JP5505884B2 - 特定の屈折率を有するシリカを含む合わせガラス用中間膜 - Google Patents
特定の屈折率を有するシリカを含む合わせガラス用中間膜 Download PDFInfo
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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
- B32B17/10761—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
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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
- B32B17/10688—Adjustment of the adherence to the glass layers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0016—Plasticisers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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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
- B32B2264/00—Composition or properties of particles which form a particulate layer or are present as additives
- B32B2264/10—Inorganic particles
- B32B2264/102—Oxide or hydroxide
- B32B2264/1021—Silica
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/25—Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
- Y10T428/259—Silicic material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31627—Next to aldehyde or ketone condensation product
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31551—Of polyamidoester [polyurethane, polyisocyanate, polycarbamate, etc.]
- Y10T428/31627—Next to aldehyde or ketone condensation product
- Y10T428/3163—Next to acetal of polymerized unsaturated alcohol [e.g., formal butyral, etc.]
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31855—Of addition polymer from unsaturated monomers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31942—Of aldehyde or ketone condensation product
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/31504—Composite [nonstructural laminate]
- Y10T428/31942—Of aldehyde or ketone condensation product
- Y10T428/31946—Next to second aldehyde or ketone condensation product
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Joining Of Glass To Other Materials (AREA)
- Laminated Bodies (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Description
R1−O(−R2−O)n−CO−R5 I
R1−O(−R2−O)n−CO−R3−CO−(O−R4−)m−O−R6 II
R3:直接結合、2価の炭素数1〜12の脂肪族又は芳香族残基、
R2、R4:独立してH、炭素数1〜12の脂肪族又は芳香族残基、
n、m:独立して1〜10の整数であり、好ましくは1〜5である。
(a)上記中間膜の伸度50%及び/または100%における引張応力が、フュームドシリカ(C)を含まない同一組成物の中間膜の少なくとも1.2倍であり、かつ、
(b)上記中間膜のガラス転移温度Tgaと、フュームドシリカ(C)を含まない同一組成物の中間膜のガラス転移温度Tgbの差が3℃以内(|Tga−Tgb|≦3)
である合わせガラス用中間膜が好ましい。
エチルアルコール/THF(80:20)の混合物100mL中に、PVB膜3〜4gをマグネチックスターラーで終夜溶解させた。希釈塩酸(c=0.01mol/L)10mLを添加した。タイトロプロセッサー(例えば、メトローム社製など)を用いて、過剰の塩酸を2−プロパノールの水酸化テトラブチルアンモニウム溶液(TBAH、c=0.01mol/L)で、ブランクサンプルに対して電位差滴定する。アルカリ滴定量は、次のように計算される。
サンプル100gあたりのml(0.01モル/L HCl)=(ml TBAHblank−ml TBAHsample)×100/g(サンプル重量)
引張特性は、DIN EN ISO 527−1及びDIN EN ISO 527−3に従って、寸法15mm×120mmの短冊状試験片を伸長速度200mm/minで測定した。
膜の黄色度Δbインデックスは、可視光の光度計Hunterlab“Colorquest XE”において、リファレンスの対ガラスに対して2層の2mmのフロートガラスの間にフィルムを積層したものをL、a、b−システムで測定することで決定された;b値(積層物)―b値(対ガラス)=Δb。
膜のヘイズは、積層された状態で、すなわち、ヘイズのない透明な2mmのフロートガラスの間に積層された状態で、Hunterlab“Colorquest XE”において、20℃でASTM 1003に従って決定された。
フュームドシリカを、105℃のオーブン中で2時間乾燥させる。乾燥させたフュームドシリカを適切な無極性溶媒中に2%含有する懸濁液が、密封されたバイアル瓶に満たされ、80℃で4時間保持される。その間、良好な均質性を得るために、バイアル瓶は時々攪拌される。この懸濁液は、光学測定用のキュベットへ移され、550nmにおける光透過率をサンプル温度の関数として記録する。光透過率がその最大値(最小のヘイズ)をとるときの温度が得られ、デジタル屈折計(例えばKernchen GmbHのABBEMAT−WRなど)において同じ温度で測定される溶媒のみの屈折率が、フュームドシリカの屈折率と等しいとする。適切な溶媒は、例えば、リモネンや、パラチノール10−P、3G8又はその他のような可塑剤であり、予想されるフュームドシリカの屈折率に従い選択される。
高精度自動屈折計としては、例えばKernchen GmbHの“ABBEMAT−WR”などを用いて、平らな表面を有する円状のPVBフィルムのサンプルを高精度自動屈折計のサンプル用モールド中で、20℃にて測定する。
ガラス転移温度は、フィルムサンプルの、1Hz、振幅0.05%、加熱レート2K/minで測定する、動的熱機械分析(DMTA)により求められる損失係数(tanδ)曲線の極大値から求められる。
本発明の実施例と比較例のPVBフィルムはそれぞれ同条件にて作成し、溶融温度約200℃で押出し法によって、スリットダイから溶融した混合物を押し出した。PVBポリマーと任意に選択されるフュームドシリカは同時にホッパーに供給し、一方、溶解状態のUV吸収化合物を含んだ可塑剤は、別途液体成分として添加される。塩基性化合物は、水溶液として、別の注入口から押出し機へ供給された。膜厚は実施例及び比較例のすべてにおいて0.76mmであった。
実施例W5又は比較例C10の多層膜の作成は、厚さ0.38mmの膜1層(中心層)を、比較例C1の厚さ0.20mmの2層で挟み込んで作成した。完成した多層膜は厚さ0.78mmであり、その光学及び力学的特性を単層膜と同様の方法で評価した。
シリカ:pH3.8で1.1%のA1203を含有するデグザの商用グレード アエロジル(登録商標)MOX170がフュームドシリカを含有するフィルムの作成に用いられる。付加的な無機酸化物を含まないpH4.1であるデグザ商用グレード アエロジル(登録商標)130、付加的な無機酸化物を含まないpH4.1であるキャボットの商用グレードCAB−O−SIL(登録商標)M5及び付加的な無機酸化物を含まないpH7.0であるTOSO−Silicaの商用グレードNIPGEL(登録商標)AY−200が比較のために使用される。
クラレヨーロッパ GmbH製
可塑剤: DBEA (ジ−(2−ブトキシエチル)−アジペート)
3G8 (トリエチレングリコール−ジ−2−エチルヘキサノエート)
塩基性化合物: 酢酸カリウム及び酢酸マグネシウム
下記の表2〜4に示すように、本発明の中間膜は、改善された引張強度と許容される範囲のヘイズ値及び黄色度を示した。
Claims (11)
- ポリビニルアセタール(A)、少なくとも1種の可塑剤(B)、フュームドシリカ(C)及び少なくとも1種の塩基性化合物(D)を含み、フュームドシリカ(C)と可塑化ポリビニルアセタール(A+B)の屈折率の差が0.015以下であり、重量比C/(A+B)が2.7/100〜60/100である合わせガラスに有用な中間膜。
- 塩基性化合物(D)が、炭素数1〜15の有機カルボン酸の金属塩である請求項1記載の中間膜。
- ASTM D 1003に準じた0.76mm厚の上記中間膜のヘイズ値が2.0%以下である請求項1または2に記載の中間膜。
- 上記中間膜のアルカリ滴定量が3mlを超える請求項1〜3のいずれかに記載の中間膜。
但し、前記アルカリ滴定量(ml)は、中間膜100gあたりのアルカリ滴定に要する濃度0.01mol/Lの塩酸の量(ml)であり、下記測定方法により求められる。
エチルアルコール/THF(80:20)の混合物100mL中に、中間膜(sample)3〜4gを溶解させた後、濃度0.01mol/Lの塩酸10mLを添加し、
タイトロプロセッサーを用いて、過剰の塩酸を2−プロパノールの水酸化テトラブチルアンモニウム溶液(TBAH、濃度0.01mol/L)で、ブランクサンプル(blank)に対して電位差滴定し、
中間膜100gあたりのアルカリ滴定量(ml)を次のように計算する。
アルカリ滴定量(ml)=
[TBAH blank (ml)−TBAH sample (ml)]×100(g)/sample(g)
式中、TBAH blank は、ブランクサンプルを電位差滴定したときの水酸化テトラブチルアンモニウム溶液の滴定量(ml)であり、TBAH sample は、中間膜を電位差滴定したときの水酸化テトラブチルアンモニウム溶液の滴定量(ml)である。 - Al2O3、TiO2,MgO及びZrO2からなる群より選択される少なくとも1種によってフュームドシリカ(C)がドープされる請求項1〜4のいずれかに記載の中間膜。
- 上記中間膜の伸度50%及び/または100%における引張応力が、フュームドシリカ(C)を含まない同一組成物の中間膜の少なくとも1.2倍である請求項1〜5のいずれかに記載の中間膜。
- 上記中間膜のガラス転移温度Tgaと、フュームドシリカ(C)を含まない同一組成物の中間膜のガラス転移温度Tgbの差が3℃以内(|Tga−Tgb|≦3)である請求項1〜6のいずれかに記載の中間膜。
- a)上記中間膜の伸度50%及び/または100%における引張応力が、フュームドシリカ(C)を含まない同一組成物の中間膜の少なくとも1.2倍であり、かつ、
b)上記中間膜のガラス転移温度Tgaと、フュームドシリカ(C)を含まない同一組成物の中間膜のガラス転移温度Tgbの差が3℃以内(|Tga−Tgb|≦3)
である請求項1〜7のいずれかに記載の中間膜。 - ポリビニルアセタール(A’)及び少なくとも1種の可塑剤(B’)を含む少なくとも1つの層または膜と、ポリビニルアセタール(A)、少なくとも1種の可塑剤(B)、フュームドシリカ(C)及び少なくとも1種の塩基性化合物(D)を含む少なくとも1つの層または膜とからなり、フュームドシリカ(C)と可塑化ポリビニルアセタール(A+B)の屈折率の差が0.015以下であり、重量比C/(A+B)が2.7/100〜60/100である合わせガラスに有用な多層膜。
- ポリビニルアセタール(A)、少なくとも1種の可塑剤(B)、フュームドシリカ(C)及び少なくとも1種の塩基性化合物(D)を含み、フュームドシリカ(C)と可塑化ポリビニルアセタール(A+B)の屈折率の差が0.015以下であり、重量比C/(A+B)が2.7/100〜60/100である少なくとも1つの層または膜が、ポリビニルアセタール(A’)及び少なくとも1種の可塑剤(B’)を含む少なくとも2つの膜に挟まれてなる請求項9記載の多層膜。
- 合わせガラスにおける請求項1〜8のいずれかに記載の中間膜または請求項9または10に記載の多層膜としての使用。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP20070105692 EP1977885A1 (en) | 2007-04-05 | 2007-04-05 | Interlayer films for laminated glazing containing silica with specific refractive index |
EP07105692.3 | 2007-04-05 | ||
PCT/EP2008/054094 WO2008122608A1 (en) | 2007-04-05 | 2008-04-04 | Interlayer films for laminated glazing containing silica with specific refractive index |
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JP2010523449A JP2010523449A (ja) | 2010-07-15 |
JP5505884B2 true JP5505884B2 (ja) | 2014-05-28 |
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JP2010501524A Active JP5505884B2 (ja) | 2007-04-05 | 2008-04-04 | 特定の屈折率を有するシリカを含む合わせガラス用中間膜 |
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US (1) | US8039112B2 (ja) |
EP (2) | EP1977885A1 (ja) |
JP (1) | JP5505884B2 (ja) |
CN (1) | CN101678649B (ja) |
WO (1) | WO2008122608A1 (ja) |
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EP2028224A1 (de) * | 2007-07-30 | 2009-02-25 | Nanoresins AG | Weichmacherzusammensetzung |
US8551621B2 (en) * | 2008-09-30 | 2013-10-08 | Sekisui Chemical Co., Ltd. | Interlayer for laminated glass and laminated glass |
US9238354B2 (en) * | 2009-12-25 | 2016-01-19 | Sekisui Chemical Co., Ltd. | Intermediate film for laminated glass, multilayer intermediate film for laminated glass, and laminated glass |
US8790784B2 (en) | 2010-07-16 | 2014-07-29 | Sekisui Chemical Co., Ltd. | Intermediate film for laminated glass and laminated glass |
US10384423B2 (en) * | 2012-06-11 | 2019-08-20 | Sumitomo Metal Mining Co., Ltd. | Heat shielding lamination structure |
US9254625B2 (en) | 2013-06-10 | 2016-02-09 | Solutia Inc. | Polymer interlayers having improved optical properties |
EP2813543B1 (de) * | 2013-06-14 | 2018-10-24 | Kuraray Europe GmbH | PVB-Folie mit UV-Schutz und geringem Gelbwert für Verbundsicherheitsglas |
WO2015040663A1 (ja) * | 2013-09-17 | 2015-03-26 | 株式会社クラレ | ポリビニルアセタールを含有するシート |
KR102307080B1 (ko) | 2014-02-25 | 2021-10-01 | 세키스이가가쿠 고교가부시키가이샤 | 접합 유리용 중간막, 접합 유리용 중간막의 제조 방법 및 접합 유리 |
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-
2007
- 2007-04-05 EP EP20070105692 patent/EP1977885A1/en not_active Withdrawn
-
2008
- 2008-04-04 EP EP20080735835 patent/EP2144753A1/en not_active Withdrawn
- 2008-04-04 WO PCT/EP2008/054094 patent/WO2008122608A1/en active Application Filing
- 2008-04-04 CN CN2008800111844A patent/CN101678649B/zh not_active Expired - Fee Related
- 2008-04-04 US US12/594,737 patent/US8039112B2/en not_active Expired - Fee Related
- 2008-04-04 JP JP2010501524A patent/JP5505884B2/ja active Active
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EP1977885A1 (en) | 2008-10-08 |
EP2144753A1 (en) | 2010-01-20 |
CN101678649B (zh) | 2013-10-30 |
US20100124647A1 (en) | 2010-05-20 |
WO2008122608A1 (en) | 2008-10-16 |
CN101678649A (zh) | 2010-03-24 |
US8039112B2 (en) | 2011-10-18 |
JP2010523449A (ja) | 2010-07-15 |
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