JP2014506830A - アミド化された表面を有するポリイミドナノウェブを用いたろ過方法およびそのための装置 - Google Patents
アミド化された表面を有するポリイミドナノウェブを用いたろ過方法およびそのための装置 Download PDFInfo
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- JP2014506830A JP2014506830A JP2013543271A JP2013543271A JP2014506830A JP 2014506830 A JP2014506830 A JP 2014506830A JP 2013543271 A JP2013543271 A JP 2013543271A JP 2013543271 A JP2013543271 A JP 2013543271A JP 2014506830 A JP2014506830 A JP 2014506830A
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- nanoweb
- aromatic polyimide
- polyimide
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- 239000001301 oxygen Substances 0.000 claims description 34
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Abstract
Description
第1の金属製集電器を含む第1の層と;
第1の金属製集電器と接着して接触する、第1の電極材料を含む第2の層と;
第1の電極材料と接着して接触する、芳香族ポリイミドナノウェブを含む第3の層であって、前記ナノウェブが、自由表面積を有し、その少なくとも一部が、ヒドロカルビル基を含む官能基を含む第二級アミドを含む第3の層と、
芳香族ポリイミドナノウェブと接着して接触する、第2の電極材料を含む第4の層と;
第2の電極材料と接着して接触する、第2の金属製集電器を含む第5の層とを含む。
ポリマーの製造
[HMT E115199−39PI=ポリマー21109、紡糸SF44P1DBX001D15IR20IM501]
DMF溶媒中のPMDAおよびODAのポリアミド酸を、過剰なODAを用いて業界標準方法にしたがって製造して、97%の化学量論量および23重量%の固体を得た。ポリアミド酸を、0.04重量%の無水フタル酸(末端封止剤の重量%を確認する必要がある)で末端封止した。
そのように製造されたPAA溶液を、図7に示される装置に充填した。図7は、好適なエレクトロブロー装置の一実施形態を示す。34℃の温度および55℃のプロセスガス温度および5833メートル/分の速度で、5.5バールの溶液圧力で(本発明者らの仮特許出願に)記載されるエレクトロブロープロセスにしたがって、ポリアミド酸溶液を紡糸してナノ繊維ウェブにした。得られたナノウェブは、63%の多孔率で厚さ21〜26ミクロンであった。
それぞれ重さ約35mgの、そのように製造されたポリイミドナノ繊維ウェブの8つの試料を、加熱マントルが装着されたPyrex(登録商標)容器中で、窒素下で、100mLの無水N,Nジメチルホルムアミド(DMF)(Aldrich 227056)に溶解させた5.0gmのオクタデシルアミン(Aldrich 305391)の予め加熱された溶液に加えた。表1に示される各期間の後、示される溶液温度で、1つの試料を取り出し、トルエン中で4回すすぎ、真空オーブン中、減圧下で95℃で1時間乾燥させた。未処理の出発材料の試料を比較のために確保した。
5gのn−ドデシルアミンを、100mLのDMF溶媒に溶解させた。実施例1のポリイミドナノウェブの試料を、50℃でそれぞれ1時間および20時間の期間にわたって溶液中に浸漬した。試料を同時に浸漬させ、異なる時間間隔の後に取り出し、次に、イソプロパノールで3回すすいだ。走査電子顕微鏡法は、未反応の対照と比べて繊維形態の変化を示さなかった。
DMF中のn−ヘキサデシルアミンの5重量%溶液を製造した。実施例1のポリイミドナノウェブの試料を、それぞれ1時間および20時間の期間にわたって50℃で溶液中に浸漬し、次に、イソプロパノールで3回すすいだ。走査電子顕微鏡法は、未反応の対照と比べて繊維形態の変化を示さなかった。拡散反射赤外分光法は、脂肪族基を確認する2852および2919cm−1における吸収ピークを示した。1545、1650および3267cm−1におけるピークにより、第二級アミド基が確認された。反応生成物の赤外線スペクトルは、元のポリイミドの1700および1500cm−1における強い吸収ピークを保ち、これは、アミド化反応が主にナノ繊維の表面上のポリマーの薄層に限定されることを示唆していた。
2つの1インチ×3インチ幅のストリップを、実施例10〜13のアミド化されたナノウェブのそれぞれから切断し、真空チャンバ中、90℃で一晩乾燥させた。このように乾燥された試験片を、電気化学的コイン電池中に組み込んだ。
ポリ(アミド酸)溶液2(PAA2)
97%の化学量論量および23.5重量%の固体で、DMF中のPMDA/ODAのポリアミド酸を製造した。アミド酸を、0.04重量%の無水フタル酸で末端封止した(確認する必要がある)。
そのように製造されたPAA溶液を、図7に示される装置に充填した。図7は、好適なエレクトロブロー装置の一実施形態を示す。37℃の温度および72℃のプロセスガス温度および5833メートル/分の速度で、5.5バールの溶液圧力で、(本発明者らの仮特許出願に)記載されるエレクトロブロープロセスにしたがって、ポリアミド酸溶液を紡糸してナノ繊維ウェブにした。
このように形成されるナノウェブの2×2インチ試料をイミド化し、空気対流炉中、350℃で2分間、および450℃で2分間アニーリングした。このようにイミド化され、アニーリングされた試料を、10mLの塩化メチレンとともに20mLのガラスシンチレーションバイアルに入れ、Branson超音波浴中で15分間超音波処理した。このように超音波処理された試料を取り出し、窒素下で、真空オーブン中、100℃で10分間、窒素下で乾燥させた。
実施例18の0.06Mのヒスタミン溶液の代わりにエタノール中のN,N−ジエチルエチレンジアミン(Aldrich)の0.086Mの溶液を用いたことを除いて、実施例18の手順を、実施例18のナノウェブのさらなる2×2インチ試料を用いて繰り返した。アミド化された表面生成物の存在を、2920cm−1および2850cm−1における特性吸収の存在によって、減衰全反射(ATR)アタッチメントを用いたFTIR分析によって確認した。N,N−ジエチルエチレンジアミンで処理された試料は、0°の静的水接触角を示した。
実施例18の0.06Mのヒスタミン溶液の代わりに、エタノール中のヘキサメチレンジアミン(Aldrich)の0.05Mの溶液を用い、浸漬時間が実施例18の1時間の代わりに20時間であったことを除いて、実施例18の手順を、実施例18のナノウェブのさらなる2×2インチ試料を用いて繰り返した。アミド化された表面生成物の存在を、実施例18と同様に、FTIR分析によって確認した。接触角の分析も行った。ヘキサメチレンジアミンで処理された試料は、0°の静的水接触角を示した。
それぞれ実施例18、19および20にしたがって製造されたアミド化されたナノウェブ試料のそれぞれの1つの6mg(約2cm×2cm)のアリコート、ならびに正規化された対照の6mgのアリコートを、個々に、2mLのパスツールピペットに充填した。脱イオン水の0.20mLのアリコートを各ピペットに加え、水が、ナノウェブが充填されたカラムを通過するのに必要な時間を記録した。24時間後、水は、対照試料を保持するピペットを通過していなかった。水は、実施例18、19、および20において製造された材料が充填されたピペットを、10分間以内に完全に通過した。
Claims (15)
- 固体と流体との混合物を、表面改質ポリイミドナノウェブの表面に湿式に衝突させて、前記混合物の流体富化部分が前記表面改質ポリイミドナノウェブを通って輸送される一方、前記混合物の固体富化部分が輸送されないようにする工程を含むろ過方法であって;前記表面改質ポリイミドナノウェブが、芳香族ポリイミドのナノ繊維を含むナノウェブを含み、前記ナノウェブが、自由表面積を有し、その少なくとも一部が、炭化水素基を含む官能基を含む第二級アミドを含む方法。
- 前記官能基が、酸素、硫黄または窒素を含む官能基をさらに含む、請求項1に記載の方法。
- 前記官能基がアミンである、請求項2に記載の方法。
- 前記ナノ繊維が、50〜500ナノメートルの範囲の数平均直径を特徴とする、請求項1に記載の方法。
- 前記ナノ繊維が、100〜400ナノメートルの範囲の数平均直径を特徴とする、請求項4に記載の方法。
- 前記炭化水素基が飽和炭化水素基である、請求項1に記載の方法。
- 前記飽和炭化水素基がアルキル基である、請求項6に記載の方法。
- 前記アルキル基がn−アルキル基である、請求項7に記載の方法。
- 前記n−アルキル基が、15〜20個の炭素原子を有する、請求項8に記載の方法。
- 前記芳香族ポリイミドが全芳香族ポリイミドである、請求項1に記載の方法。
- ろ過される混合物を導入するための第1のポートと、ろ液を排出するための第2のポートとを備えたハウジングを含む装置であって、前記ハウジングが、表面改質芳香族ポリイミドナノウェブを含み、前記表面改質芳香族ポリイミドナノウェブは、前記混合物の流体富化部分が前記表面改質ポリイミドナノウェブを通って輸送される一方、前記混合物の固体富化部分が輸送されないように、ろ過される前記混合物がその前記表面に湿式に衝突するように内部に封止的に配置され;前記表面改質ポリイミドナノウェブが、芳香族ポリイミドのナノ繊維を含むナノウェブを含み、前記ナノウェブが、自由表面積を有し、その少なくとも一部が、炭化水素基を含む官能基を含む第二級アミドを含む装置。
- 前記官能基が、酸素、硫黄または窒素を含む官能基をさらに含む、請求項11に記載の装置。
- 前記官能基がアミンである、請求項12に記載の物品。
- 前記ナノ繊維が、50〜500ナノメートルの範囲の数平均直径を特徴とする、請求項11に記載の装置。
- 前記芳香族ポリイミドが全芳香族ポリイミドである、請求項11に記載の装置。
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US20140008210A1 (en) * | 2012-07-06 | 2014-01-09 | Aviva Biosciences Corporation | Methods and compositions for separating or enriching cells |
US20130130126A1 (en) * | 2011-10-12 | 2013-05-23 | Giner, Inc. | Electrochemical cell for high-voltage operation and electrode coatings for use in the same |
US8679200B2 (en) | 2011-11-18 | 2014-03-25 | E I Du Pont De Nemours And Company | Method for reducing self discharge in an electrochemical cell |
US10707526B2 (en) | 2015-03-27 | 2020-07-07 | New Dominion Enterprises Inc. | All-inorganic solvents for electrolytes |
US10707531B1 (en) | 2016-09-27 | 2020-07-07 | New Dominion Enterprises Inc. | All-inorganic solvents for electrolytes |
CN111921315A (zh) * | 2020-07-13 | 2020-11-13 | 陈刚 | 一种气液分离用捕雾器 |
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Also Published As
Publication number | Publication date |
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CN103249469A (zh) | 2013-08-14 |
CN103249469B (zh) | 2016-04-27 |
TW201226045A (en) | 2012-07-01 |
KR20140005917A (ko) | 2014-01-15 |
US20110139730A1 (en) | 2011-06-16 |
WO2012078627A3 (en) | 2012-10-04 |
EP2648830A2 (en) | 2013-10-16 |
KR101943667B1 (ko) | 2019-01-29 |
WO2012078627A2 (en) | 2012-06-14 |
EP2648830A4 (en) | 2017-04-05 |
US9475009B2 (en) | 2016-10-25 |
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