JP6529496B2 - ゴム含有グラフト重合体粉体、並びにそれを含有する太陽電池用封止材及び合わせガラス用中間膜 - Google Patents
ゴム含有グラフト重合体粉体、並びにそれを含有する太陽電池用封止材及び合わせガラス用中間膜 Download PDFInfo
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- JP6529496B2 JP6529496B2 JP2016529386A JP2016529386A JP6529496B2 JP 6529496 B2 JP6529496 B2 JP 6529496B2 JP 2016529386 A JP2016529386 A JP 2016529386A JP 2016529386 A JP2016529386 A JP 2016529386A JP 6529496 B2 JP6529496 B2 JP 6529496B2
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Description
また、本発明は、前記樹脂組成物からなるフィルムに関する。
本発明におけるゴム状重合体(X)は、特に限定されず、熱可塑性のエラストマーを用いることが好ましい。熱可塑性エラストマーとしては、各種共重合樹脂が用いられる。ゴム状重合体(X)は、屈折率調整の行いやすさや、衝撃強度などの理由から、共役ジエンを含む単量体(x)を重合させて得られるものであることが好ましい。衝撃強度と耐候性に優れるゴム状重合体(X)を得る観点から、ゴム状重合体(X)は、共役ジエンとアルキル基の炭素数が2〜8のアクリル酸アルキルエステルとを含む単量体(x)を重合させて得られるものであることがより好ましい。さらに、アルキル基の炭素数は4〜8であることがさらに好ましい。また、単量体(x)は、共役ジエンとアルキル基の炭素数が2〜8のアクリル酸アルキルエステルの他に、これらの単量体と共重合可能な他の単量体を含んでも良い。
単量体(x)を乳化重合して得られるゴム状重合体ラテックスに対して、肥大化剤を添加し、粒子が肥大化された肥大化ゴム状重合体ラテックスを得ることで、ゴム含有グラフト重合体粉体の体積平均粒子径を好ましい範囲とすることができる。
ゴム含有グラフト重合体ラテックスは、前記ゴム状重合体(X)の存在下でビニル単量体(Y)をグラフト重合して得られるものである。具体的にはゴム含有グラフト重合体ラテックスは、例えば、ゴム状重合体ラテックス又は肥大化ゴム状重合体ラテックスの存在下、ビニル単量体(Y)をグラフト重合して得ることができる。
本発明において、ゴム含有グラフト重合体粉体とは、ゴム状重合体(X)の存在下でビニル単量体(Y)をグラフト重合して得られるゴム含有グラフト重合体ラテックスを粉体化させたものであり、例えば、ゴム含有グラフト重合体ラテックスを凝固させ、脱水、洗浄した後、乾燥させることにより得られる。
本発明のフィルムにおけるポリビニルアセタールの含有割合は40質量%以上であることが好ましく、50質量%以上であることがより好ましく、60質量%以上であることがさらに好ましい。ポリビニルアセタールの含有割合が40質量%未満であると、耐腐食性及び接着性が不十分となる傾向となる。また、無機物(酸化チタン、タルク等)を混合することも可能である。
本発明において樹脂組成物は、ゴム含有グラフト重合体粉体とポリビニルアセタールとを含有する。
本発明のフィルムに用いられるゴム含有グラフト重合体粉体とポリビニルアセタールとを含有する樹脂組成物は、本発明の効果を損なわない範囲であれば、可塑剤、接着力調整剤、酸化防止剤、紫外線吸収剤、光安定剤、ブロッキング防止剤、顔料、染料、機能性無機化合物等を、必要に応じてさらに含んでいてもよい。
本発明のフィルムにおけるカルシウムイオンの含有量は0〜100ppmであり、0〜85ppmであることが好ましく、0〜70ppmであることがより好ましい。カルシウムイオンの含有量をこの範囲とすることで、ガラスとの接着性及び耐腐食性を向上させることができる。カルシウムイオンの含有量をこの範囲とする方法としては、ゴム含有グラフト重合体粉体の調製における洗浄条件を調整する方法;凝析剤を選択する方法(たとえばカルシウムを含まない凝析剤を使用する)が挙げられる。
ゴム含有グラフト重合体の屈折率について、JIS K 7142のA法に基づき測定した。結果を表3及び4に示す。
ゴム含有グラフト重合体粉体1gを最大650℃で燃焼させることにより乾式灰化した。灰分を濃塩酸5mlで溶解し、精製水で50mlにメスアップして資料とし、ICP発光分光分析装置(IRIS Intrepid II XSP:サーモフィッシャーサイエンティフィック株式会社製)を用いて測定した。測定によりカルシウムイオンの含有量を求めた。結果を表1、表3及び表4に示す。
ゴム状重合体ラテックス、肥大化ゴム質共重合体ラテックス及びゴム含有グラフト重合体ラテックスの体積平均粒子径は、大塚電子株式会社製の粒子径測定器ELS800を用いて測定した。ゴム含有グラフト重合体ラテックスの濃度はおよそ0.1%に調製し、必要に応じて更に希釈して測定に供した。
[ゴム状重合体ラテックスの製造]
1,3−ブタジエンを除く物質については、その中に含まれる酸素を窒素で置換し、実質上重合反応を阻害しない状態とした。その後、アクリル酸ブチル60部、1,3−ブタジエン40部、ジイソプロピルベンゼンパーオキサイド0.2部、牛脂酸カリウム1部、N−ラウロイルザルコシン酸ナトリウム0.5部、ピロリン酸ナトリウム0.5部、硫酸第一鉄0.005部、デキストロース0,3部、脱イオン水200部をオートクレーブに仕込み、50度で9時間かけて重合を行った。その結果、モノマー転化率97%前後、体積平均粒子径0.07〜0.08μmのゴム状重合体ラテックスが得られた。
硫酸第一鉄0.003部、エチレンジアミン四酢酸ナトリウム0.009部、ナトリウムホルムアルデヒドスルホキシレート0.3部、牛脂酸カリウム1.725部、ジアルキルスルホコハク酸ナトリウム2.5部、及び脱イオン水200部を反応容器に加え、内温を60度に昇温したあと、アクリル酸ブチル85部、メタクリル酸15部及びクメンヒドロパーオキサイド0.5部からなる混合物を、2時間にわたり連続滴下で投入して重合させた。さらに2時間撹拌を続けることにより、モノマー転化率97%以上の酸基含有共重合体ラテックスを得た。
ゴム状重合体のポリマー固形分100部を含むゴム状重合体ラテックスを入れた反応容器に、脱イオン水37部を加え、内温を40度に昇温した後、4.5%水酸化ナトリウム水溶液によりpHを7〜8に調整した。その後、酸基含有共重合体ラテックス2.9部を加えて30分間保持した後、硫酸ナトリウム0.33部を加えてさらに10分間保持することによって肥大化ゴム状重合体ラテックスを得た。このときの体積平均粒子径は0.280μmであった。
蒸留水150質量部、硫酸0.6質量部からなる水溶液を50℃に加温し、撹拌しながら前記ゴム含有重合体ラテックス100質量部を投入した。投入後、80℃に昇温して10分間保持して凝固させ、洗浄脱水の後60℃で24時間乾燥させて白色のゴム含有グラフト重合体粉体(A1)を得た。このゴム含有グラフト重合体粉体のカルシウムイオン含有量は0.8ppm以下であった。
粉体化に用いる凝析剤である硫酸と酢酸カルシウムの使用量を表1に記載の通りに変更した以外は製造例1と同様の方法でゴム含有グラフト重合体粉体(A2〜A5)を得た。それぞれのゴム含有グラフト重合体粉体のカルシウムイオン量を表1に示す。
撹拌機を取り付けた2m3反応器に、PVA(平均重合度1000、けん化度99モル%)の7.5質量%水溶液1700kg、ブチルアルデヒド74.6kg及び2,6−ジ−t−ブチル−4−メチルフェノール0.13kgを仕込み、全体を14℃に冷却した。ここに、濃度20質量%の硝酸水溶液160.1Lを添加して、PVAのブチラール化を開始した。添加終了後から10分後に昇温を開始し、90分かけて65℃まで昇温し、さらに120分反応を行った。その後、室温まで冷却して析出したPVB(ポリビニルブチラール)をろ過した後、PVBに対して10倍量のイオン交換水で10回洗浄した。その後、0.3質量%水酸化ナトリウム水溶液を用いて十分に中和を行い、さらにPVBに対して10倍量のイオン交換水で10回洗浄し、脱水した後、乾燥させ、PVBを得た。得られたPVBについて、JIS K 7142のA法に基づき屈折率を測定したところ、1.491であった。
製造例6で合成したPVB(PVB−1)100質量部に対して、製造例1で得られたゴム含有グラフト重合体粉体11質量部を添加し、PVBの量に基づいてさらに酸化防止剤400ppmを添加し、公知の押出機を用いて、押出し時の樹脂温度が200℃になる条件下で、厚さ0.38mmのポリビニルブチラールフィルムを作製した。
得られたポリビニルブチラールフィルム1gを最大650℃で燃焼させることにより乾式灰化した。灰分を濃塩酸5mlで溶解し、精製水で50mlにメスアップして資料とし、ICP発光分光分析装置(IRIS Intrepid II XSP:サーモフィッシャーサイエンティフィック株式会社製)を用いて測定した。測定によりアルカリ金属イオンとアルカリ土類金属イオンの合計量を求めた。また、合わせてカルシウムイオンの含有量を求めた。結果を表3に示す。
得られたポリビニルブチラールフィルムを23℃、65%RHで24時間調湿して、含水率を1.5%に調整した。次いで、市販のフロートガラス(厚さ3.0mm、大きさ縦300mm×横300mm)を、フロートガラス/ポリビニルブチラールフィルム2枚/フロートガラスとなるように重ね、バキュームバックに投入して100℃、−0.09MPa(ゲージ圧)で処理して仮接着し、オートクレーブで160℃、1.0MPa(ゲージ圧)で処理して、合わせガラスを作製した。その後、合わせガラスを−18℃の温度で4時間放置した後、頭部の重さが0.45kgのハンマーで打って、ガラスの粒子径が6mm以下になるまで粉砕した。ポリビニルブチラールフィルムから剥離したガラス片を振り落とし、中間膜の露出度(%)をもとに、表2に示す基準にしたがってパンメル値を求めた。結果を表3に示す。パンメル値が大きいほど可塑化フィルムのガラス板に対する接着性が高いことを示す。ここで、露出度は、中間膜の全体の面積に対する、ガラス片が剥がれて中間膜が露出した部分の面積の割合である。
パンメル試験と同様にして合わせガラスを作製した。JIS K 7136に基づいて、作製した合わせガラスを用いてヘイズを測定した。結果を表3に示す。
得られたポリビニルブチラールフィルムについて、式(1)により熱水試験後の酸性成分溶出量を測定した。
図1に示すように、大きさ100mm×100mm、厚さ4mmのガラス基板11上に透明電極層12として、厚さ約700nmのSnO2膜をCVD法にて形成した。次に透明電極層12上に、プラズマCVD装置で基板全面に光電変換ユニット13としてアモルファスシリコン系薄膜を形成した。ここで、p型層13aとしてはp層のアモルファスSi膜(膜厚約15nm)、i型層13bはi層のアモルファスSi膜(膜厚約500nm)、n型層13cはn層のアモルファスSi膜(膜厚約3nm)である。次に、裏面電極14としてスパッタ法により基板全面にZnO膜(膜厚約80nm)とAg膜(膜厚約200nm)を形成し、ガラス基板上に太陽電池セルを形成した。
<条件>
熱板温度 :165℃
真空引き時間:12分
プレス圧力 :50kPa
プレス時間 :17分
太陽電池セルに電気特性が測定できるように配線を施した以外は、上記と同様の方法により太陽電池モジュールを作製した。この太陽電池モジュールについて、85℃、85%RHの条件下で2000時間暴露した前後の変換効率をAM1.5、1000W/m2の基準太陽光を照射して測定した。なお、変換効率の測定には、日清紡メカトロニクス株式会社製ソーラーシミュレーターを使用した。そして、暴露前の変換効率を100%(基準)とした場合の、暴露後の変換効率の低下率(%)を算出した。
PVBとゴム含有グラフト重合体粉体の合計量に対して、酢酸25ppm及び酢酸マグネシウム175ppmを添加した以外は、実施例1と同様にして、ポリビニルブチラールフィルムを作製した。作製したポリビニルブチラールフィルムを用いて、実施例1と同様の方法で、各種の物性評価を実施した。その結果を、表3に示す。
表3又は表4に記載の組成となるようにゴム含有グラフト重合体を添加し、PVBとゴム含有グラフト重合体粉体の合計量に対して、酢酸及び酢酸マグネシウムの合計量が表3又は表4に記載した量となるように添加した以外は、実施例1と同様にして、ポリビニルブチラールフィルムを作製した。この場合、添加した酢酸及び酢酸マグネシウムの質量比は1:7とした。作製したポリビニルブチラールフィルムを用いて、実施例1と同様の方法により、各種の物性評価を実施した。結果を表3及び表4に示す。
ゴム含有グラフト重合体粉体として、ゴム含有グラフト重合体B1(三菱レイヨン株式会社製;メタブレンS2006)を使用し、PVBとゴム含有グラフト重合体粉体の合計量に対して、酢酸及び酢酸マグネシウムの合計量が表4に記載した量となるように添加した以外は、実施例1と同様にしてポリビニルブチラールフィルムを作製した。この場合、添加した酢酸及び酢酸マグネシウムの質量比は1:7とした。作製したポリビニルブチラールフィルムを用いて、実施例1と同様の方法により、各種の物性評価を実施した。結果を表4に示す。
12 透明電極層
13 光電変換ユニット
13a p型層
13b i型層
13c n型層
14 裏面電極
15 封止材
16 ガラス基板
Claims (13)
- 屈折率が1.469〜1.519であるゴム含有グラフト重合体粉体と、ポリビニルアセタールとを含有する樹脂組成物からなり、かつ、カルシウムイオンを0〜100ppm、アルカリ金属イオンとアルカリ土類金属イオンを合計で1〜1100ppm含有するフィルムであって、
ゴム含有グラフト重合体粉体がゴム状重合体(X)を含有し、
ゴム状重合体(X)が、共役ジエン単位(x1)25〜75質量%、アルキル基の炭素数が2〜8のアクリル酸アルキルエステル単位(x2)75〜25質量%、及び共重合可能な他の単量体単位(x3)0〜5質量%を含有する、フィルム。 - 前記樹脂組成物中、ポリビニルアセタール100質量部に対してゴム含有グラフト重合体粉体の含有量が1〜100質量部である、請求項1に記載のフィルム。
- 前記樹脂組成物がさらにマグネシウム塩を含有する、請求項1又は2に記載のフィルム。
- 前記ゴム含有グラフト重合体粉体中のカルシウムイオンの含有量が0〜1000ppmである、請求項1〜3のいずれかに記載のフィルム。
- ポリビニルアセタールとゴム含有グラフト重合体粉体との屈折率の差が±0.02以下であり、カルシウムイオンを0〜100ppm、アルカリ金属イオンとアルカリ土類金属イオンを合計で1〜1100ppm含有するフィルム用樹脂組成物であって、
ゴム含有グラフト重合体粉体がゴム状重合体(X)を含有し、
ゴム状重合体(X)が、共役ジエン単位(x1)25〜75質量%、アルキル基の炭素数が2〜8のアクリル酸アルキルエステル単位(x2)75〜25質量%、及び共重合可能な他の単量体単位(x3)0〜5質量%を含有する、フィルム用樹脂組成物。 - カルシウムイオンの含有量が0〜750ppmであり、屈折率が1.469〜1.519であり、
ゴム状重合体(X)を含有し、
ゴム状重合体(X)が、共役ジエン単位(x1)25〜75質量%、アルキル基の炭素数が2〜8のアクリル酸アルキルエステル単位(x2)75〜25質量%、及び共重合可能な他の単量体単位(x3)0〜5質量%を含有する、ポリビニルアセタール樹脂フィルム用ゴム含有グラフト重合体粉体。 - ゴム状重合体(X)の存在下でビニル単量体(Y)をグラフト重合して得られるゴム含有グラフト重合体ラテックスを、無機酸、有機酸、無機酸または有機酸のアルカリ金属塩、及び無機酸または有機酸のアルミニウム塩から選ばれる少なくとも1種を含む凝析剤を用いて凝固して回収して得られる、請求項6に記載のポリビニルアセタール樹脂フィルム用ゴム含有グラフト重合体粉体。
- 前記ビニル単量体(Y)が、メタクリル酸メチル(y1)50〜100質量%とアルキル基の炭素数が1〜8のアクリル酸アルキルエステル及び/又はスチレン(y2)50〜0質量%を含有する、請求項7に記載のポリビニルアセタール樹脂フィルム用ゴム含有グラフト重合体粉体。
- 前記ゴム状重合体(X)のポリマー固形分100質量部の存在下に、前記ビニル単量体(Y)10〜1000質量部をグラフト重合して得られたものである、請求項7又は8に記載のポリビニルアセタール樹脂フィルム用ゴム含有グラフト重合体粉体。
- 請求項6〜9のいずれかに記載のポリビニルアセタール樹脂フィルム用ゴム含有グラフト重合体粉体と、ポリビニルアセタールとを含有する樹脂組成物。
- 請求項10に記載の樹脂組成物からなるフィルム。
- 請求項1〜4及び11のいずれかに記載のフィルムを有する合わせガラス用中間膜又は太陽電池用封止材。
- 請求項12に記載の合わせガラス用中間膜又は太陽電池用封止材により作製される合わせガラス又は太陽電池。
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JP6394728B1 (ja) * | 2017-03-23 | 2018-09-26 | 日本ゼオン株式会社 | 非水系二次電池正極用バインダー組成物、非水系二次電池正極用組成物、非水系二次電池用正極および非水系二次電池 |
DE202017107931U1 (de) * | 2017-12-28 | 2019-04-01 | Inalfa Roof Systems Group B.V. | Dachkonstruktion für ein Fahrzeug und ein semi-transparentes Photovoltaik-Paneel darin |
CN108312670B (zh) * | 2018-01-30 | 2020-09-22 | 四川雄港玻璃有限公司 | 一种夹胶玻璃的生产工艺 |
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US9475262B2 (en) * | 2010-08-23 | 2016-10-25 | Kuraray Co., Ltd. | Solar-cell sealant and laminated-glass interlayer |
CN104918969A (zh) * | 2012-12-17 | 2015-09-16 | 株式会社可乐丽 | 含橡胶接枝聚合物粉体、以及含有其的太阳能电池用密封材料及夹层玻璃用中间膜 |
JP2014201679A (ja) * | 2013-04-05 | 2014-10-27 | 三菱化学株式会社 | ポリカーボネート樹脂組成物、及びこれを用いた成形品 |
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US20170145173A1 (en) | 2017-05-25 |
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