JP5568115B2 - 遮熱合わせガラス用中間膜の改質方法 - Google Patents
遮熱合わせガラス用中間膜の改質方法 Download PDFInfo
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- JP5568115B2 JP5568115B2 JP2012186760A JP2012186760A JP5568115B2 JP 5568115 B2 JP5568115 B2 JP 5568115B2 JP 2012186760 A JP2012186760 A JP 2012186760A JP 2012186760 A JP2012186760 A JP 2012186760A JP 5568115 B2 JP5568115 B2 JP 5568115B2
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- Prior art keywords
- heat
- laminated glass
- fine particles
- interlayer film
- shielding
- 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.)
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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 claims description 11
- 229920002554 vinyl polymer Polymers 0.000 claims description 11
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- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 4
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- UBMUZYGBAGFCDF-UHFFFAOYSA-N trimethoxy(2-phenylethyl)silane Chemical compound CO[Si](OC)(OC)CCC1=CC=CC=C1 UBMUZYGBAGFCDF-UHFFFAOYSA-N 0.000 description 1
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- XQEGZYAXBCFSBS-UHFFFAOYSA-N trimethoxy-(4-methylphenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=C(C)C=C1 XQEGZYAXBCFSBS-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical compound C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 description 1
- OXFUXNFMHFCELM-UHFFFAOYSA-N tripropan-2-yl phosphate Chemical compound CC(C)OP(=O)(OC(C)C)OC(C)C OXFUXNFMHFCELM-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
-
- 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
- B32B17/10009—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 number, the constitution or treatment of glass sheets
- B32B17/10036—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 number, the constitution or treatment of glass sheets comprising two outer glass sheets
-
- 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
- B60—VEHICLES IN GENERAL
- B60J—WINDOWS, WINDSCREENS, NON-FIXED ROOFS, DOORS, OR SIMILAR DEVICES FOR VEHICLES; REMOVABLE EXTERNAL PROTECTIVE COVERINGS SPECIALLY ADAPTED FOR VEHICLES
- B60J1/00—Windows; Windscreens; Accessories therefor
-
- 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
-
- 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
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
- Y10T428/2991—Coated
-
- 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.]
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Joining Of Glass To Other Materials (AREA)
- Laminated Bodies (AREA)
- Treatments Of Macromolecular Shaped Articles (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
以下に本発明を詳述する。
これにより、中間膜樹脂の劣化に伴う合わせガラスの黄変化を生じることなく、可視光に対する高い透明性と、優れた遮熱性能を同時に有する合わせガラス用中間膜を得ることができる。
中間膜の状態で高エネルギー線を照射する場合、湿気や熱による樹脂の劣化や状態変化を防ぐために、例えば、ポリエチレンテレフタレートフィルムを中間膜に圧着させ水分との接触を防ぐ、また、熱変形を防ぐためには、高強度にて短時間照射するのではなく、低強度にて長時間照射する等、充分な注意が必要である。
また、合わせガラスにした状態で高エネルギー線を照射する場合、シェードガラスやグリーンガラスを用いた場合には高エネルギー線の透過を妨げ、充分なエネルギーを遮熱性微粒子に与えられない場合があるため、衝撃強度を保持した状態で、高エネルギー線の全てが吸収されない程度に薄いものを用いる、若しくは中間膜の状態で高エネルギー線を照射した後に合わせガラスを作製すればよい。
なお、上記イエローインデックス値(YI)、及び、上記CIE1976L*a*b*表示系におけるb*値は、可視光透過率の測定における測定データから求めることができる。また、イエローインデックス値変化(ΔYI)、及び、b*値変化(Δb*)とは、下記式(1)及び(2)で示される、高エネルギー線照射後の値から、高エネルギー線照射前の値を減ずることにより求まる値とする。
ΔYI=YI(高エネルギー線照射後)−YI(高エネルギー線照射前) (1)
Δb*=b*(高エネルギー線照射後)−b*(高エネルギー線照射前) (2)
上記原料となるポリビニルアルコールは、通常、ポリ酢酸ビニルをケン化することにより得られる、ケン化度80〜99.8モル%のポリビニルアルコールが一般的に用いられる。
また、上記ポリビニルアルコールの重合度の好ましい下限は200、好ましい上限は3000である。200未満であると、得られる合わせガラスの耐貫通性が低下することがあり、3000を超えると、樹脂膜の成形性が悪くなり、また、樹脂膜の剛性が大きくなり過ぎ、加工性が悪くなることがある。より好ましい下限は500、より好ましい上限は2000である。
上記一塩基性有機酸エステル系可塑剤としては、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系エステルが挙げられる。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のトリエチレングリコール等が好適である。
上記有機リン酸系可塑剤としては、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。
上記接着力調整剤としては特に限定されないが、アルカリ金属塩及び/又はアルカリ土類金属塩が好適に用いられる。上記アルカリ金属塩及び/又はアルカリ土類金属塩としては特に限定されず、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特に限定されず、例えば、オクチル酸、ヘキシル酸、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。
上記紫外線吸収剤としては、Propanedioc acid,[(4−methoxyphenyl)−methylene]−dimethyl ester(Clariant社製:Hostavin・PR−25)等のマロン酸エステル系紫外線吸収剤、及び/又は、2−Ethyl,2’−ethoxy−oxalanilide(Clariant社製:Sanduvor・VSU)等のシュウ酸アニリド系紫外線吸収剤が好適である。
上記ベンゾトリアゾール系紫外線吸収剤としては、例えば、2−(2’−ヒドロキシ−5’−メチルフェニル)ベンゾトリアール(Tinuvin P、チバガイギー社製)、2−(2’−ヒドロキシ−3’,5’−ジ−t−ブチルフェニル)ベンゾトリアゾール(Tinuvin 320、チバガイギー社製)、2−(2’−ヒドロキシ−3’−t−ブチル−5’−メチルフェニル)−5−クロロベンゾトリアール(Tinuvin 326、チバガイギー社製)、2−(2’−ヒドロキシ−3’,5’−ジ−アミルフェニル)ベンゾトリアゾール(Tinuvin 328、チバガイギー社製)等や、LA−57(アデカアーガス社製)等のヒンダードアミン系のものが挙げられる。
上記ベンゾフェノン系紫外線吸収剤としては、例えば、オクタベンゾン(Chimassorb81、チバガイギー社製)等が挙げられる。
上記トリアジン系紫外線吸収剤としては、例えば、2−(4,6−ジフェニル−1,3,5−トリアジン−2−イル)−5−(ヘキシル)オキシトフェノール(Tinuvin 1577FF、チバガイギー社製)等が挙げられる。
上記ベンゾエート系としては、例えば、2,4−ジ−tert−ブチルフェニル−3,5−ジ−tert−ブチル−4−ヒドロキシベンゾエート(Tinuvin 120、チバガイギー社製)等が挙げられる。
上記変性シリコーンオイルは、単独で使用してもよく、2種以上を併用してもよい。
上記変性シリコーンオイルの分子量の好ましい下限は800、好ましい上限は5000である。800未満であると、表面への局在化が低下することがあり、5000を超えると、樹脂との相溶性が不良となり、得られる合わせガラス用中間膜の表面にブリードアウトしてガラスとの接着力が低下することがある。より好ましい下限は1500、より好ましい上限は4000である。
本発明の遮熱合わせガラス用中間膜の改質方法により得られる遮熱合わせガラス用中間膜(以下、改質中間膜ともいう)もまた、本発明の1つである。
可視光透過率変化(ΔTv)=Tv(高エネルギー線照射後)
−Tv(高エネルギー線照射前) (3)
これにより、可視光領域においては高い透明性が得られ、更に、熱的作用の原因となる赤外線、特に、皮膚への吸収が高くなる波長領域が上記範囲にあることで、皮膚温度の上昇を抑えることができる。
赤外線透過率変化(ΔTir)=Tir(高エネルギー線照射後)
−Tir(高エネルギー線照射前) (4)
上記改質中間膜を用いてなる合わせガラスもまた、本発明の1つである。
(1)遮熱性微粒子の表面処理
脱水処理したエタノール(ナカライテスク社製)に、不活性物質としてテトラエトキシシラン(信越シリコーン社製、KBE04)を2重量%となるように溶解させ、あらかじめ100℃にて1時間熱処理したITO粉末(三井金属社製)を20重量%となるように懸濁させた溶液を調製した。得られた調製溶液をビーズミルを用いて充分に撹拌することにより、ITO微粒子の表面に酸化ケイ素を被覆すると同時に微粉砕化した。続いて分散液中の粒子を遠心分離機により回収した。その後回収した粒子を150℃で熱処理することにより、酸化ケイ素で表面が処理されたITO微粒子を得た。
2−[5−クロロ(2H)−ベンゾトリアゾール−2−イル]−4−メチル−6−(tert−ブチル)フェノール(チバ・スペシャルティ・ケミカルズ社製 TINUVIN326)、高分子フェノール系酸化防止剤(チバガイギー社製、イルガノックス 1010)、2−エチルヘキサン酸(ナカライテスク社製)を溶解させたトリエチレングリコールビス(2−エチルヘキサノエート)(協和発酵工業社製 3GO)に対して、酸化ケイ素により表面処理されたITO微粒子をポリオキシアルキレンアルキルフェニルエーテルリン酸エステル(第一工業社製、プライサーフA210G)を溶解させたエタノール(ナカライテスク社製)を分散液として、ペイントシェーカーを用いて分散させることにより、ITO微粒子含有可塑剤溶液を得た。
得られたITO微粒子含有可塑剤溶液をプラスト機にてポリビニルブチラール樹脂(積水化学工業社製 エスレック BH−8)と混練し、押出機により金型よりシート状に押し出して、厚さ760μmの合わせガラス用中間膜を得た。それぞれの成分の仕込み組成は表1に示す通りである。
得られたITO微粒子含有中間膜を、その両端から透明なフロートガラス(縦30cm×横30cm×厚さ2.5mm)で挟み込み、これをゴムバック内に入れ、20torrの真空度で20分間脱気した後、脱気したままオーブンに移し、更に90℃で30分間保持しつつ真空プレスした。このようにして予備圧着された合わせガラスをオートクレーブ中で135℃、圧力12kg/cm2の条件で20分間圧着を行い、合わせガラスを得た。
(5)高エネルギー線の照射
得られた合わせガラスに、高エネルギー線としてスーパーUV光、及び、スーパーXe光を以下に示す条件にて照射し、未照射のものと比較を行った。
5cm×10cmの照射サンプルを作製し、以下の条件で本発明の方法の実施を行った。
試験装置 :アイスーパーUVテスター(岩崎電気社製、SUV−F11型)
UV強度 :100mW/cm2
限定波長 :295〜450nm
ブラックパネル温度:63℃
装置内相対温度 :50%
照射距離 :235mm
照射時間 :300時間
5cm×10cmの照射サンプルを作製し、以下の条件で本発明の方法の実施を行った。
試験装置 :SuperXenonWeatherMeter S×2−75(スガ試験機株式会社製)
UV強度 :180W/m2
ブラックパネル温度:63℃
装置内相対温度 :50%
照射時間 :300時間
不活性物質として、テトラエトキシシランの代わりに、テトラノルマルブトキシジルコニウム(松本製薬工業社製、オルガチックスZA60)を用いた以外は実験例1と同様の方法により、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
不活性物質として、テトラエトキシシランの代わりに、アルミニウムsec−ブチレート(川研ファインケミカル社製、ASBN)を用いた以外は実験例1と同様の方法により、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
めのう乳鉢にて2時間粉砕することにより表面をアモルファス化したITO微粒子を得た。次に、実験例1と同様の方法により、ITO微粒子含有可塑剤溶液を作製し、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
リン酸の5%水溶液にてITO粉末(三井金属社製)を超音波照射しながら、懸濁・撹拌させ、続いて回収した粉末を100℃にて乾燥させることにより、リン酸の吸着したITO粉末を得た。これを更にモリブデン酸アンモニウムの5%硝酸酸性水溶液にて超音波照射しながら、懸濁・撹拌させ、続いて回収した粉末を100℃にて乾燥させることにより、リンモリブデン酸アンモニウムで被覆されたITO粉末を得た。次に、実験例1と同様の方法により、ITO微粒子含有可塑剤溶液を作製し、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
リン酸の5%水溶液にてITO粉末を超音波照射しながら、懸濁・撹拌させ、続いて回収した粉末を100℃にて乾燥させることにより、リン酸の吸着したITO粉末を得た。これを更に蒸留水、塩化ナトリウム、炭酸水素ナトリウム、塩化カリウム、リン酸−水素カリウム、塩化マグネシウム、塩化カルシウム、硫酸ナトリウム、トリスヒドロキシメチルアミノメタンにより、Na+=142mM、K+=5mM、Mg2+=1.5mM、Ca2+=2.5mM、Cl−=148.8mM、HPO4 2−=1.0mM、SO4 2−=0.5mM、となるように調整したリン酸水溶液にて、ジェットミルを用いて表面処理及び微粉砕化させた。続いて回収した粉末を100℃にて乾燥させることにより水酸アパタイトで表面が被覆されたITO粉末を得た。次に、実験例1と同様の方法により、ITO微粒子含有可塑剤溶液を作製し、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
不活性物質として、テトラエトキシシランの代わりに、3−メタクリロキシプロピルトリメトキシシラン(信越シリコーン社製、KBM503)を用いた以外は実験例1と同様の方法により、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
不活性物質として、テトラエトキシシランの代わりに、2−(3,4エポキシシクロヘキシル)エチルトリメトキシシラン(信越シリコーン社製、KBM303)を用いた以外は実験例1と同様の方法により、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
不活性物質として、テトラエトキシシランの代わりに、フェニルメトキシシラン(信越シリコーン社製、KBM103)を用いた以外は実験例1と同様の方法により、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
表面を不活性物質にて保護していないITO微粒子を用いた以外は実験例1と同様の方法により、ITO微粒子含有可塑剤溶液を作製し、合わせガラス用中間膜及び合わせガラスを作製し、高エネルギー線を照射した。
実験例1〜9及び参考例1で作製した合わせガラスについて以下の方法により評価した。結果を表1〜3に示した。
中間膜の超薄片作成後、以下の透過型電子顕微鏡(TEM)を使用して、以下の測定条件でITO微粒子の分散状態を撮影、観察した。なお、撮影は3μm×4μmの範囲を×20000倍で撮影し、写真の焼付けで3倍に引き伸ばした。
ITO微粒子の粒子径は、上記撮影により得られた写真中の微粒子の最も長い径とした。また、上記撮影範囲3μm×4μm中の全微粒子の粒子径を測定し、体積換算平均により、平均粒子径を求めた。
観察装置 :透過型電子顕微鏡(日立製作所株式会社製 H−7100FA型)
加速電圧 :100kV
切片作製装置:ウルトラミクロトーム(ライカ株式会社製 EM−ULTRACUT・S)
:REICHERT−NISSEI−FCS(凍結切削システムライカ株式会社製 FC−S型)
ナイフ :DIATOME ULTRA CRYO DRY(DIATOME株式会社製)
直記分光光度計(島津製作所社製、U−4000)を使用して、JIS Z 8722及びJIS R 3106に準拠して、380〜780nmの波長領域での可視光透過率Tv、300〜2500nmの日射透過率Ts、イエローインデックス値、及び、CIE1976L*a*b*表示系におけるb*を求めた。
波長領域780〜2100nmの近赤外線領域の赤外線透過率TirをJIS Z 8722及びJIS R 3106記載の重量係数を用い、規格化することにより求めた。得られたTirの大小により、合わせガラスの遮熱性能を評価した。
高エネルギー線照射後の合わせガラスのヘイズ値(曇り価)をJIS K 6714(1995)「航空機用メタクリル樹脂板」に準拠して測定した。
上記イエローインテックス値、及び、上記CIE1976L*a*b*表示系におけるb*値は、可視光透過率の測定における測定データから求め、その変化値から耐候性、及び、耐光性を評価した。
Claims (11)
- 不活性物質により被覆された遮熱性微粒子、マトリックス樹脂、及び、液状可塑剤を含有する遮熱合わせガラス用中間膜に対して、3.0eV以上のエネルギーを有する電磁波を含む高エネルギー線を照射することにより、波長380〜780nmの可視光透過率を向上させると同時に、波長780〜2100nmの近赤外線透過率を低下させる遮熱合わせガラス用中間膜の改質方法であって、
前記遮熱性微粒子の表面をアモルファス(非晶質)金属酸化物で保護することにより遮熱性微粒子の表面を不活性化する
ことを特徴とする遮熱合わせガラス用中間膜の改質方法。 - 高エネルギー線は、スーパーUV光、UV線、可視光線、スーパーXe光、Xe光、レーザー光、電子線及びマイクロ波からなる群より選択される少なくとも1種であることを特徴とする請求項1記載の遮熱合わせガラス用中間膜の改質方法。
- 高エネルギー線は、波長300〜450nmの光を含むことを特徴とする請求項1又は2記載の遮熱合わせガラス用中間膜の改質方法。
- 高エネルギー線の照射の前後において、下記式(1)で示される遮熱合わせガラス用中間膜のイエローインデックス値変化(ΔYI)が0%以下であり、かつ、下記式(2)で示されるCIE1976L*a*b*表示系におけるb*値変化(Δb*)が0%以下である範囲で高エネルギー線を照射することを特徴とする請求項1、2又は3記載の遮熱合わせガラス用中間膜の改質方法。
ΔYI=YI(高エネルギー線照射後)−YI(高エネルギー線照射前) (1)
Δb*=b*(高エネルギー線照射後)−b*(高エネルギー線照射前) (2) - アモルファス金属酸化物はアモルファス酸化インジウム、アモルファス酸化錫、アモルファス酸化アンチモン、アモルファス錫ドープ酸化インジウム、アモルファス酸化アンチモンドープ酸化錫、アモルファス酸化ケイ素、アモルファス酸化アルミニウム、アモルファス酸化ジルコニウム、アモルファス酸化カルシウム、アモルファス酸化チタン、アモルファス酸化亜鉛、及び、アモルファス酸化セリウムからなる群より選択される少なくとも1種であることを特徴とする請求項1、2、3又は4記載の遮熱合わせガラス用中間膜の改質方法。
- 遮熱合わせガラス用中間膜は、平均粒子径が100nm以下である表面を保護された錫ドープ酸化インジウム(ITO)微粒子を、マトリックス樹脂100重量部に対して、3.0重量部以下含有することを特徴とする請求項1、2、3、4又は5記載の遮熱合わせガラス用中間膜の改質方法。
- 遮熱性微粒子は、錫ドープ酸化インジウム(ITO)微粒子、アンチモンドープ酸化錫(ATO)微粒子、アルミニウムドープ酸化亜鉛微粒子、インジウムドープ酸化亜鉛微粒子、ガリウムドープ酸化亜鉛微粒子、6ホウ化ランタン微粒子及び6ホウ化セリウム微粒子からなる群より選択される少なくとも1種であることを特徴とする請求項1、2、3、4、5又は6記載の遮熱合わせガラス用中間膜の改質方法。
- マトリックス樹脂は、ポリビニルアセタール樹脂であることを特徴とする請求項1、2、3、4、5、6又は7記載の遮熱合わせガラス用中間膜の改質方法。
- 液状可塑剤は、ジヘキシルアジペート、トリエチレングリコール−ジ−2−エチルヘキサノエート、テトラエチレングリコール−ジ−2−エチルヘキサノエート、テトラエチレングリコール−ジ−2−エチルブチレート、テトラエチレングリコール−ジ−2−ヘプタノエート、及び、トリエチレングリコール−ジ−ヘプタエートからなる群より選択される少なくとも1種であることを特徴とする請求項1、2、3、4、5、6、7又は8記載の遮熱合わせガラス用中間膜の改質方法。
- 請求項1、2、3、4、5、6、7、8又は9記載の遮熱合わせガラス用中間膜の改質方法により改質された遮熱合わせガラス用中間膜であって、
不活性物質により被覆された遮熱性微粒子、マトリックス樹脂、及び、液状可塑剤を含有し、波長380〜780nmの可視光透過率が70%以上、かつ、波長300〜2100nmにおける日射透過率が85%以下、かつ、ヘイズ値が1.0%以下である
ことを特徴とする遮熱合わせガラス用中間膜。 - 請求項10記載の遮熱合わせガラス用中間膜を用いてなることを特徴とする合わせガラス。
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WO1999033566A1 (fr) * | 1997-12-25 | 1999-07-08 | Japan As Represented By Director General Of The Agency Of Industrial Science And Technology | Poudre photocatalysante pour la purification de l'environnement, composition polymere contenant ladite poudre et article moule la comprenant, et leurs procedes de production |
JP2000016841A (ja) | 1998-07-03 | 2000-01-18 | Nippon Shokubai Co Ltd | 合わせガラスおよびこれに使用する中間膜 |
JP2000154046A (ja) * | 1998-11-16 | 2000-06-06 | Nippon Shokubai Co Ltd | 合わせガラスおよびこれに用いる樹脂中間層 |
JP2000264632A (ja) | 1999-03-15 | 2000-09-26 | Kanagawa Prefecture | 紫外線遮蔽能を有する透明性金属酸化物超微粒子 |
EP1227070B1 (en) | 1999-10-01 | 2011-04-06 | Sekisui Chemical Co., Ltd. | Intermediate film for laminated glass |
JP2001240769A (ja) | 2000-02-25 | 2001-09-04 | Nippon Shokubai Co Ltd | 表面改質された無機系微粒子およびその用途と無機系微粒子の表面改質方法 |
JP2002326846A (ja) * | 2001-04-27 | 2002-11-12 | Sekisui Chem Co Ltd | 合わせガラス用中間膜及び合わせガラス |
AU2002356116B2 (en) * | 2001-07-26 | 2007-05-17 | Sekisui Chemical Co., Ltd. | Laminated glass-use intermediate film and laminated glass |
JP2003261361A (ja) * | 2002-03-11 | 2003-09-16 | Sekisui Chem Co Ltd | 合わせガラス用中間膜及び合わせガラス |
JP4512940B2 (ja) * | 2003-12-24 | 2010-07-28 | 三菱マテリアル株式会社 | 錫ドープ酸化インジウム微粒子分散液とその製造方法、および該分散液を用いた熱線遮蔽性を有する合わせガラス用中間膜、ならびにその合わせガラス |
WO2005118503A1 (ja) * | 2004-06-01 | 2005-12-15 | Sekisui Chemical Co., Ltd. | 合わせガラス用中間膜及び合わせガラス |
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Also Published As
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CA2574493A1 (en) | 2006-02-09 |
EP1795508A1 (en) | 2007-06-13 |
AU2005268127A1 (en) | 2006-02-09 |
US7754337B2 (en) | 2010-07-13 |
CN1989081A (zh) | 2007-06-27 |
EP1795508A4 (en) | 2009-11-25 |
WO2006013944A1 (ja) | 2006-02-09 |
CN1989081B (zh) | 2010-12-15 |
KR20070041769A (ko) | 2007-04-19 |
RU2382002C2 (ru) | 2010-02-20 |
KR101211333B1 (ko) | 2012-12-11 |
JP2012236767A (ja) | 2012-12-06 |
JPWO2006013944A1 (ja) | 2008-05-01 |
BRPI0513093A (pt) | 2008-04-29 |
US20070077411A1 (en) | 2007-04-05 |
JP5132935B2 (ja) | 2013-01-30 |
BRPI0513093B1 (pt) | 2015-07-21 |
MXPA06014100A (es) | 2007-03-07 |
RU2007107950A (ru) | 2008-09-10 |
EP3103636A1 (en) | 2016-12-14 |
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