JP2009524205A - ホスホン酸含有電解液 - Google Patents
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Abstract
Description
IECが1.8ミリ当量のスルホン化ポリエーテルケトンをDMSO中に溶解させる。10重量%の溶液50gを使用する。該溶液は、スルホン重合体5gを含む。そのスルホン酸基に相当するアミノホスホン酸[ジエチレントリアミノ−ペンタメチレン−ホスホン酸(DTPMP)]を溶液に加える。最大で約5g加えることができる。この例では、3g加える。そこで、アミノホスホン酸を溶解させる。ガラス板上に薄膜として、その溶液をキャストする。膜の厚さは約600μである。乾燥オーブン中約100℃の温度にて溶媒を蒸発させる。これは、確立された膜の製造方法である。溶媒を完全に除去した後、ガラス板から慎重に膜を引き離す。これは、該板が温かいままであるか又はその箔を吹付け瓶で慎重に加湿すると容易である。次いで、箔を板から引き離すことは容易である。その後、得られた箔を80%ホスホン酸中に浸漬させ、60℃の乾燥オーブンに置く。それによって、その箔は、ホスホン酸を取り入れる。ホスホン酸(PA)での後処理の後、膜は約20℃の温度でより高い温度と同等のプロトン伝導性を有する。
加熱したDMSO中に、IECが1.3ミリ当量のスルホン化ポリエーテルエーテルケトンを溶解させる。10重量%の溶液50gを使用する。該溶液は、スルホン化重合体5gを含む。そのスルホン酸基に相当するアミノホスホン酸[ジエチレン−トリアミノ−ペンタメチレン−ホスホン酸(DTPMP)]を溶液に加える。最大で約2gを加えることができ、この例では、1.5gを加える。そこで、アミノホスホン酸を溶解させる。
IECが1.8ミリ当量のスルホン化ポリエーテルケトン(SPEK)をDMSO中に溶解させる。15重量%の溶液を使用する。この溶液にスルホン酸基に相当するアミノホスホン酸[ジエチレン−トリアミノ−ペンタメチレン−ホスホン酸(DTPMP)]を加える。ガラス板上に薄膜として、その溶液をキャストする。膜の厚さは約600μである。乾燥オーブン中約100℃の温度にて溶媒を蒸発させる。これは、確立された膜の製造方法である。溶媒を完全に除去した後、ガラス板から慎重に膜を引き離す。これは、該板が温かいままであるか又はその膜を吹付け瓶で慎重に加湿すると容易である。次いで、箔を板から引き離すことは容易である。その後、得られた箔を80%ホスホン酸中に浸漬させ、60℃の乾燥オーブンに置く。それによって、その箔は、ホスホン酸を取り入れる。ホスホン酸(PA)での後処理の後、膜は約20℃の温度でより高い温度と同等のプロトン伝導性を有する。膜は、水を含み、外気から積極的に水を吸収する。プロトン伝導性は、一面では水性伝導機構に基づいており、無水状態では、取り込まれたホスホン酸に基づいている。膜がSPEK1gとDTPMP1.03gとを含む場合、そのときのアミノホスホン酸は、正確に一つの窒素原子でスルホン化重合体に結合している。ここで、二つの残存する窒素原子は、それぞれホスホン酸一分子を付ける。これは、下記に示すイオン交換容量をもたらす:SPEK=1.8、SPEK+DTPMP=9.75、SPEK+DTPMP+PA=12.83。これは、出発重合体のIECが非常に増大し、そのため、そのプロトン伝導性をも増大することを意味する。
1)PBI膜中でのATMPの固定化
厚さ60μのPBI箔(10×10cm2)を50重量%のATMP水溶液に浸漬させる。80℃で24時間、その溶液をオーブン中に置いておく。次いで、膜を取り除き、その表面をポンプで乾燥させる。
厚さ60μのPBI膜(10×10cm2)を50重量%のPA水溶液に浸漬させる。80℃で24時間、その溶液をオーブン中に置いておく。例1)のようにして、その箔を乾燥させる。
厚さ60μのPBI膜(10×10cm2)をATMPとPAの水溶液に浸漬させる。その溶液は、ATMP25重量%とPA25重量%とを含む。80℃にて24時間、その溶液をオーブン中に置いておく。例1)のようにして、膜を乾燥させる。
厚さ60μのPBI膜(10×10cm2)をATMPとPAの水溶液に浸漬させる。その溶液は、ATMP25重量%とPA25重量%とを含む。80℃にて24時間、その溶液をオーブン中に置いておく。その膜を130℃で乾燥させた後、再び上記ATMPとPAの水溶液に浸漬させる。
Claims (9)
- スルホン化重合体と塩基性ホスホン酸との溶液を製造する方法であって、
前記重合体を非プロトン性溶媒に溶解し、且つ、この溶液に前記塩基性ホスホン酸、特にアミノホスホン酸を加えることを特徴とする方法。 - 一種以上の低分子ホスホン酸とスルホン化重合体(B)との混合物(A)の少なくともいずれかを含み、そのために溶媒が非プロトン性であることを特徴とする溶液。
- 膜、粒子、塗料及び形物を製造するための請求項1又は2に記載の溶液の使用。
- 膜処理、特に燃料電池における請求項3に記載の膜の使用。
- 一種以上の低分子ホスホン酸の混合物のいずれかを含むことを特徴とするPBI膜。
- ATMP及びホスホン酸を含むことを特徴とするPBI膜。
- PBI箔を、後の工程で又は他から独立して、a)希釈若しくは濃縮したホスホン酸溶液及び/又はb)ATMPの水溶液若しくはホスホン酸溶液に浸漬させることを特徴とするPBIのドーピング方法。
- 固定化ATMP、ホスホン酸及びスルホン化ポリエーテルケトンを含むPBI膜。
- 膜、特に膜燃料電池として請求項1〜4のいずれかに記載のドープされた膜の使用。
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Application Number | Priority Date | Filing Date | Title |
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DE102006003316.7 | 2006-01-23 | ||
DE102006003316 | 2006-01-23 | ||
PCT/DE2007/000133 WO2007082526A2 (de) | 2006-01-23 | 2007-01-23 | Phosphonsäurehaltiger elektrolyt |
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JP2009524205A true JP2009524205A (ja) | 2009-06-25 |
JP2009524205A5 JP2009524205A5 (ja) | 2010-03-11 |
JP5539651B2 JP5539651B2 (ja) | 2014-07-02 |
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JP2008551646A Expired - Fee Related JP5539651B2 (ja) | 2006-01-23 | 2007-01-23 | ホスホン酸含有電解液 |
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US (2) | US9023557B2 (ja) |
EP (1) | EP1979972B1 (ja) |
JP (1) | JP5539651B2 (ja) |
AU (1) | AU2007207228A1 (ja) |
DE (1) | DE112007000226A5 (ja) |
WO (1) | WO2007082526A2 (ja) |
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JP2019534284A (ja) * | 2016-11-08 | 2019-11-28 | ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア | 臨床設定用[f−18]fddnpの複数ドーズ合成方法 |
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DE112007000280A5 (de) * | 2006-02-03 | 2008-10-30 | HÄRING, Thomas | Phosphonsäure-haltige Blends und Phosphonsäure-haltige Polymere |
CN106823824B (zh) * | 2017-01-18 | 2019-07-26 | 燕山大学 | 载带多氨基膦酸官能基团的聚醚砜功能分离膜的制备方法 |
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JP5539651B2 (ja) | 2014-07-02 |
WO2007082526A2 (de) | 2007-07-26 |
US9023557B2 (en) | 2015-05-05 |
DE112007000226A5 (de) | 2008-10-23 |
US20150232624A1 (en) | 2015-08-20 |
AU2007207228A1 (en) | 2007-07-26 |
EP1979972A2 (de) | 2008-10-15 |
US10556996B2 (en) | 2020-02-11 |
US20100047655A1 (en) | 2010-02-25 |
EP1979972B1 (de) | 2015-11-18 |
WO2007082526A3 (de) | 2008-01-24 |
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