JP6073590B2 - 積層体形成用シート製造用組成物、その製造方法、及び積層体形成用シート - Google Patents
積層体形成用シート製造用組成物、その製造方法、及び積層体形成用シート Download PDFInfo
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- JP6073590B2 JP6073590B2 JP2012163453A JP2012163453A JP6073590B2 JP 6073590 B2 JP6073590 B2 JP 6073590B2 JP 2012163453 A JP2012163453 A JP 2012163453A JP 2012163453 A JP2012163453 A JP 2012163453A JP 6073590 B2 JP6073590 B2 JP 6073590B2
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- 238000000879 optical micrograph Methods 0.000 description 1
- 239000001301 oxygen Chemical group 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- LYXOWKPVTCPORE-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanone Chemical compound C=1C=C(C=2C=CC=CC=2)C=CC=1C(=O)C1=CC=CC=C1 LYXOWKPVTCPORE-UHFFFAOYSA-N 0.000 description 1
- 239000011990 phillips catalyst Substances 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 150000007519 polyprotic acids Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003329 sebacic acid derivatives Chemical class 0.000 description 1
- WYKYCHHWIJXDAO-UHFFFAOYSA-N tert-butyl 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)C WYKYCHHWIJXDAO-UHFFFAOYSA-N 0.000 description 1
- JZFHXRUVMKEOFG-UHFFFAOYSA-N tert-butyl dodecaneperoxoate Chemical compound CCCCCCCCCCCC(=O)OOC(C)(C)C JZFHXRUVMKEOFG-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
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Description
(2)前記ポリエチレンからなる島相の平均アスペクト比(平均長径(l)/平均短径(d))が、40以下である。これにより、更にPEの配合比を高くすることができる。
(3)組成物の粘度が30000Pa・sとなる温度が、70〜100℃であり、且つ組成物の粘度が20000〜50000Pa・sとなる温度範囲の幅が5.0℃以上である。
(4)前記ポリエチレンが、低密度ポリエチレン及び/又は直鎖状低密度ポリエチレンから選択される1種以上のポリエチレンからなる。これらのポリエチレンは比較的低融点で、結晶化度が低い点で好ましい。
(5)前記ポリエチレンが、2種以上のポリエチレンからなる。
(6)前記ポリエチレンが、1種以上の低密度ポリエチレン、及び1種以上の直鎖状低密度ポリエチレンからなる。低密度ポリエチレンと直鎖状低密度ポリエチレンとを併用することで、引張強度に優れ、且つ比較的低融点の組成物を得ることができる。
(7)前記エチレン−酢酸ビニル共重合体のJIS K7210で規定されるメルトフローレートが、1.0〜50g/10分である。
(8)前記エチレン−酢酸ビニル共重合体の酢酸ビニル含有量が、20〜40質量%である。
本発明において、ポリエチレン(PE)は、JISに規定される通り、エチレンを主体とする重合体であり、エチレンの単独重合体、エチレンと5モル%以下の炭素数3以上のα−オレフィン例えばブテン−1、ヘキセン−1、4―メチルペンテン−1、オクテン−1等との共重合体、エチレンと官能基に炭素、酸素、および水素だけを有する1モル%以下の非オレフィン単量体との共重合体を含む(JISK6922−1:1997附属書参照)。PEは一般に、その密度によって分類され、高密度ポリエチレン(HDPE(又はPE−HD))、低密度ポリエチレン(LDPE(又はPE−LD))、直鎖状低密度ポリエチレン(LLDPE(又はPE−LLD)等が挙げられる。PEとしてはどのようなものでも良いが、比較的融点が低く、結晶化度が低い、低密度ポリエチレン及び/又は直鎖状低密度ポリエチレンから選択される1種以上のポリエチレンからなることが好ましい。
本発明において、エチレン−酢酸ビニル共重合体(EVA)における酢酸ビニルの含有率は、通常、EVAの質量に対して20〜45質量%である。EVAの酢酸ビニル単位の含有量が低い程、得られる組成物が硬くなる傾向がある。酢酸ビニルの含有量が20質量%未満では、本発明の組成物を用いて得られる積層体形成用シートを高温で架橋硬化させた場合に、架橋硬化後のシートの透明性が充分でないおそれがある。また、45質量%を超えると、得られる架橋硬化後のシートの硬さが不十分となる場合があり、更にカルボン酸、アルコール、アミン等が発生し積層体における他の部材等との界面で発泡が生じ易くなるおそれがある。
架橋剤は、EVAの架橋構造を形成することができるもので、本発明の組成物を用いて得られる積層体形成用シートの強度、接着性及び耐久性を向上することができる。架橋剤は、有機過酸化物又は光重合開始剤を用いることが好ましい。なかでも、接着力、透明性、耐湿性、耐貫通性の温度依存性が改善された積層体形成用シートが得られることから、有機過酸化物を用いるのが好ましい。
架橋助剤は、EVAのゲル分率を向上させ、本発明の組成物を用いて得られる積層体形成用シートの接着性及び耐久性を向上させることができる。
接着向上剤としては、シランカップリング剤を用いることができる。これにより、得られる積層体形成用シートの接着力を、更に向上させることができる。前記シランカップリング剤としては、γ−クロロプロピルトリメトキシシラン、ビニルトリエトキシシラン、ビニルトリス(β−メトキシエトキシ)シラン、γ−メタクリロキシプロピルトリメトキシシラン、ビニルトリアセトキシシラン、γ−グリシドキシプロピルトリメトキシシラン、γ−グリシドキシプロピルトリエトキシシラン、β−(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、ビニルトリクロロシラン、γ−メルカプトプロピルトリメトキシシラン、γ−アミノプロピルトリエトキシシラン、N−β−(アミノエチル)−γ−アミノプロピルトリメトキシシランを挙げることができる。これらシランカップリング剤は、単独で使用しても、又は2種以上組み合わせて使用しても良い。なかでも、γ−メタクリロキシプロピルトリメトキシシランが特に好ましく挙げられる。
可塑剤としては、トリスイソデシルホスファイト、トリスノニルフェニルホスファイト等のホスファイトやリン酸エステル等のリン含有化合物、アジピン酸エーテルエステル、トリメリテートn−オクチル、フタル酸ジオクチル、アジピン酸ジヘキシル、セバシン酸ジブチル等の多塩基酸のエステル、2,2,4−トリメチル−1,3−ペンタンジオールジソブチレート、トリ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ヘプタノエート、トリエチレングリコールジペラルゴネート等の多価アルコールのエステル、エポキシ化脂肪酸アルキルエステル等が使用できる。
本発明の積層体形成用シート製造用組成物の製造方法は、上述の海島構造が形成される条件であれば、特に制限はない。特にPEの配合比が高い組成物の場合は、海島構造が形成され難いので、上述の海島構造を形成する混練条件を含むことが好ましい。即ち、EVA及びPEを、EVAの粘度VEVA[Pa・s]に対して、PEの粘度VPE[Pa・s]が0.1〜20倍となる条件下、特にPEの配合比がEVAの配合比より高い組成物の場合、好ましくは1倍より大きく20倍以下、更に好ましくは2〜15倍、特に好ましくは4〜13倍となる条件下で混練する混練工程を含むことが好ましく、更に混練工程が、せん断速度10〜1500s-1、更に好ましくは100〜1000s-1、特に好ましくは200〜800s-1の条件で混練する工程であることが好ましい。
本発明の積層体形成用シートは、本発明の積層体形成用シート製造用組成物をシート状に製膜することで得られるものである。本発明の積層体形成用シートは、本発明の組成物を、必要に応じてロール練り等の二次混練を行った後、通常の押出成形、又はカレンダ成形(カレンダリング)等により成形してシート状物を得る方法により製造することができる。製膜時の加熱温度は、特に架橋剤を配合する場合、架橋剤が反応しない或いはほとんど反応しない温度とすることが好ましい。例えば、50〜90℃、特に40〜80℃とするのが好ましい。積層体形成用シートの厚さは、特に制限されず、用途によって適宜設定することができる。一般に、50μm〜2mmの範囲である。
本発明の積層体形成用シートは、本発明の組成物を用いて製造されているので、PEを含むことにより、耐熱性等が付与され、且つEVA組成物と同様な条件で得られるため、高品質且つ低コストの積層体形成用シートである。また、EVA組成物から形成されたシートと同様に用いることができるため、合わせガラス用中間膜又は太陽電池用封止膜として好ましく使用することができる。
表1及び2に示す物性のEVA及びPEを各配合量、混練条件で混練し、EVA及びPE混合組成物を調製した。各組成物におけるEVAの粘度に対する及びPEの粘度(PE粘度/EVA粘度)は、キャピログラフ(東洋精機社製)を用い、せん断速度6.1s-1、温度は混練温度となる120℃で各樹脂の粘度を測定し、算出した。
評価結果を表1及び2に示す。
12 中間膜
21 表面側透明保護部材
22 裏面側保護部材
23A 表面側封止膜
23B 裏面側封止膜
24 太陽電池用セル
Claims (8)
- エチレン−酢酸ビニル共重合体、及びポリエチレンを含む積層体形成用シート製造用組成物の製造方法であって、
前記エチレン−酢酸ビニル共重合体(EVA)及び前記ポリエチレン(PE)を、EVAの粘度V EVA [Pa・s]に対するPEの粘度V PE [Pa・s]が0.14〜15倍となる条件下で混練する混練工程を含み、
該条件において、EVAの粘度V EVA が2000〜20000Pa・sであり、PEの粘度V PE が30000〜50000Pa・sであり、
前記混練する際のせん断速度が150〜500 s−1 であり、
前記組成物は、前記エチレン−酢酸ビニル共重合体が海相であり、前記ポリエチレンが島相である海島構造を有し、
前記混練工程において、前記エチレン−酢酸ビニル共重合体(EVA)と前記ポリエチレン(PE)の体積比(EVA:PE)が、90:10〜30:70の範囲であり、
前記積層体形成用シートが、合わせガラス用中間膜又は太陽電池用封止膜であることを特徴とする製造方法。 - 組成物の粘度が30000Pa・sとなる温度が、70〜100℃であり、且つ組成物の粘度が20000〜50000Pa・sとなる温度範囲の幅が5.0℃以上である請求項1に記載の製造方法。
- 前記ポリエチレンが、低密度ポリエチレン及び/又は直鎖状低密度ポリエチレンから選択される1種以上のポリエチレンからなる請求項1又は2に記載の製造方法。
- 前記ポリエチレンが、2種以上のポリエチレンからなる請求項1〜3のいずれか1項に記載の製造方法。
- 前記ポリエチレンが、1種以上の低密度ポリエチレン、及び1種以上の直鎖状低密度ポリエチレンからなる請求項4に記載の製造方法。
- 前記エチレン−酢酸ビニル共重合体のJIS K7210で規定されるメルトフローレートが、1.0〜50.0g/10分である請求項1〜5のいずれか1項に記載の製造方法。
- 前記エチレン−酢酸ビニル共重合体の酢酸ビニル含有量が、20〜40質量%である請求項1〜6のいずれか1項に記載の製造方法。
- 前記混練工程が、70〜130℃の温度条件で混練する工程である請求項1〜7のいずれか1項に記載の製造方法。
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