JP5250025B2 - 強化シリコーン樹脂フィルム - Google Patents
強化シリコーン樹脂フィルム Download PDFInfo
- Publication number
- JP5250025B2 JP5250025B2 JP2010506395A JP2010506395A JP5250025B2 JP 5250025 B2 JP5250025 B2 JP 5250025B2 JP 2010506395 A JP2010506395 A JP 2010506395A JP 2010506395 A JP2010506395 A JP 2010506395A JP 5250025 B2 JP5250025 B2 JP 5250025B2
- Authority
- JP
- Japan
- Prior art keywords
- silicone resin
- alternatively
- polymer
- resin film
- composition
- 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.)
- Expired - Fee Related
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- C08J5/18—Manufacture of films or sheets
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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Description
本願は、2007年5月1日付で出願された米国仮特許出願第60/915,137号明細書の米国特許法第119条(e)項に基づく利益を主張するものである。米国仮特許出願第60/915,137号明細書は、参照により本明細書中に援用される。
第1の高分子層を形成すること、及び
第1の高分子層上に少なくとも1つのさらなる高分子層を形成することを含む方法であって、高分子層の少なくとも1つが、ジシリロキサン単位を含む少なくとも1つのシリコーン樹脂の硬化生成物を含み、且つ高分子層の少なくとも1つが炭素ナノ材料を含む、方法によって調製することができる。第1の高分子層及びさらなる高分子層(複数可)は、強化シリコーン樹脂フィルムの高分子層について上記に記載及び例示した通りである。
R1 2SiO1/2単位(M単位)、R1 2SiO2/2単位(D単位)、R1SiO3/2単位(T単位)及びSiO4/2単位(Q単位)(式中、R1は上記に記載及び例示した通りである)
で表され得る。
本実施例では、化学的に酸化させた炭素ナノファイバの調製を説明する。Pyrograf(登録商標)−III炭素ナノファイバ(2.0g)、12.5mLの濃硝酸、及び37.5mLの濃硫酸を、冷却器、温度計、テフロン(登録商標)加工磁気攪拌棒及び温度制御器を備える500mL容の三つ口フラスコ中で順次混合した。混合物を80℃に加熱してこの温度で3時間維持した。その後、フラスコを1ガロン(3.79リットル)のバケツに入れたドライアイス層上に置くことによって、混合物を冷却した。この混合物を、ナイロン膜(0.8μm)を含有するブフナー漏斗に注ぎ、炭素ナノファイバを減圧濾過により回収した。濾液のpHが洗浄水のpHと等しくなるまで、膜上に残るナノファイバを脱イオン水で数回洗浄した。最後の洗浄後、減圧しながらさらに15分間漏斗中で炭素ナノファイバを保持した。その後、フィルター膜上に担持されるナノファイバを炉内で100℃にて1時間放置した。炭素ナノファイバをフィルター膜から取り出し、乾燥した封止ガラスジャー内に貯蔵した。
ジシラン組成物A(15g)を、28.6gのPhSiCl3、120gのメチルイソブチルケトン及び19.48gの無水メタノールと混合した。反応により産生されたHClを、フラスコの開口部から逃がした。液体混合物を密閉ビンに入れ、氷水浴中で冷却した後、攪拌子及び温度計を備える三つ口丸底フラスコの上部に取り付けられた添加漏斗に移した。脱イオン水(120g)をフラスコに入れ、外部の氷水浴で2℃〜4℃に冷やした。添加漏斗中の混合物は、冷却した脱イオン水に10分間にわたって継続的に添加されたが、その間、混合物の温度は3℃〜5℃上昇した。添加の完了後、混合物を氷浴中で1時間攪拌した。次にフラスコを水浴で50℃〜75℃に加熱し、1時間その温度に維持した。混合物を室温まで冷やした後、NaCl(10g)の水溶液(200mL)で4回洗浄した。各洗浄の後、水相を廃棄した。有機相を単離し、遠心分離して、濾過した。有機相はシリコーン樹脂分を21.25%(w/w)有していた。
実施例1の酸化させた炭素ナノファイバ(0.011g)及び26gの実施例2のシリコーン樹脂製剤をガラスバイアル内で混合した。このバイアルを超音波浴に30分間入れた。次に、この混合物を2000rpmで30分間遠心分離にかけた。上澄みシリコーン組成物を用いて、以下に記載するように強化シリコーン樹脂フィルムを調製した。
約5cm/秒の速度で布を組成物中に通すことによって、ガラス布(38.1cm×8.9cm)に、実施例3のシリコーン組成物を含浸させた。次に、含浸させた布をドラフトチャンバー内に室温で2時間垂直に吊り下げ、その後、サイクル(50℃、2時間;2.5℃/分で50℃から150℃まで、150℃、0.5時間)に従って空気循環炉内で硬化した。炉のスイッチを切り、強化シリコーン樹脂フィルムを室温に冷却した。
ジシラン組成物A(50g)を、31gのMeSiCl3、300gのメチルイソブチルケトン及び80mlの無水メタノールと混合した。反応により産生されたHClを、フラスコの開口部から逃がした。液体混合物を密閉ビンに入れ、氷水浴中で冷却した後、攪拌子及び温度計を備える三つ口丸底フラスコの上部に取り付けられた添加漏斗に移した。脱イオン水(250g)をフラスコに入れ、外部の氷水浴で2℃〜4℃に冷やした。添加漏斗中の混合物は、冷却した脱イオン水に10分間にわたって継続的に添加されたが、その間、混合物の温度は3℃〜5℃上昇した。添加の完了後、混合物を氷浴中で1時間攪拌した。次にフラスコを水浴で50℃〜75℃に加熱し、1時間その温度に維持した。混合物を室温まで冷やした後、NaCl(10g)の水溶液(200mL)で4回洗浄した。各洗浄の後、水相を廃棄した。有機相を単離し、遠心分離して、濾過した。有機相はシリコーン樹脂分を13.70%(w/w)有していた。80℃、5mmHg(667Pa)の圧力下で濃縮し、シリコーン樹脂を27.40%(w/w)含有する溶液を産生した。
実施例1の酸化させた炭素ナノファイバ(0.011g)及び26gの実施例5のシリコーン樹脂製剤をガラスバイアル内で混合した。このバイアルを超音波浴に30分間入れた。次に、この混合物を2000rpmで30分間遠心分離にかけた。上澄みシリコーン組成物を用いて、以下に記載するように強化シリコーン樹脂フィルムを調製した。
実施例3のシリコーン組成物を実施例6のシリコーン組成物に置き換えた以外は、実施例4の方法に従って強化シリコーン樹脂フィルムを調製した。強化シリコーン樹脂フィルムの機械特性を表1に示す。
Claims (10)
- 少なくとも2つの高分子層を含む強化シリコーン樹脂フィルムであって、該高分子層の少なくとも1つが、式O(3−a)/2R1 aSi−SiR1 bO(3−b)/2(I)(式中、各R1は独立して、−H、ヒドロカルビル又は置換ヒドロカルビルであり、aは0、1又は2であり、且つbは0、1、2又は3である)を有するジシリロキサン単位を含む少なくとも1つのシリコーン樹脂の硬化生成物を含み、且つ前記高分子層の少なくとも1つが炭素ナノ材料を含む、強化シリコーン樹脂フィルム。
- 前記高分子層がそれぞれ0.01μm〜1000μmの厚みを有する、請求項1に記載の強化シリコーン樹脂フィルム。
- 2〜10の高分子層を含む、請求項1又は2に記載の強化シリコーン樹脂フィルム。
- 前記炭素ナノ材料が、炭素ナノ粒子、繊維状炭素ナノ材料、層状炭素ナノ材料、炭素ナノファイバ及び酸化された炭素ナノ材料の少なくとも1つから選択される、請求項1〜3のいずれか1項に記載の強化シリコーン樹脂フィルム。
- 前記高分子層中の前記炭素ナノ材料の濃度が、該高分子層の総重量に基づき、0.001%(w/w)〜50%(w/w)である、請求項1〜4のいずれか1項に記載の強化シリコーン樹脂フィルム。
- 前記高分子層の少なくとも1つが、炭素ナノ材料及び繊維強化材の少なくとも1つから選択される強化材を含む、請求項1〜5のいずれか1項に記載の強化シリコーン樹脂フィルム。
- 前記シリコーン樹脂が、前記式(I)を有する少なくとも5mol%のジシリロキサン単位を含む、請求項1〜6のいずれか1項に記載の強化シリコーン樹脂フィルム。
- 前記シリコーン樹脂が、
(A)式[O(3−a)/2R1 aSi−SiR1 bO(3−b)/2]v(R1 3SiO1/2)w(R1 2SiO2/2)x(R1SiO3/2)y(SiO4/2)z(II)(式中、各R1は独立して、−H、ヒドロカルビル又は置換ヒドロカルビルであり、aは0、1、又は2であり、bは0、1、2又は3であり、vは0.01〜1であり、wは0〜0.84であり、xは0〜0.99であり、yは0〜0.99であり、zは0〜0.95であり、且つv+w+x+y+z=1である)を有するシリコーン樹脂、及び
(B)式O(3−a)/2R1 aSi−SiR1 bO(3−b)/2(I)(式中、各R1は独立して、−H、ヒドロカルビル又は置換ヒドロカルビルであり、aは0、1又は2であり、且つbは0、1、2又は3である)を有するジシリロキサン単位と、粒子の形状を有するシロキサン単位とを含むシリコーン樹脂
から選択される、請求項1に記載の強化シリコーン樹脂フィルム。 - 前記シリコーン樹脂(B)が、10mol%〜70mol%の、前記式(I)を有するジシリロキサン単位を含む、請求項8に記載の強化シリコーン樹脂フィルム。
- 前記シリコーン樹脂(B)中の粒子が、0.001μm〜500μmのメジアン径を有する、請求項8に記載の強化シリコーン樹脂フィルム。
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-
2008
- 2008-04-16 JP JP2010506395A patent/JP5250025B2/ja not_active Expired - Fee Related
- 2008-04-16 WO PCT/US2008/060432 patent/WO2008137262A2/en active Application Filing
- 2008-04-16 CN CN2008800143281A patent/CN101675097B/zh not_active Expired - Fee Related
- 2008-04-16 EP EP20080745939 patent/EP2142589A2/en not_active Withdrawn
- 2008-04-16 KR KR20097024955A patent/KR20100017503A/ko active IP Right Grant
- 2008-04-16 US US12/596,740 patent/US20100129625A1/en not_active Abandoned
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Publication number | Publication date |
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EP2142589A2 (en) | 2010-01-13 |
JP2010527297A (ja) | 2010-08-12 |
KR20100017503A (ko) | 2010-02-16 |
CN101675097B (zh) | 2012-03-14 |
US20100129625A1 (en) | 2010-05-27 |
WO2008137262A2 (en) | 2008-11-13 |
CN101675097A (zh) | 2010-03-17 |
WO2008137262A3 (en) | 2009-09-17 |
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