JP2015519292A - 多孔性炭素質組成物 - Google Patents
多孔性炭素質組成物 Download PDFInfo
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Abstract
Description
(1)ほとんどの石炭および石油由来ピッチは、発泡を行う前に処理が必要であり、前処理は、主に、熱処理によるピッチの重合/縮合を含む、および
(2)メソフェーズピッチは、安定化処理が必要であり、この処理をしなければ、後段の熱処理の間の膨張または軟化により発泡体構造が失われる。
(I)多孔性炭素質組成物を調製ための硬化性液体炭素前駆体配合物を用意するステップであって、(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、もしくは(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを混合することを含み、液体組成物が、ポロゲン添加前、任意成分添加前、硬化前、および炭化前に、25℃で10,000mPa−s未満の純粘度を有し、硬化される液体組成物が、組成物中に存在するポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するステップ、
(II)ステップ(I)の液体配合物を硬化し、硬化炭素前駆体組成物を形成するステップであって、硬化炭素前駆体が、組成物中に存在するポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するステップ、ならびに
(III)ステップ(II)の硬化炭素前駆体組成物を炭化して、多孔性炭素質組成物を形成するステップ、
を含む。
次の実施例は、本発明をさらに詳細に例示するが、その範囲を限定するものと解釈されるべきではない。
下記の実施例で使われている種々の用語および表記を、ここで下記により説明する。
「DVBDO」は、少なくとも95%の純度のジビニルベンゼンジオキシドを意味する。
「MPTS」は、メチルp−トルエンスルホナートを意味する。
「TGA」は、熱重量分析を意味する。
前駆体組成物の粘度の測定
本発明の硬化性液体炭素前駆体配合物の粘度を、液体試料の温度およびペルチェプレートの表面に作用する法線力の両方を制御する50mm直径平滑ステンレス鋼上部プレートおよび下部ペルチェプレートアセンブリを備えたねじりレオメータ(torsional rheometer)TA Instruments AR2000で測定した。約2mLの配合物を下部プレート上に置いた後で、2枚のプレートの間が300ミクロンのギャップになるまで上部プレートを液体配合物上に下ろした。その後、上部プレートを0.001 rad/sの名目速度で回転させ、この間に、下部プレートの温度を10℃/分の速度で25℃から65℃に上げた。TAソフトウェアで粘度を自動的に計算し、温度の関数として出力した。
炭素収率(%C)を、TA Instruments Q5000 Thermogravimetric Analyzerを使った熱重量分析により、窒素下、10℃/分の速度で25℃から1,000℃まで昇温させて測定した。「%C」を上記分析完了時のwt%炭素残渣と定義する。
この実施例1では、独立気泡多孔性炭素質組成物をThe Dow Chemical Companyから市販されている100−200Dowex(商標)1x8イオン交換樹脂であるポロゲンを使って製造した。
Claims (25)
- 多孔性炭素質組成物を調製するための硬化性液体炭素前駆体配合物であって、(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを含み、前記液体組成物が、ポロゲンの添加前、任意成分の添加前、硬化前、および炭化前に、25℃で、10,000mPa−s未満の純粘度を有し、さらに、硬化される前記液体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有する配合物。
- 前記ポロゲンが、発泡剤、分散ガス、犠牲テンプレート、中空材料、またはこれらの組み合わせを含む請求項1に記載の配合物。
- 前記発泡剤が、150℃未満の沸点を有する液体を含み、前記液体が、液体炭化水素、フルオロカーボン、クロロカーボン、クロロフルオロカーボン、およびこれらの混合物を含む請求項2に記載の配合物。
- 前記分散ガスが、20℃未満の沸点を有するガスを含み、前記分散ガスが、空気、窒素、ガス状炭化水素、二酸化炭素、およびこれらの混合物を含む請求項2に記載の配合物。
- 前記犠牲テンプレートが、600℃未満の温度で熱分解するポリマー粒子を含む請求項2に記載の配合物。
- 前記中空材料が、球、管、円柱、円板、立方体、星形、およびこれらの混合物などの任意の形状物を含む請求項2に記載の配合物。
- 前記エポキシ樹脂または前記硬化剤が、ポロゲンを含む請求項1に記載の配合物。
- 前記配合物が、無溶媒低粘度液体芳香族エポキシ樹脂を含み、前記液体芳香族エポキシ樹脂液体配合物が、少なくとも1種のジビニルアレーンジオキシドを含む請求項1に記載の配合物。
- (d)少なくとも1種の硬化触媒を含む請求項1に記載の配合物。
- 多孔性炭素質組成物を調製するための硬化炭素前駆体組成物であって、(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを含む硬化性液体炭素前駆体配合物の硬化反応生成物を含み、前記液体組成物が、ポロゲンの添加前、任意成分の添加前、硬化前、および炭化前に、25℃で、10,000mPa−s未満の純粘度を有し、さらに、硬化される前記液体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有し、および、ポロゲンおよびいずれの任意成分も存在しない場合に測定して、前記硬化炭素前駆体組成物が少なくとも35重量パーセントの炭素収率を有する硬化炭素前駆体組成物。
- 前記少なくとも1種のポロゲンが、硬化の間に気孔を生成し、硬化多孔性炭素前駆体組成物を形成する請求項10に記載の硬化炭素前駆体組成物。
- 前記少なくとも1種のポロゲンが、分散ガス、発泡剤、またはこれらの混合物を含む請求項10に記載の硬化炭素前駆体組成物。
- 多孔性炭素質組成物であって、(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを含む硬化性液体炭素前駆体配合物から調製された硬化組成物の炭化反応生成物を含み、前記液体組成物が、ポロゲンの添加前、任意成分の添加前、硬化前、および炭化前に、25℃で、10,000mPa−s未満の純粘度を有し、さらに、硬化される前記液体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有し、および、前記硬化炭素前駆体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有する多孔性炭素質組成物。
- 前記少なくとも1種のポロゲンが、炭化の間に気孔を生成し、発泡炭素質組成物を形成する請求項13に記載の多孔性炭素質組成物。
- 前記少なくとも1種のポロゲンが、犠牲テンプレートを含む請求項14に記載の多孔性炭素質組成物。
- 多孔性炭素質組成物の調製のための硬化性液体炭素前駆体配合物を調製するプロセスであって、(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、もしくは(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを混合することを含み、前記液体組成物が、ポロゲンの添加前、任意成分の添加前、硬化前、および炭化前に、25℃で、10,000mPa−s未満の純粘度を有し、さらに、硬化される前記液体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するプロセス。
- 硬化炭素前駆体組成物を調製するプロセスであって、
(I)(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、もしくは(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを混合することを含む多孔性炭素質組成物を調製するための硬化性液体炭素前駆体配合物を用意するステップであって、前記液体組成物が、ポロゲンの添加前、任意成分の添加前、硬化前、および炭化前に、25℃で、10,000mPa−s未満の純粘度を有し、さらに、前記硬化炭素前駆体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するステップ、ならびに、
(II)前記ステップ(I)の配合物を硬化させて、硬化炭素前駆体組成物を形成するステップであって、前記硬化炭素前駆体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するステップ、
を含むプロセス。 - 多孔性炭素質組成物を調製するプロセスであって、
(I)(a)少なくとも1種の芳香族エポキシ樹脂、(b)(i)少なくとも1種の芳香族共反応性硬化剤、もしくは(b)(ii)少なくとも1種の触媒硬化剤、または(b)(iii)これらの混合物、および(c)少なくとも1種のポロゲンを混合することを含む多孔性炭素質組成物を調製するための硬化性液体炭素前駆体配合物を用意するステップであって、前記液体組成物が、ポロゲンの添加前、任意成分の添加前、硬化前、および炭化前に、25℃で、10,000mPa−s未満の純粘度を有し、さらに、硬化される前記液体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するステップ、
(II)前記ステップ(I)の配合物を硬化させて、硬化炭素前駆体組成物を形成するステップであって、前記硬化炭素前駆体組成物が、前記組成物中に存在する前記ポロゲンおよびいずれの任意成分の重量にも関係なく、少なくとも35重量パーセントの炭素収率を有するステップ、ならびに、
(III)前記ステップ(II)の硬化炭素前駆体組成物を炭化して、多孔性炭素質組成物を形成するステップ、
を含むプロセス。 - 前記ステップ(II)で配合物を硬化させる前に、前記ステップ(I)の配合物を発泡させるステップを含む請求項17または請求項18に記載のプロセス。
- 前記ステップ(I)の配合物を同時に発泡および硬化させるステップを含む請求項17または請求項18に記載のプロセス。
- 前記炭化ステップ(III)の前に、前記ステップ(II)の硬化生成物に形状付与するステップを含む請求項17または請求項18に記載のプロセス。
- 前記少なくとも1種のポロゲンが、硬化、炭化、またはこれらの組み合わせの間に発泡構造体を生成する請求項18に記載のプロセス。
- 前記請求項17に記載のプロセスにより調製される硬化多孔性物品。
- 前記請求項18に記載のプロセスにより調製される炭化多孔性炭素質組成物物品。
- 熱絶縁材料を含む請求項24に記載の炭化多孔性物品。
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