JP5500607B2 - ポリベンゾイミダゾール−ポリエーテルケトンケトンブレンド体および混和性ブレンド体 - Google Patents
ポリベンゾイミダゾール−ポリエーテルケトンケトンブレンド体および混和性ブレンド体 Download PDFInfo
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- JP5500607B2 JP5500607B2 JP2012084501A JP2012084501A JP5500607B2 JP 5500607 B2 JP5500607 B2 JP 5500607B2 JP 2012084501 A JP2012084501 A JP 2012084501A JP 2012084501 A JP2012084501 A JP 2012084501A JP 5500607 B2 JP5500607 B2 JP 5500607B2
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- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
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- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
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- ITMCEJHCFYSIIV-UHFFFAOYSA-N triflic acid Chemical compound OS(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-N 0.000 description 1
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Description
前述のことは、以下の詳細な記述と付属図面を参照することによってより容易に明白となるであろう。なお、TGAは熱重量分析のことである。
1/Tg=m1/Tg1+m2/Tg2 ただし、mはそれぞれの質量分率、または
1/Tg=w/Tg1+(1−w)/Tg2 ただし、wは重量分率
実験 311
溶液法によるPBI/PEKK比90:10の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、18グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に2グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、20グラムのPBI/PEKK比90:10のブレンド体を得た。このブレンド体は次の熱的特性を有した。二回目のDSCスキャンの結果、409℃の単一Tgを得た。窒素下におけるTdの開始温度は612℃であり、10℃/minでの10%重量損失のTdは636℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比80:20の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、16グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に4グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、14.6グラムのPBI/PEKK比80:20のブレンド体を得た。このブレンド体は次の熱的特性を有した。二回目のDSCスキャンの結果、414℃の単一Tgを得た。窒素下におけるTdの開始温度は559℃であり、10℃/minでの10%重量損失のTdは630℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比70:30の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、14グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に6グラムのPEKKを添加した。得られた混合物を1時間室温で撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、19.6グラムのPBI/PEKK比70:30のブレンド体を得た。このブレンド体は次の熱的特性を有した。二回目のDSCスキャンの結果、157℃及び418℃のTgを得た(しかし、157℃のTgは異常値であろうと思われる)。窒素下におけるTdの開始温度は529℃であり、10℃/minでの10%重量損失のTdは580℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比40:60の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、12グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に8グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、11.3グラムのPBI/PEKK比60:40のブレンド体を得た。このブレンド体は次の熱的特性を有した。二回目のDSCスキャンの結果、410℃の単一Tgを得た。窒素下におけるTdの開始温度は582℃であり、10℃/minでの10%重量損失のTdは652℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比50:50の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、10グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に10グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、19.9グラムのPBI/PEKK比50:50のブレンド体を得た。このブレンド体は次の熱的特性を有した。二回目のDSCスキャンの結果、162℃、219℃(非常に弱い中間Tg)および405℃のTgを得た。窒素下におけるTdの開始温度は559℃であり、10℃/minでの10%重量損失のTdは557℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比40:60の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、8グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に12グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、19.7グラムのPBI/PEKK比40:60のブレンド体を得た。このブレンド体は次の熱的特性を有した。二回目のDSCスキャンの結果、165℃の単一Tgを得た。窒素下におけるTdの開始温度は550℃であり、10℃/minでの10%重量損失のTdは576℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比30:70の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、6グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に14グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、19.3グラムのPBI/PEKK比30:70のブレンド体を得た。このブレンド体は木質組織および次の熱的特性を有した。二回目のDSCスキャンの結果、163℃の単一Tgを得た。窒素下におけるTdの開始温度は559℃であり、10℃/minでの10%重量損失のTdは570℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比20:80の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、4グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に16グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、19.3グラムのPBI/PEKK比20:80のブレンド体を得た。このブレンド体は木質組織および次の熱的特性を有した。二回目のDSCスキャンの結果、159.5℃の単一Tgを得た。窒素下におけるTdの開始温度は559℃であり、10℃/minでの10%重量損失のTdは568℃であった。(Td=分解温度)
溶液法によるPBI/PEKK比10:90の調製
4つのブレードを持つガラス製メカニカルスターラーと窒素吸気口及び排気口を装備した500ml三口樹脂フラスコの中に、2グラムのPBI100と180グラムの96%硫酸を添加した。この混合物を60℃で1時間撹拌してPBIを溶解し、室温まで冷却した。冷却したPBI溶液に18グラムのPEKKを添加した。得られた混合物を室温で1時間撹拌し、これを1リットルの水の中にワーリングブレンダーで高速撹拌しながら注入し、次にこれを濾過して高分子ブレンド体を回収した。このブレンド体を水で洗浄し、水酸化アンモニウムで中和し、濾過し、水で再洗浄し、次に120℃真空下で一晩かけて乾燥し、20.9グラムのPBI/PEKK比10:90のブレンド体を得た。このブレンド体は木質組織および次の熱的特性を有した。二回目のDSCスキャンの結果、163.5℃の単一Tgを得た。窒素下におけるTdの開始温度は559℃であり、10℃/minでの10%重量損失のTdは568℃であった。(Td=分解温度)
Claims (4)
- ポリベンゾイミダゾール(PBI)とポリエーテルケトンケトン(PEKK)を用意する工程と、
複数の加熱帯を有する押出機を用意する工程と、
前記PBIを前記PEKKと予乾燥混合して乾燥混合物を得る工程と、
前記乾燥混合物を前記押出機に送出する工程と、
前記加熱帯を240℃から410℃の範囲に設定する工程と、
前記乾燥混合物ブレンド体を前記押出機に通過させて溶融する工程と、
PBI/PEKK比が60:40から80:20までの任意の比率のPBI/PEKK比を持つPBIとPEKKの溶融ブレンド体を得る工程と
を含む、ポリベンゾイミダゾール(PBI)とポリエーテルケトンケトン(PEKK)の溶融ブレンド体を製造する製法。 - 前記押出機は、スクリューが30〜160rpmの範囲で稼働されるスクリュー押出機であることを特徴とする、請求項1に記載のポリベンゾイミダゾール(PBI)とポリエーテルケトンケトン(PEKK)の溶融ブレンド体を製造する製法。
- 前記ブレンド体は、60:40から80:20のPBI/PEKK比の範囲において、600℃での重量損失が20%未満であることを特徴とする、請求項1又は2に記載の製法により作られたポリベンゾイミダゾール(PBI)とポリエーテルケトンケトン(PEKK)の混和性ブレンド体。
- 前記ブレンド体は60:40から80:20のPBI/PEKK比を有し、前記ブレンド体は400℃より高いガラス転移温度Tgを有することを特徴とする、請求項1又は2に記載の製法により作られたポリベンゾイミダゾール(PBI)とポリエーテルケトンケトン(PEKK)の混和性ブレンド体。
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EP2957586B1 (en) | 2020-12-02 |
JP6192572B2 (ja) | 2017-09-06 |
JP2010518196A (ja) | 2010-05-27 |
US20080185751A1 (en) | 2008-08-07 |
US7915351B2 (en) | 2011-03-29 |
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US20100305277A1 (en) | 2010-12-02 |
JP2014098170A (ja) | 2014-05-29 |
JP5296710B2 (ja) | 2013-09-25 |
EP2957586A1 (en) | 2015-12-23 |
US9156983B2 (en) | 2015-10-13 |
WO2008097709A1 (en) | 2008-08-14 |
US8802789B2 (en) | 2014-08-12 |
US8309662B2 (en) | 2012-11-13 |
US20140309377A1 (en) | 2014-10-16 |
JP2012126922A (ja) | 2012-07-05 |
US20130035454A1 (en) | 2013-02-07 |
EP2109633B1 (en) | 2015-10-07 |
EP2109633A1 (en) | 2009-10-21 |
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