. Of these, dibutyl sebacic acid ester, dioctyl azelaic acid ester, dibutyl carbitol adipic acid ester and the like are preferable.
上記有機エステル可塑剤は特に限定されず、トリエチレングリコールジ−2−エチルブチレート、トリエチレングリコールジ−2−エチルヘキサノエート、トリエチレングリコールジカプリレート、トリエチレングリコールジ−n−オクタノエート、トリエチレングリコールジ−n−ヘプタノエート、テトラエチレングリコールジ−n−ヘプタノエート、テトラエチレングリコールジ−2−エチルヘキサノエート、ジブチルセバケート、ジオクチルアゼレート、ジブチルカルビトールアジペート、エチレングリコールジ−2−エチルブチレート、1,3−プロピレングリコールジ−2−エチルブチレート、1,4−ブチレングリコールジ−2−エチルブチレート、ジエチレングリコールジ−2−エチルブチレート、ジエチレングリコールジ−2−エチルヘキサノエート、ジプロピレングリコールジ−2−エチルブチレート、トリエチレングリコールジ−2−エチルペンタノエート、テトラエチレングリコールジ−2−エチルブチレート、ジエチレングリコールジカプリエート、アジピン酸ジヘキシル、アジピン酸ジオクチル、アジピン酸ヘキシルシクロヘキシル、アジピン酸ジイソノニル、アジピン酸ヘプチルノニル、セバシン酸ジブチル、油変性セバシン酸アルキド、リン酸エステルとアジピン酸エステルとの混合物、アジピン酸エステル、炭素数4〜9のアルキルアルコール及び炭素数4〜9の環状アルコールから作製された混合型アジピン酸エステル、アジピン酸ヘキシル等の炭素数6〜8のアジピン酸エステル等が挙げられる。 The organic ester plasticizer is not particularly limited, and triethylene glycol di-2-ethylbutyrate, triethylene glycol di-2-ethylhexanoate, triethylene glycol dicaprylate, triethylene glycol di-n-octanoate, Triethylene glycol di-n-heptanoate, tetraethylene glycol di-n-heptanoate, tetraethylene glycol di-2-ethylhexanoate, dibutyl sebacate, dioctyl azelate, dibutyl carbitol adipate, ethylene glycol di-2-ethyl Butyrate, 1,3-propylene glycol di-2-ethyl butyrate, 1,4-butylene glycol di-2-ethyl butyrate, diethylene glycol di-2-ethyl butyrate, diethylene glycol di- -Ethyl hexanoate, dipropylene glycol di-2-ethyl butyrate, triethylene glycol di-2-ethyl pentanoate, tetraethylene glycol di-2-ethyl butyrate, diethylene glycol dicapryate, dihexyl adipate, adipine Dioctyl acid, hexyl cyclohexyl adipate, diisononyl adipate, heptylnonyl adipate, dibutyl sebacate, oil-modified sebacic acid alkyd, a mixture of phosphate ester and adipic acid ester, adipic acid ester, alkyl alcohol having 4 to 9 carbon atoms and Examples thereof include mixed adipic acid esters prepared from cyclic alcohols having 4 to 9 carbon atoms and adipic acid esters having 6 to 8 carbon atoms such as hexyl adipate.
上記有機リン酸可塑剤は特に限定されず、例えば、トリブトキシエチルホスフェート、イソデシルフェニルホスフェート、トリイソプロピルホスフェート等が挙げられる。 The organophosphate plasticizer is not particularly limited, and examples thereof include tributoxyethyl phosphate, isodecylphenyl phosphate, triisopropyl phosphate, and the like.
更に、上記可塑剤として、加水分解を起こしにくいため、トリエチレングリコールジ−2−エチルヘキサノエート(3GO)、トリエチレングリコールジ−2−エチルブチレート(3GH)、テトラエチレングリコールジ−2−エチルヘキサノエート(4GO)、ジヘキシルアジペート(DHA)を含有することが好ましく、テトラエチレングリコールジ−2−エチルヘキサノエート(4GO)、トリエチレングリコールジ−2−エチルヘキサノエート(3GO)を含有することがより好ましく、特にトリエチレングリコールジ−2−エチルヘキサノエート(3GO)を含有することがより好ましい。 Furthermore, since it is difficult to cause hydrolysis as the plasticizer, triethylene glycol di-2-ethylhexanoate (3GO), triethylene glycol di-2-ethylbutyrate (3GH), tetraethylene glycol di-2- It preferably contains ethyl hexanoate (4GO) and dihexyl adipate (DHA), and tetraethylene glycol di-2-ethylhexanoate (4GO) and triethylene glycol di-2-ethylhexanoate (3GO). More preferably, it contains triethylene glycol di-2-ethylhexanoate (3GO).
上記接着層における上記可塑剤の含有量は特に限定されないが、上記ポリビニルアセタール100重量部に対する好ましい下限が30重量部、好ましい上限が90重量部である。上記可塑剤の含有量が30重量部以上であると、合わせガラス用中間膜の溶融粘度が低くなり、これを合わせガラス用中間膜として合わせガラスを製造する際の脱気性が高くなる。上記可塑剤の含有量が90重量部以下であると、合わせガラス用中間膜の透明性が高くなる。上記可塑剤の含有量のより好ましい下限は35重量部、より好ましい上限は70重量部、更に好ましい上限は63重量部である。 The content of the plasticizer in the adhesive layer is not particularly limited, but a preferable lower limit with respect to 100 parts by weight of the polyvinyl acetal is 30 parts by weight, and a preferable upper limit is 90 parts by weight. When the content of the plasticizer is 30 parts by weight or more, the melt viscosity of the laminated glass interlayer film is lowered, and the degassing property when the laminated glass is produced using this laminated glass interlayer film is increased. When the content of the plasticizer is 90 parts by weight or less, the transparency of the interlayer film for laminated glass increases. The minimum with more preferable content of the said plasticizer is 35 weight part, a more preferable upper limit is 70 weight part, and a still more preferable upper limit is 63 weight part.
上記接着層は、接着力調整剤を含有することが好ましい。接着力調整剤を含有することにより、ガラスに対する接着力を調整して、耐貫通性に優れる合わせガラスを得ることができる。
上記接着力調整剤としては、例えば、アルカリ金属塩又はアルカリ土類金属塩が好適に用いられる。上記接着力調整剤として、例えば、カリウム、ナトリウム、マグネシウム等の塩が挙げられる。
上記塩を構成する酸としては、例えば、オクチル酸、ヘキシル酸、2−エチル酪酸、酪酸、酢酸、蟻酸等のカルボン酸の有機酸、又は、塩酸、硝酸等の無機酸が挙げられる。
The adhesive layer preferably contains an adhesive strength modifier. By containing the adhesive strength adjusting agent, the adhesive strength to glass can be adjusted, and a laminated glass excellent in penetration resistance can be obtained.
As said adhesive force regulator, an alkali metal salt or alkaline-earth metal salt is used suitably, for example. As said adhesive force regulator, salts, such as potassium, sodium, magnesium, are mentioned, for example.
Examples of the acid constituting the salt include organic acids of carboxylic acids such as octylic acid, hexylic acid, 2-ethylbutyric acid, butyric acid, acetic acid, formic acid, and inorganic acids such as hydrochloric acid and nitric acid.
本発明の合わせガラス用中間膜に遮熱性が要求される場合には、上記接着層は、熱線吸収剤を含有してもよい。
上記熱線吸収剤は、赤外線を遮蔽する性能を有すれば特に限定されないが、錫ドープ酸化インジウム(ITO)粒子、アンチモンドープ酸化錫(ATO)粒子、アルミニウムドープ酸化亜鉛(AZO)粒子、インジウムドープ酸化亜鉛(IZO)粒子、錫ドープ酸化亜鉛粒子、珪素ドープ酸化亜鉛粒子、6ホウ化ランタン粒子及び6ホウ化セリウム粒子からなる群より選択される少なくとも1種が好適である。
When heat-shielding property is requested | required of the intermediate film for laminated glasses of this invention, the said contact bonding layer may contain a heat ray absorber.
The heat ray absorber is not particularly limited as long as it has the ability to shield infrared rays, but is tin-doped indium oxide (ITO) particles, antimony-doped tin oxide (ATO) particles, aluminum-doped zinc oxide (AZO) particles, indium-doped oxide. At least one selected from the group consisting of zinc (IZO) particles, tin-doped zinc oxide particles, silicon-doped zinc oxide particles, lanthanum hexaboride particles and cerium hexaboride particles is preferred.
上記接着層は、必要に応じて、紫外線遮蔽剤、酸化防止剤、光安定剤、帯電防止剤等の従来公知の添加剤を含有してもよい。 The adhesive layer may contain conventionally known additives such as an ultraviolet shielding agent, an antioxidant, a light stabilizer, and an antistatic agent as necessary.
上記接着層の厚みは特に限定されないが、好ましい下限は100μm、好ましい上限は500μmである。また、上記接着層が複数存在する場合には、上記接着層の厚みの合計の好ましい下限は200μm、好ましい上限は1000μmである。上記接着層の厚み及び厚みの合計がこの範囲内であると、充分な耐久性が得られ、また、得られる合わせガラスの透明性、対貫通性等の基本品質が満たされる。上記接着層の厚みのより好ましい下限は250μm、より好ましい上限は400μmである。上記接着層の厚みの合計のより好ましい下限は500μm、より好ましい上限は800μmである。 Although the thickness of the said contact bonding layer is not specifically limited, A preferable minimum is 100 micrometers and a preferable upper limit is 500 micrometers. When a plurality of the adhesive layers are present, a preferable lower limit of the total thickness of the adhesive layers is 200 μm, and a preferable upper limit is 1000 μm. When the total thickness and thickness of the adhesive layer are within this range, sufficient durability can be obtained, and basic qualities such as transparency and penetrability of the obtained laminated glass are satisfied. The more preferable lower limit of the thickness of the adhesive layer is 250 μm, and the more preferable upper limit is 400 μm. The more preferable lower limit of the total thickness of the adhesive layer is 500 μm, and the more preferable upper limit is 800 μm.
本発明の合わせガラス用中間膜は、上記接着層の調光層に接する側の表面に透明導電層を有することが好ましい。このような透明導電層を有することにより、該透明導電層を介して上記調光体層に電圧を加えることにより、容易に光の透過率を変化させることができる。
上記透明導電層は、例えば、スズドープ酸化インジウム(ITO)、フッ素ドープ酸化スズ(FTO)等を含むことが好ましい。
The interlayer film for laminated glass of the present invention preferably has a transparent conductive layer on the surface of the adhesive layer on the side in contact with the light control layer. By having such a transparent conductive layer, it is possible to easily change the light transmittance by applying a voltage to the light control layer through the transparent conductive layer.
The transparent conductive layer preferably contains, for example, tin-doped indium oxide (ITO), fluorine-doped tin oxide (FTO), or the like.
本発明の合わせガラス用中間膜においては、上記調光体層は、周縁部がシール層により封止されている。これにより、ラミネート工程時に調光体層から調光体が染み出してしまうのを防止することができる。 In the interlayer film for laminated glass of the present invention, the light control layer is sealed at its peripheral edge portion by a seal layer. Thereby, it can prevent that a light control body oozes out from a light control layer at the time of a lamination process.
図1に、本発明の合わせガラス用中間膜の断面の一例を示す模式図を示した。
図1(a)に示した合わせガラス用中間膜1は、厚み方向に接着層2、調光体層3、接着層2の順に積層された構造を有する。接着層2の調光体層3に接する側の表面には、透明導電層4が設けられている。図1(a)において調光体層3は、その周縁部がシール層5により封止されている。シール層5は、2つの接着層2(透明導電層4)に挟み込まれている。
図1(b)に示した合わせガラス用中間膜10は、厚み方向に接着層20、調光体層30、接着層20の順に積層された構造を有する。接着層20の調光体層30に接する側の表面には、透明導電層40が設けられている。図1(b)において調光体層30は、その周縁部がシール層50により封止されている。シール層50は、接着層20(透明導電層40)、調光体層30、接着層20(透明導電層40)からなる積層体の周縁部に配置されている。
In FIG. 1, the schematic diagram which shows an example of the cross section of the intermediate film for laminated glasses of this invention was shown.
The interlayer film 1 for laminated glass shown in FIG. 1A has a structure in which an adhesive layer 2, a
The interlayer film for
上記シール層は、上記調光体層から調光体が染み出すのを防止できるものであれば特に限定されないが、光硬化性樹脂又は熱硬化性樹脂からなることが好ましい。光硬化性樹脂又は熱硬化性樹脂を用いれば、ラミネート工程前に光硬化性樹脂又は熱硬化性樹脂を硬化させてシール層を形成させることにより、確実に上記調光体層をシール層により封止して、調光体の染み出しを確実に防止することができる。なかでも、取り扱い性の点から、光硬化性樹脂を含有するシール剤がより好ましい。 The seal layer is not particularly limited as long as it can prevent the light adjuster from seeping out from the light adjuster layer, but is preferably made of a photocurable resin or a thermosetting resin. If a photocurable resin or a thermosetting resin is used, the photocurable resin or the thermosetting resin is cured before the laminating process to form a seal layer, thereby reliably sealing the light control layer with the seal layer. It is possible to reliably prevent the light control body from seeping out. Especially, the sealing agent containing photocurable resin is more preferable from the point of handleability.
上記光硬化性樹脂としては、光を照射することにより硬化するものであれば特に限定されないが、例えば、(メタ)アクリル樹脂、ウレタン樹脂等が好適である。上記(メタ)アクリル樹脂としては、多官能(メタ)アクリレートであることが好ましい。
上記熱硬化性樹脂としては、加熱することにより硬化するものであれば特に限定されないが、例えば、エポキシ樹脂、アミド樹脂等が好適である。
Although it will not specifically limit as said photocurable resin if it hardens | cures by irradiating light, For example, (meth) acrylic resin, urethane resin, etc. are suitable. The (meth) acrylic resin is preferably a polyfunctional (meth) acrylate.
The thermosetting resin is not particularly limited as long as it is cured by heating, and for example, an epoxy resin, an amide resin, and the like are preferable.
本発明の合わせガラス用中間膜を製造する方法としては特に限定されないが、例えば、一方の面に透明導電層を形成した2枚の接着層を作製する工程と、一方の透明導電層を形成した接着層の透明導電層側の周縁部に、光硬化性樹脂を含有するシール剤を枠状に塗工する工程と、上記透明導電層を形成した接着層上のシール剤の枠の内側に調光体を塗工して調光体層を形成する工程と、他方の透明導電層を形成した接着層を、透明導電層が調光体層側になるように重ね合わせた積層体を得る工程と、上記積層体に光を照射してシール剤を硬化させてシール層を形成する工程と、シール層形成後の積層体を30〜100℃の温度をかけながら圧着してラミネートする工程を有する方法が好適である。
なお、光硬化性樹脂を含有するシール剤が、光を照射してから硬化するまでにタイムラグがある、いわゆる後硬化性の光硬化性シール剤である場合には、上記積層体を得る工程の前に、光照射を行ってもよい。
Although it does not specifically limit as a method to manufacture the intermediate film for laminated glasses of this invention, For example, the process of producing two contact bonding layers which formed the transparent conductive layer in one side, and one transparent conductive layer were formed. A step of applying a sealant containing a photocurable resin in a frame shape on the peripheral edge of the adhesive layer on the transparent conductive layer side, and an inner side of the frame of the sealant on the adhesive layer on which the transparent conductive layer is formed. A step of forming a light control layer by applying a light body, and a step of obtaining a laminate in which the adhesive layer on which the other transparent conductive layer is formed is overlapped so that the transparent conductive layer is on the light control layer side And a step of irradiating the laminate with light to cure the sealant to form a seal layer, and a step of pressing and laminating the laminate after forming the seal layer while applying a temperature of 30 to 100 ° C. The method is preferred.
In the case where the sealant containing the photocurable resin is a so-called post-curing photocurable sealant having a time lag from irradiation to curing, the step of obtaining the laminate Before, light irradiation may be performed.
また、例えば、一方の面に透明導電層を形成した2枚の接着層を作製する工程と、一方の透明導電層を形成した接着層の透明導電層側の周縁部に、熱硬化性樹脂を含有するシール剤を枠状に塗工する工程と、上記透明導電層を形成した接着層上のシール剤の枠の内側に調光体を塗工して調光体層を形成する工程と、他方の透明導電層を形成した接着層を、透明導電層が調光体層側になるように重ね合わせて積層体を得る工程と、上記積層体を加熱してシール剤を硬化させてシール層を形成する工程と、シール層形成後の積層体を30〜100℃の温度をかけながら圧着してラミネートする工程を有する方法も好適である。
これらの合わせガラス用中間膜の製造方法もまた、本発明の1つである。
Also, for example, a thermosetting resin is applied to the peripheral portion on the transparent conductive layer side of the adhesive layer on which one transparent conductive layer is formed, and a step of preparing two adhesive layers having a transparent conductive layer formed on one side. A step of coating the sealing agent contained in a frame shape, a step of applying a light modulator on the inner side of the frame of the sealing agent on the adhesive layer on which the transparent conductive layer is formed, and forming a light modulator layer; The step of superimposing the adhesive layer on which the other transparent conductive layer is formed so that the transparent conductive layer is on the light control layer side to obtain a laminate, and heating the laminate to cure the sealing agent to seal layer A method including a step of forming a laminate and a step of pressing and laminating the laminate after forming the seal layer while applying a temperature of 30 to 100 ° C. is also suitable.
A method for producing these interlayer films for laminated glass is also one aspect of the present invention.
本発明の合わせガラス用中間膜が、一対のガラス板の間に積層されている合わせガラスもまた、本発明の1つである。
上記ガラス板は、一般に使用されている透明板ガラスを使用することができる。例えば、フロート板ガラス、磨き板ガラス、型板ガラス、網入りガラス、線入り板ガラス、着色された板ガラス、熱線吸収ガラス、熱線反射ガラス、グリーンガラス等の無機ガラスが挙げられる。また、ガラスの表面に紫外線遮蔽コート層を有する紫外線遮蔽ガラスも用いることができる。更に、ポリエチレンテレフタレート、ポリカーボネート、ポリアクリレート等の有機プラスチックス板を用いることもできる。
上記ガラス板として、2種類以上のガラス板を用いてもよい。例えば、透明フロート板ガラスと、グリーンガラスのような着色されたガラス板との間に、本発明の合わせガラス用中間膜を積層した合わせガラスが挙げられる。また、上記ガラス板として、2種以上の厚さの異なるガラス板を用いてもよい。
The laminated glass in which the interlayer film for laminated glass of the present invention is laminated between a pair of glass plates is also one aspect of the present invention.
The said glass plate can use the transparent plate glass generally used. Examples thereof include inorganic glass such as float plate glass, polished plate glass, template glass, netted glass, wire-containing plate glass, colored plate glass, heat ray absorbing glass, heat ray reflecting glass, and green glass. Further, an ultraviolet shielding glass having an ultraviolet shielding coating layer on the glass surface can also be used. Furthermore, organic plastics plates such as polyethylene terephthalate, polycarbonate, and polyacrylate can also be used.
Two or more types of glass plates may be used as the glass plate. For example, the laminated glass which laminated | stacked the intermediate film for laminated glasses of this invention between transparent float plate glass and colored glass plates like green glass is mentioned. Moreover, you may use the glass plate from which 2 or more types of thickness differs as said glass plate.
本発明によれば、調光体層を有しながら、周辺部に調光体の染み出しがない合わせガラス用中間膜、該合わせガラス用中間膜を用いた合わせガラス、及び、該合わせガラス用中間膜の製造方法を提供できる。 ADVANTAGE OF THE INVENTION According to this invention, it has a light control body layer, the intermediate film for laminated glasses which does not bleed out a light control body in a peripheral part, the laminated glass using this intermediate film for laminated glasses, and this laminated glass use An intermediate film manufacturing method can be provided.
以下に実施例を挙げて本発明の態様を更に詳しく説明するが、本発明はこれら実施例にのみ限定されるものではない。 Hereinafter, embodiments of the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.
(実施例1)
(1)接着層及び透明導電層の調製
ポリビニルブチラール(水酸基の含有率30モル%、アセチル化度1モル%、ブチラール化度69モル%、平均重合度1700)100重量部に対し、可塑剤としてトリエチレングリコールジ−2−エチルヘキサノエート(3GO)40重量部を添加し、ミキシングロールで充分に混練し、樹脂組成物を得た。得られた樹脂組成物を押出機により押出して、ポリビニルブチラール(PVB)からなる厚み380μmの単層の樹脂膜を得た。
次に、厚み40μmのポリエチレンテレフタレートフィルムに、スパッタ法及び蒸着イオンプレーティング法により、スズドープ酸化インジウム(ITO)からなる厚みが10μmの層を形成し、透明導電層を得た。得られた透明導電層と、上記単層の樹脂膜とを、厚み方向に単層の樹脂膜、透明導電層、単層の樹脂膜の順に積層後、80℃で貼り合わせる事で、透明導電層付き接着層を得た。得られた透明導電層付き接着層は、縦300mm、横300mmの大きさに切断した。
Example 1
(1) Preparation of adhesive layer and transparent conductive layer Polyvinyl butyral (
Next, a layer having a thickness of 10 μm made of tin-doped indium oxide (ITO) was formed on a polyethylene terephthalate film having a thickness of 40 μm by sputtering and vapor deposition ion plating to obtain a transparent conductive layer. After laminating the obtained transparent conductive layer and the single layer resin film in the thickness direction in the order of a single layer resin film, a transparent conductive layer and a single layer resin film, the transparent conductive layer is bonded at 80 ° C. A layered adhesive layer was obtained. The obtained adhesive layer with a transparent conductive layer was cut into a size of 300 mm in length and 300 mm in width.
(2)シール剤の塗工
光硬化性樹脂として多官能アクリレート100重量部と、紫外線吸収剤としてベンゾフェノン2重量部とを混合して、光硬化性シール剤を調製した。
得られた光硬化性シール剤を、スクリーン印刷法により、透明導電層付き接着層の透明導電層側の周縁部に線幅が5mmとなるようにして枠状に塗工した。
(2) Coating of sealant 100 parts by weight of a polyfunctional acrylate as a photocurable resin and 2 parts by weight of benzophenone as an ultraviolet absorber were mixed to prepare a photocurable sealant.
The obtained photocurable sealant was applied in a frame shape by screen printing so that the line width of the adhesive layer with a transparent conductive layer on the transparent conductive layer side was 5 mm.
(3)調光体層の形成
調光体として液晶(STN型液晶(DIC社製))を用い、該調光体70重量部に30重量部の割合で高分子架橋体(多官能アクリレートポリマー)を配合したものを、得られた透明導電層付き接着層上のシール剤の枠の内側に塗工して調光体層を形成した。
(3) Formation of a light control layer A liquid crystal (STN type liquid crystal (manufactured by DIC)) is used as a light control body, and a polymer crosslinked body (polyfunctional acrylate polymer) at a ratio of 30 parts by weight to 70 parts by weight of the light control body. ) Was applied to the inside of the sealant frame on the obtained adhesive layer with a transparent conductive layer to form a light control layer.
(4)合わせガラス用中間膜の製造
別に準備した透明導電層付き接着層を、調光体を形成した透明導電層付き接着層の調光体層を透明電極層で挟み込むように重ね合わせて積層体を得た。得られた積層体に、高圧水銀ランプを用いて波長350nm、強度1000mW/cm2の紫外線を10秒間照射してシール剤を硬化させてシール層を形成した。
次いで、シール層が形成された積層体を、40℃の温度をかけながら圧着しラミネートして、合わせガラス用中間膜を得た。なお、ラミネート温度90℃の条件でも、合わせガラス用中間膜を製造した。
(4) Laminate the adhesive layer with a transparent conductive layer prepared for each production of the interlayer film for laminated glass so that the light control layer of the adhesive layer with the transparent conductive layer forming the light control member is sandwiched between the transparent electrode layers. Got the body. The obtained laminate was irradiated with ultraviolet rays having a wavelength of 350 nm and an intensity of 1000 mW / cm 2 for 10 seconds using a high-pressure mercury lamp to cure the sealant to form a seal layer.
Next, the laminate on which the seal layer was formed was pressure-bonded and laminated while applying a temperature of 40 ° C. to obtain an interlayer film for laminated glass. Note that an interlayer film for laminated glass was produced even under the condition of a lamination temperature of 90 ° C.
(実施例2)
調光体として液晶(STN型液晶(DIC社製))を用い、該調光体100重量部に0.001重量部の割合でスペーサ粒子(積水化学工業社製、商品名「ミクロパール」)を配合したものを用いて調光体層を形成した以外は実施例1と同様にして、合わせガラス用中間膜を得た。
(Example 2)
Liquid crystal (STN type liquid crystal (manufactured by DIC)) was used as the light control member, and spacer particles (trade name “Micropearl” manufactured by Sekisui Chemical Co., Ltd.) at a ratio of 0.001 part by weight to 100 parts by weight of the light control member. An interlayer film for laminated glass was obtained in the same manner as in Example 1 except that the light control layer was formed using the blended material.
(実施例3)
PVBからなる単層の樹脂膜に代えて、エチレン−酢酸ビニル共重合体フィルム(積水化学工業社製)を単層の樹脂膜として用いた以外は実施例2と同様にして、合わせガラス用中間膜を得た。
(Example 3)
In the same manner as in Example 2 except that an ethylene-vinyl acetate copolymer film (manufactured by Sekisui Chemical Co., Ltd.) was used as the single-layer resin film instead of the single-layer resin film made of PVB, an intermediate for laminated glass A membrane was obtained.
(比較例1、2)
シール層を形成しなかった以外は実施例1、3と同様にして、合わせガラス用中間膜を得た。
(Comparative Examples 1 and 2)
An interlayer film for laminated glass was obtained in the same manner as in Examples 1 and 3 except that the seal layer was not formed.
(評価)
実施例及び比較例で得られた合わせガラス用中間膜について以下の評価を行った。結果を表1に示した。
(Evaluation)
The following evaluation was performed about the intermediate film for laminated glasses obtained by the Example and the comparative example. The results are shown in Table 1.
(1)調光体の染み出しの評価
得られた合わせガラス用中間膜の周辺部を目視にて観察して、調光体の染み出しが全く認められなかった場合を「○」と、ごく軽微な染み出しが認められた場合を「△」、染み出しが認められた場合を「×」と評価した。
なお、調光体の染み出しの評価は、貼り合わせを40℃、90℃で行った合わせガラス用中間膜について行った。
(1) Evaluation of seepage of light control body The periphery of the obtained interlayer film for laminated glass was visually observed, and a case where no seepage of the light control body was observed was marked with “○”. The case where slight exudation was observed was evaluated as “Δ”, and the case where exudation was observed was evaluated as “x”.
In addition, evaluation of the light control body oozing-out was performed on an interlayer film for laminated glass that was bonded at 40 ° C. and 90 ° C.
(2)調光性の評価
得られた合わせガラス用中間膜に−2Vの電圧を印加し、目視にて観察して、合わせガラス用中間膜の光の透過率の変化が認められた場合を「○」と、認められなかった場合を「×」と評価した。
なお、調光性の評価は、貼り合わせを40℃で行った合わせガラス用中間膜について行った。ただし、調光体の大きな染み出しがあった比較例1、2については、調光性の評価は中止した。
(2) Evaluation of light control property A voltage of -2 V was applied to the obtained interlayer film for laminated glass and observed visually, and a change in light transmittance of the interlayer film for laminated glass was observed. The case where it was not recognized as “O” was evaluated as “X”.
In addition, dimming property evaluation was performed about the intermediate film for laminated glasses which bonded together at 40 degreeC. However, for Comparative Examples 1 and 2 in which there was a large exudation of the dimmer, the evaluation of the dimming property was stopped.
本発明によれば、調光体層を有しながら、周辺部に調光体の染み出しがない合わせガラス用中間膜、該合わせガラス用中間膜を用いた合わせガラス、及び、該合わせガラス用中間膜の製造方法を提供できる。 ADVANTAGE OF THE INVENTION According to this invention, it has a light control body layer, the intermediate film for laminated glasses which does not bleed out a light control body in a peripheral part, the laminated glass using this intermediate film for laminated glasses, and this laminated glass use An intermediate film manufacturing method can be provided.
1 合わせガラス用中間膜
2 接着層
3 調光体層
4 透明導電層
5 シール層
10 合わせガラス用中間膜
20 接着層
30 調光体層
40 透明導電層
50 シール層
DESCRIPTION OF SYMBOLS 1 Intermediate film 2 for laminated
Claims (10)
一方の面に透明導電層を形成した2枚の接着層を作製する工程と、一方の透明導電層を形成した接着層の透明導電層側の周縁部に、光硬化性樹脂を含有するシール剤を枠状に塗工する工程と、前記透明導電層を形成した接着層上のシール剤の枠の内側に調光体を塗工して調光体層を形成する工程と、他方の透明導電層を形成した接着層を、透明導電層が調光体層側になるように重ね合わせた積層体を得る工程と、前記積層体に光を照射してシール剤を硬化させてシール層を形成する工程と、シール層形成後の積層体を30〜100℃の温度をかけながら圧着してラミネートする工程を有する
ことを特徴とする合わせガラス用中間膜の製造方法。 A method for producing an interlayer film for laminated glass according to claim 1, 2, 3, 4, 5, 6 or 7,
A step of producing two adhesive layers having a transparent conductive layer formed on one surface, and a sealant containing a photocurable resin at the peripheral edge of the transparent conductive layer side of the adhesive layer having one transparent conductive layer formed A step of applying a light control body on the inner side of the frame of the sealing agent on the adhesive layer on which the transparent conductive layer is formed, and a step of forming the light control layer. A step of obtaining a laminate in which the adhesive layer on which the layer is formed is overlaid so that the transparent conductive layer is on the light control layer side, and the sealant is cured by irradiating the laminate with light to form a seal layer A method for producing an interlayer film for laminated glass, the method comprising: a step of pressing and laminating the laminate after forming the seal layer while applying a temperature of 30 to 100 ° C.
一方の面に透明導電層を形成した2枚の接着層を作製する工程と、一方の透明導電層を形成した接着層の透明導電層側の周縁部に、熱硬化性樹脂を含有するシール剤を枠状に塗工する工程と、前記透明導電層を形成した接着層上のシール剤の枠の内側に調光体を塗工して調光体層を形成する工程と、他方の透明導電層を形成した接着層を、透明導電層が調光体層側になるように重ね合わせて積層体を得る工程と、前記積層体を加熱してシール剤を硬化させてシール層を形成する工程と、シール層形成後の積層体を30〜100℃の温度をかけながら圧着してラミネートする工程を有する
ことを特徴とする合わせガラス用中間膜の製造方法。 A method for producing an interlayer film for laminated glass according to claim 1, 2, 3, 4, 5, 6 or 7,
A step of producing two adhesive layers having a transparent conductive layer formed on one surface thereof, and a sealing agent containing a thermosetting resin at the peripheral portion on the transparent conductive layer side of the adhesive layer having one transparent conductive layer formed A step of applying a light control body on the inner side of the frame of the sealing agent on the adhesive layer on which the transparent conductive layer is formed, and a step of forming the light control layer. A step of superimposing the adhesive layer on which the layers are formed so that the transparent conductive layer is on the light control layer side to obtain a laminate, and a step of heating the laminate to cure the sealing agent to form a seal layer And a method for producing an interlayer film for laminated glass, comprising: a step of pressing and laminating the laminate after forming the seal layer while applying a temperature of 30 to 100 ° C.
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