JP5276167B2 - ガラス/ポリオレフィンフィルム積層構造を作製する方法 - Google Patents
ガラス/ポリオレフィンフィルム積層構造を作製する方法 Download PDFInfo
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- JP5276167B2 JP5276167B2 JP2011518809A JP2011518809A JP5276167B2 JP 5276167 B2 JP5276167 B2 JP 5276167B2 JP 2011518809 A JP2011518809 A JP 2011518809A JP 2011518809 A JP2011518809 A JP 2011518809A JP 5276167 B2 JP5276167 B2 JP 5276167B2
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- Prior art keywords
- layer
- polyolefin
- catalyst
- glass
- alkoxysilane
- Prior art date
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- 229920000098 polyolefin Polymers 0.000 title claims abstract description 136
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- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000003054 catalyst Substances 0.000 claims abstract description 92
- 238000000034 method Methods 0.000 claims abstract description 41
- 239000004711 α-olefin Substances 0.000 claims description 22
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- 239000000155 melt Substances 0.000 claims description 7
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims description 4
- 239000002841 Lewis acid Substances 0.000 claims description 3
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- 238000005507 spraying Methods 0.000 claims 1
- 230000001815 facial effect Effects 0.000 abstract 7
- 239000010410 layer Substances 0.000 description 121
- 239000010408 film Substances 0.000 description 44
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- 229910000077 silane Inorganic materials 0.000 description 21
- 229920000642 polymer Polymers 0.000 description 20
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
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- 150000001875 compounds Chemical class 0.000 description 8
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 6
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
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- 125000000524 functional group Chemical group 0.000 description 3
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- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 3
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229920006254 polymer film Polymers 0.000 description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 3
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- 239000000377 silicon dioxide Substances 0.000 description 3
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- AFFLGGQVNFXPEV-UHFFFAOYSA-N 1-decene Chemical compound CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 2
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- DZSNXHKDHIDHNY-UHFFFAOYSA-K 2,2-bis(prop-2-enoxymethyl)butan-1-olate 2,2-dimethyloctanoate zirconium(4+) Chemical compound [Zr+4].CCCCCCC(C)(C)C([O-])=O.CCCCCCC(C)(C)C([O-])=O.CCCCCCC(C)(C)C([O-])=O.CCC(C[O-])(COCC=C)COCC=C DZSNXHKDHIDHNY-UHFFFAOYSA-K 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- SWZOQAGVRGQLDV-UHFFFAOYSA-N 4-[2-(4-hydroxy-2,2,6,6-tetramethylpiperidin-1-yl)ethoxy]-4-oxobutanoic acid Chemical compound CC1(C)CC(O)CC(C)(C)N1CCOC(=O)CCC(O)=O SWZOQAGVRGQLDV-UHFFFAOYSA-N 0.000 description 2
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- KVOZXXSUSRZIKD-UHFFFAOYSA-N Prop-2-enylcyclohexane Chemical compound C=CCC1CCCCC1 KVOZXXSUSRZIKD-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- ZYQYMLXWTHUVFM-UHFFFAOYSA-K [Zr+3].C(CCCCCC(C)(C)C)(=O)[O-].C(CCCCCC(C)(C)C)(=O)[O-].C(CCCCCC(C)(C)C)(=O)[O-] Chemical compound [Zr+3].C(CCCCCC(C)(C)C)(=O)[O-].C(CCCCCC(C)(C)C)(=O)[O-].C(CCCCCC(C)(C)C)(=O)[O-] ZYQYMLXWTHUVFM-UHFFFAOYSA-K 0.000 description 2
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- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
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- 238000000576 coating method Methods 0.000 description 2
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- 125000004122 cyclic group Chemical group 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000012968 metallocene catalyst Substances 0.000 description 2
- ORECYURYFJYPKY-UHFFFAOYSA-N n,n'-bis(2,2,6,6-tetramethylpiperidin-4-yl)hexane-1,6-diamine;2,4,6-trichloro-1,3,5-triazine;2,4,4-trimethylpentan-2-amine Chemical compound CC(C)(C)CC(C)(C)N.ClC1=NC(Cl)=NC(Cl)=N1.C1C(C)(C)NC(C)(C)CC1NCCCCCCNC1CC(C)(C)NC(C)(C)C1 ORECYURYFJYPKY-UHFFFAOYSA-N 0.000 description 2
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- WGKLOLBTFWFKOD-UHFFFAOYSA-N tris(2-nonylphenyl) phosphite Chemical compound CCCCCCCCCC1=CC=CC=C1OP(OC=1C(=CC=CC=1)CCCCCCCCC)OC1=CC=CC=C1CCCCCCCCC WGKLOLBTFWFKOD-UHFFFAOYSA-N 0.000 description 2
- CJYDNDLQIIGSTH-UHFFFAOYSA-N 1-(3,5,7-trinitro-1,3,5,7-tetrazocan-1-yl)ethanone Chemical compound CC(=O)N1CN([N+]([O-])=O)CN([N+]([O-])=O)CN([N+]([O-])=O)C1 CJYDNDLQIIGSTH-UHFFFAOYSA-N 0.000 description 1
- LGJCFVYMIJLQJO-UHFFFAOYSA-N 1-dodecylperoxydodecane Chemical compound CCCCCCCCCCCCOOCCCCCCCCCCCC LGJCFVYMIJLQJO-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は積層構造に関する。一態様において、本発明は、ガラスとポリオレフィンフィルムとの積層構造に関し、一方、他の態様において、本発明は光起電性モジュールに関する。さらに他の態様において、本発明は、ポリオレフィンフィルムがガラスに接着接触している積層構造を作製する方法に関し、一方、さらに他の態様において本発明は、ポリオレフィンフィルムがシランで架橋され、かつガラスに対する良好な接着を示す積層構造を作製する方法に関する。
A.第1PO層の1つの対外表面をガラス層の1つの表面に;
B.触媒層を、第1PO層のガラス層と接着接触している対外表面と反対側の第1PO層の対外表面に;及び
C.第2PO層を、触媒層の第1PO層と接着接触している対外表面と反対側の触媒層の対外表面に、
接着接触させて貼り付けることを含む。
これらの層は、互いに任意の順で貼り付けることができ、例えば、触媒層が第1PO層に貼り付けられる前に、第2PO層を触媒層に貼り付けることができ、又は第1PO層がガラスに貼り付けられる前に、触媒層を第1PO層に貼り付けることもできる。
本発明の実施に有用なポリオレフィンコポリマーは、グラフト前に、立方センチメートル当たりのグラム(g/cm3)で0.91未満、好ましくは0.905未満、より好ましくは0.89未満、さらにより好ましくは0.88未満及びさらにより好ましくは0.875未満の密度を通常は有する。ポリオレフィンコポリマーは、0.85g/cm3を超え、好ましくは0.855g/cm3を超え及びより好ましくは0.86g/cm3を超える密度を通常は有する。密度はASTM D−792の手順により測定される。低密度ポリオレフィンコポリマーは、半結晶性、柔軟性として一般に特徴づけられ、優れた光学的性質、例えば、可視及びUV光の高い透過率及び低い曇り価を有する。
通常の意味で、ガラスは、ソーダライムガラス、ホウケイ酸ガラス、アクリルガラス、糖ガラス、アイシングラス(Muscovy−ガラス)、又はアルミニウムオキシナイトライドを含むが、これらに限定されない窓、多くの瓶、又は眼鏡に使用されるような硬く、脆く、透明な固体のことである。技術的な意味で、ガラスは、結晶化せずに剛直な状態に冷却された無機溶融生成物である。多くのガラスは、それらの主成分及びガラス形成材としてシリカを含む。
硬化は架橋触媒で促進され、この機能を提供する任意の触媒を、本発明の実施に使用することができる。本発明の実施に使用される触媒は、1wt%未満、好ましくは約5000ppm未満、より好ましくは2500ppm未満、及び100ppmのような低い濃度で架橋反応を触媒する十分な強度のルイス若しくはブレーンステッド酸又は塩基である。触媒は、積層構造を構築するために使用される条件下で分解に対して抵抗性である。触媒は、積層化工程中及び後に、PO樹脂を通って十分急速に拡散し、アルコキシシラン基に接触することが好ましい。触媒は、積層構造、例えば、光起電性の電池の性能を、構造の有用な寿命中に、乱さない又は劣化させないことが好ましい。触媒は、PO樹脂のガラスに対する接着を妨害しない又は劣化させないことが好ましい。芳香族スルホン酸、有機スズ化合物、有機チタン化合物、有機亜鉛化合物、及び有機ジルコニウム化合物を含むが、これらに限定されない多くの材料が、当業者に知られた触媒として作用し得る。具体的な例として、ドデシルベンゼンスルホン酸、ジブチルスズジラウレート及びKenrich Petrochemicalsにより商品名Ken−React NZ01で工業的に製造されているネオペンチル(ジアリロキシ)ジルコニウムトリネオデカノエートが挙げられる。
本発明の積層構造は、(i)ガラス層、(ii)第1アルコキシシラン含有ポリオレフィン(PO)層、(iii)触媒層、及び(iv)第2アルコキシシラン含有ポリオレフィン層を含む構造である。これらの構造は、多数の異なった方法のいずれか1つにより構築することができる。例えば1つの方法において、構造は、層の上に単に造られた層であり、例えば、第1アルコキシシラン含有ポリオレフィン層が任意の適当な様式でガラスに貼り付けられ、続いて触媒層が第1アルコキシシラン含有ポリオレフィン層に貼り付けられ、続いて第2アルコキシシラン含有ポリオレフィン層が触媒層に貼り付けられる。触媒層の第1アルコキシシラン含有ポリオレフィンへの貼り付け、及び第2アルコキシシラン含有ポリオレフィンの触媒層への貼り付けは、当技術分野において知られている任意の工程、例えば、押出し、カレンダー加工、溶液キャスト又は射出成形により行うことができる。他の方法においては、第1アルコキシシラン含有ポリオレフィン層及び第2アルコキシシラン含有ポリオレフィン層と触媒層とが多層構造に形成されて、次にそれがガラス層に貼り付けられる。
ENGAGE(登録商標)8100樹脂(The Dow Chemical Companyから入手し得る)は、密度が0.87g/cm3及びメルトインデックスが1(ASTM D1238にしたがって測定)のエチレン−オクテンコポリマーである。樹脂を、Ciba Specialties Chemicals Corporationから入手し得る抗酸化剤IRGANOX 1076(登録商標)(オクタデシル3,5−ジ−(tert)−ブチル−4−ヒドロキシヒドロシンナメート))の100ppm、及び表1に名を示した数種の他の添加剤と混合する。
CHIMASSORB 944 LDは、Ciba Specialty Chemicals Corporationから入手し得るオリゴマー性の立体障害アミンの光安定剤(ポリ[[6−[1,1,3,3−テトラメチルブチル)アミノ]−s−トリアジン−2,4−ジイル]−[(2,2,6,6−テトラメチル−4−ピペリジル)イミノ]−ヘキサメチレン−[(2,2,6,6−テトラメチル−4−ピペリジル)イミノ])である。
接着試験に使用された方法は180°剥離試験である。試験試料は、圧縮成形機中加圧下でガラス上にフィルムを置くことにより調製した。所望の接着幅は1.0インチである。試験設定の目的で、テフロン(登録商標)シートをガラスと材料との間に置いて、ガラスとポリマーとを分離する。ガラス/フィルム試料調製の条件は以下の通りである:
1)2000lbsで160℃3分間
2)8000lbsで160℃30分間
3)8000lbsで室温に冷却。
4)試料を枠から取り出し、接着試験前に48時間放置して材料を室温に慣らす。
接着強度は材料試験機(インストロン 5581)を用いて測定する。負荷速度は2インチ/分であり、試験は周囲条件(24℃及び50%RH)で行った。ガラスに対する接着を評価するために安定な剥離領域が必要である(約2インチ)。安定な剥離領域における剥離負荷のフィルム幅に対する比が接着強度として報告される。結果を表3で報告する。
ENGAGE(登録商標)8200樹脂(The Dow Chemical Companyから入手し得る)は、密度が0.87g/cm3及びメルトインデックスが5(ASTM D1238にしたがって測定)のエチレン−オクテンコポリマーである。それにVTMSをグラフトして、Killion Singleスクリュー押出し機で上記と同様な条件でフィルムに成形する。合計8グラムの重量の5層のVTMSグラフトポリオレフィンフィルムを、図1に示すようにガラスのシート上に置く。触媒(Kenrich Petrochemicalsにより工業的に製造されたネオペンチル(ジアリロキシ)ジルコニウムトリネオデカノエートであるKen−React NZ01)を、図1に示すように注射器を使用して第4層と第5層との間に量を変えて適用する。触媒の最高濃度、20,000ppmを無希釈で適用し、触媒の最低濃度を酢酸エチルに溶解した0.5mLの溶液として適用した。
1.3,000lb、150℃で3分間;
2.8,000lb、150℃で7分間;及び
3.周囲条件で室温に冷却。
接着試験は、周囲条件(24℃及び50%RH)でインストロン試験機を使用して、2インチ/分の負荷速度で実施する。剥離負荷のフィルム幅に対する比(N/mm)を接着強度として報告し、試験は安定な剥離領域が観察された後で停止する。試験結果は図3に示す。ガラスに対する接着は、20,000ppmの濃縮された触媒で消失するが、触媒濃度が2000ppmに減少すると改善される。触媒濃度が1000ppm未満であると、それはさらに改善される。
Claims (10)
- 積層構造を作製する方法であって、該構造は、(i)ガラス層、(ii)アルコキシシラン基をグラフトされたポリオレフィンからなる第1ポリオレフィン層、(iii)触媒層、及び(iv)アルコキシシラン基をグラフトされたポリオレフィンからなる第2ポリオレフィン層を含み、各層は反対側を向く対外表面を有し、
A.第1ポリオレフィン層の1つの対外表面をガラス層の1つの対外表面に;
B.触媒層を、第1ポリオレフィン層のガラス層と接着接触している対外表面と反対側の第1ポリオレフィン層の対外表面に;及び
C.第2ポリオレフィン層を、触媒層の第1ポリオレフィン層と接着接触している対外表面と反対側の触媒層の対外表面に
接着接触させて貼り付ける工程を含む方法。 - 第1ポリオレフィン層の1つの対外表面上に、触媒を含む組成物を塗布、噴霧又は擦りつけることにより触媒層が適用される、請求項1に記載の方法。
- 触媒層が、フィルム内に均一に分布された触媒を含むフィルムである、請求項1に記載の方法。
- 触媒層のフィルムが、アルコキシシラン基を含まないことを除いて第1ポリオレフィン層及び第2ポリオレフィン層と同じポリオレフィンを含む、請求項3に記載の方法。
- 第1ポリオレフィン層及び第2ポリオレフィン層の少なくとも1つが実質的に鎖状のエチレンコポリマーである、請求項3に記載の方法。
- (i)ガラス層、(ii)アルコキシシラン基をグラフトされたポリオレフィンからなる第1ポリオレフィン層、(iii)触媒層、及び(iv)アルコキシシラン基をグラフトされたポリオレフィンからなる第2ポリオレフィン層を含み、各層は、反対側を向く対外表面を有する積層構造であって、
A.第1ポリオレフィン層のガラス層の1つの対外表面と接着接触している1つの対外表面;
B.第1ポリオレフィン層のガラス層と接着接触している対外表面と反対側の第1ポリオレフィン層の対外表面と接着接触している触媒層の1つの対外表面;及び
C.触媒層の第1ポリオレフィン層と接着接触している対外表面と反対側の触媒層の対外表面と接着接触している第2ポリオレフィン層の1つの対外表面
を含む積層構造。 - 第1ポリオレフィン層及び第2ポリオレフィン層が、グラフト前に0.91g/cm3未満の密度及び75g/10分未満のメルトインデックスを有したエチレン/α−オレフィンコポリマーを含む、請求項6に記載の積層構造。
- 触媒層も、グラフト前に0.91g/cm3未満の密度及び75g/10分未満のメルトインデックスを有したエチレン/α−オレフィンコポリマーを含む、請求項6に記載の積層構造。
- 触媒層がルイス若しくはブレーンステッド酸又は塩基を含む、請求項6に記載の積層構造。
- PVパネル、太陽電池、安全ガラス又は断熱ガラスの形態にある、請求項6に記載の積層構造。
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US8084908P | 2008-07-15 | 2008-07-15 | |
US61/080,849 | 2008-07-15 | ||
PCT/US2009/050266 WO2010009017A1 (en) | 2008-07-15 | 2009-07-10 | Method of making a laminated glass/polyolefin film structure |
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US (1) | US20110168239A1 (ja) |
EP (1) | EP2308098B1 (ja) |
JP (1) | JP5276167B2 (ja) |
KR (1) | KR101595241B1 (ja) |
CN (1) | CN102089889B (ja) |
AT (1) | ATE544183T1 (ja) |
BR (1) | BRPI0910371A2 (ja) |
ES (1) | ES2381217T3 (ja) |
WO (1) | WO2010009017A1 (ja) |
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-
2009
- 2009-07-10 AT AT09790282T patent/ATE544183T1/de active
- 2009-07-10 CN CN200980127530XA patent/CN102089889B/zh not_active Expired - Fee Related
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- 2009-07-10 WO PCT/US2009/050266 patent/WO2010009017A1/en active Application Filing
- 2009-07-10 US US13/002,736 patent/US20110168239A1/en not_active Abandoned
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ATE544183T1 (de) | 2012-02-15 |
WO2010009017A1 (en) | 2010-01-21 |
JP2011528294A (ja) | 2011-11-17 |
CN102089889A (zh) | 2011-06-08 |
KR101595241B1 (ko) | 2016-02-18 |
BRPI0910371A2 (pt) | 2015-10-20 |
KR20110031386A (ko) | 2011-03-25 |
EP2308098A1 (en) | 2011-04-13 |
ES2381217T3 (es) | 2012-05-24 |
CN102089889B (zh) | 2012-12-19 |
US20110168239A1 (en) | 2011-07-14 |
EP2308098B1 (en) | 2012-02-01 |
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