JP6664352B2 - 重合体、組成物、塗膜、積層体、バックシート及び太陽電池モジュール - Google Patents
重合体、組成物、塗膜、積層体、バックシート及び太陽電池モジュール Download PDFInfo
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- JP6664352B2 JP6664352B2 JP2017134483A JP2017134483A JP6664352B2 JP 6664352 B2 JP6664352 B2 JP 6664352B2 JP 2017134483 A JP2017134483 A JP 2017134483A JP 2017134483 A JP2017134483 A JP 2017134483A JP 6664352 B2 JP6664352 B2 JP 6664352B2
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- vinyl
- acid
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- 229910052794 bromium Inorganic materials 0.000 description 8
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- 239000002987 primer (paints) Substances 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
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- 125000003277 amino group Chemical group 0.000 description 6
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Images
Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/62—Polymers of compounds having carbon-to-carbon double bonds
- C08G18/6275—Polymers of halogen containing compounds having carbon-to-carbon double bonds; halogenated polymers of compounds having carbon-to-carbon double bonds
- C08G18/6279—Polymers of halogen containing compounds having carbon-to-carbon double bonds; halogenated polymers of compounds having carbon-to-carbon double bonds containing fluorine atoms
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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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/082—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising vinyl resins; comprising acrylic resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Description
式(A):CH2=CH−(CH2)l−O−(CH2)m−OH
(式中、lは0または1、mは2〜20の整数)で示されるものが更に好ましく、4−ヒドロキシブチルビニルエーテル、2−ヒドロキシエチルビニルエーテル、2−ヒドロキシエチルアリルエーテル及び4−ヒドロキシブチルアリルエーテルからなる群より選択される少なくとも1種の単量体が特に好ましい。
式(B):R1aR2aC=CR3a−(CH2)n−COOH
(式中、R1a、R2aおよびR3aは、同じかまたは異なり、いずれも水素原子または炭素数1〜10の直鎖または分岐鎖状のアルキル基;nは0以上の整数)で示されるものが好ましく、たとえば、アクリル酸、メタクリル酸、ビニル酢酸、クロトン酸、ペンテン酸、ヘキセン酸、ヘプテン酸、オクテン酸、ノネン酸、デセン酸、ウンデシレン酸、ドデセン酸、トリデセン酸、テトラデセン酸、ペンタデセン酸、ヘキサデセン酸、ヘプタデセン酸、オクタデセン酸、ノナデセン酸、エイコセン酸、22−トリコセン酸等が挙げられる。なかでも、アクリル酸、クロトン酸及びウンデシレン酸からなる群より選択される少なくとも1種が好ましく、アクリル酸及びクロトン酸からなる群より選択される少なくとも1種がより好ましい。
上記一般式(1)中のR1は、上記3価以上の脂肪族多価アルコールに基づく炭化水素基であり、炭素数3〜10の脂肪族炭化水素基がより好ましく、炭素数3〜6の脂肪族炭化水素基が更に好ましい。
上記R2がフェニレン基である場合、1,2−フェニレン基(o−フェニレン基)、1,3−フェニレン基(m−フェニレン基)、及び、1,4−フェニレン基(p−フェニレン基)のいずれであってもよい。中でも、1,3−フェニレン基(m−フェニレン基)が好ましい。また、上記一般式(1)中の全てのR2が同じフェニレン基であってもよく、2種以上が混在していてもよい。
上記R2がシクロヘキシレン基である場合、1,2−シクロヘキシレン基、1,3−シクロヘキシレン基、及び、1,4−シクロヘキシレン基のいずれであってもよい。中でも、1,3−シクロヘキシレン基が好ましい。また、上記一般式(1)中の全てのR2が同じシクロヘキシレン基であってもよく、2種以上が混在していてもよい。
上記kは、3価以上の脂肪族多価アルコールの価数に対応する数である。上記kとして、より好ましくは3〜10の整数であり、更に好ましくは3〜6の整数である。
上記イソシアヌレート構造体としては、上記イソシアネートの三量化反応により得られる三量体、五量化反応により得られる五量体、七量化反応により得られる七量体等を挙げることができる。
中でも、下記一般式(3):
上記一般式(5)中のR3で表されるフェニレン基又はシクロヘキシレン基については、上記一般式(1)におけるR2について述べたとおりである。
上記ブロックイソシアネートとしては、ヘキサメチレンジイソシアネートから誘導されるポリイソシアネート化合物(以下、ポリイソシアネート化合物(II)ともいう。)をブロック化剤で反応させて得られるものが好ましい。
上記ポリイソシアネート化合物(II)としては、例えば、ヘキサメチレンジイソシアネートと3価以上の脂肪族多価アルコールとを付加重合して得られるアダクト、ヘキサメチレンジイソシアネートからなるイソシアヌレート構造体(ヌレート構造体)、及び、ヘキサメチレンジイソシアネートからなるビウレットを挙げることができる。
上記一般式(6)中のR4は、上記3価以上の脂肪族多価アルコールに基づく炭化水素基であり、炭素数3〜10の脂肪族炭化水素基がより好ましく、炭素数3〜6の脂肪族炭化水素基が更に好ましい。
上記kは、3価以上の脂肪族多価アルコールの価数に対応する数である。上記kとして、より好ましくは3〜10の整数であり、更に好ましくは3〜6の整数である。
上記イソシアヌレート構造体としては、上記イソシアネートの三量化反応により得られる三量体、五量化反応により得られる五量体、七量化反応により得られる七量体等を挙げることができる。
中でも、下記一般式(7):
ヘキサメチレンジイソシアネートと、上記のような3価以上の脂肪族多価アルコールとを付加重合することにより、上記アダクトが得られる。
中でも、活性メチレン化合物、オキシム類が好ましく、活性メチレン化合物がより好ましい。
上記一般式(9)中のR5は、上記3価以上の脂肪族多価アルコールに基づく炭化水素基であり、炭素数3〜10の脂肪族炭化水素基がより好ましく、炭素数3〜6の脂肪族炭化水素基が更に好ましい。
上記kは、3価以上の脂肪族多価アルコールの価数に対応する数である。上記kとして、より好ましくは3〜10の整数であり、更に好ましくは3〜6の整数である。
上記イソシアヌレート構造体としては、イソホロンジイソシアネートの三量化反応により得られる三量体、五量化反応により得られる五量体、七量化反応により得られる七量体等を挙げることができる。
中でも、下記一般式(11):
上記カーボンブラックの市販品としては、例えば、MA−100(三菱化学社製)、Raven−420(コロンビアカーボン社製)等が挙げられる。
上記分散剤は、実質的に塩基を含まないことが更に好ましい。なお、実質的に塩基を含まないとは、コンタミネーション、反応残査、測定誤差等を考慮し、測定値として塩基価が0.5mgKOH/g以下をいう。上記塩基価は、酸性物質を用いた酸塩基滴定法により測定することができる。
これらの難燃剤は重合体(B)の種類に応じて、少なくとも1種と配合量を任意に選ぶことができ、これらに限定されるものではない。
具体的には、上記臭素含有化合物は、デカブロモジフェニルオキサイド、1,2−ビス(2,3,4,5,6−ペンタブロモフェニル)エタン、トリス(トリブロモフェノキシ)トリアジン、エチレンビステトラブロモフタロイミド、ポリブロモフェニルインダン、臭素化フェニレンオキサイド、及び、ポリペンタブロモベンジルアクリレートからなる群より選択される少なくとも1種が好ましい。
(R9−O)b−P(=O)−(OH)3−b
(式中、bは1または2、R9は有機残基を示す)で示される有機酸性リン酸エステルなどがあげられる。
上記表面層3には、通常ガラス板が用いられるが、樹脂シート等のフレキシブルな材料を用いてもよい。
塗膜7を構成する材料は、上述した塗膜とは異なる塗膜でも、含フッ素ポリマーシートでも、ポリエステルシートでも、ポリエステル塗料の塗膜でもよい。
また、上記塗膜と封止材層との密着性をさらに向上させるために、上記塗膜に従来公知の表面処理を行ってもよい。表面処理としては、例えばコロナ放電処理、プラズマ放電処理、化成処理、ブラスト処理等が例示できる。
元素分析から測定したフッ素含有量(質量%)と1HNMRスペクトルによる組成分析から各モノマー単位の含有量(モル%)を算出した。
重合時の水酸基モノマーの実仕込量と固形分濃度を使用して計算から算出した。
JIS A 1452:1972建築材料および建築構成部分の摩耗試験方法(落砂法)による。
各参考例で得られたバックシートを初期状態とPCT(プレッシャークッカーテスト、121℃、湿度100%RH、2気圧)60時間後の塗膜に対してJIS D0202−1988に準処して碁盤目テープ剥離試験を行った。セロハンテープ(「CT24」、ニチバン社製)を用い、指の腹でフィルムに密着させた後剥離した。判定は、100マスの内、剥離しないマス目の数で表した。
SWOM(スガ試験機社製耐候性試験機:試験時間6000時間)を用い、初期の60度光沢を100として6000時間後の光沢保持率で表わす。
容量6000mlのステンレス製オートクレーブに酢酸ブチル2500g、ネオノナン酸ビニルエステル584g、4−ヒドロキシブチルビニルエーテル(HBVE)527gを投入し、減圧窒素置換の操作を行い、テトラフルオロエチレン(TFE)658gを仕込んだ。撹拌下に60.0℃まで昇温し、過酸化物系重合開始剤30gを仕込み重合を開始した。反応器内圧が1.0MPaGから0.4MPaGへ低下した時点で反応を停止し、重合体を含む溶液を得た。この重合体の組成及び水酸基価を表1に示す。
この分散液100質量部にイソシアネート系硬化剤(住化バイエル社製のスミジュールN3300)を、上記イソシアネート系硬化剤が有するイソシアネート基(NCO)と上記重合体が有する水酸基(OH)との当量比(NCO/OH)が表1の当量比になるように配合して、組成物を調製した。
参考例1と同様にして、重合体、組成物及びバックシートを作製した。結果を表1に示す。
TFE:テトラフルオロエチレン
CTFE:クロロトリフルオロエチレン
VV9:ネオノナン酸ビニルエステル
VV10:ネオデカン酸ビニルエステル
VBz:安息香酸ビニル
VAc:酢酸ビニル
EVE:エチルビニルエーテル
HBVE:4−ヒドロキシブチルビニルエーテル
HEVE:2−ヒドロキシエチルビニルエーテル
AA:アクリル酸
CA:クロトン酸
2:封止材層
3:表面層
4:バックシート
5:水不透過性シート
6:本発明の組成物から形成された塗膜
7:他の塗膜
Claims (8)
- 重合体及びポリイソシアネート化合物を含み、
前記重合体は、パーハロオレフィン単位及び水酸基含有モノマー単位を含み、かつ、水酸基価が110mgKOH/g以上であり、
前記ポリイソシアネート化合物が有するイソシアネート基(NCO)と前記重合体が有する水酸基(OH)との当量比(NCO/OH)が0.90以下である
ことを特徴とする組成物(ただし、クロロトリフルオロエチレン、シクロヘキシルビニルエーテル、イソブチルビニルエーテル、ヒドロキシブチルビニルエーテル及びアクリル酸の共重合体であって重量平均分子量が15400、水酸基価が145mgKOH/gであるフッ素樹脂コポリマーと、ヘキサメチレンジイソシアネートのイソシアヌレート体とを含み、前記イソシアヌレート体が有するイソシアネート基(NCO)と前記フッ素樹脂コポリマーが有する水酸基(OH)との当量比(NCO/OH)が0.36である塗料組成物を除く)。 - 前記パーハロオレフィンは、テトラフルオロエチレン、クロロトリフルオロエチレン、及び、ヘキサフルオロプロピレンからなる群より選択される少なくとも1種である請求項1記載の組成物。
- 前記水酸基含有モノマーは、ヒドロキシアルキルビニルエーテルである請求項1又は2記載の組成物。
- 前記重合体は、更に、水酸基及び芳香環のいずれをも含まないビニルエステル単位及び水酸基を含まないアルキルビニルエーテル単位からなる群より選択される少なくとも1種の単位(b)を含む請求項1、2又は3記載の組成物。
- 更に、溶媒を含む請求項1、2、3又は4記載の組成物。
- 請求項1、2、3、4又は5記載の組成物から形成されることを特徴とする塗膜。
- 請求項6記載の塗膜を備えることを特徴とするバックシート。
- 請求項7記載のバックシートを備えることを特徴とする太陽電池モジュール。
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