TW398099B - Process for producing polybenzimidazole fabircs for use in fuel cells - Google Patents
Process for producing polybenzimidazole fabircs for use in fuel cells Download PDFInfo
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- H01M8/103—Polymeric electrolyte materials characterised by the chemical structure of the main chain of the ion-conducting polymer having nitrogen, e.g. sulfonated polybenzimidazoles [S-PBI], polybenzimidazoles with phosphoric acid, sulfonated polyamides [S-PA] or sulfonated polyphosphazenes [S-PPh]
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Description
經濟部中央標準局員工消費合作社印製 五、發明説明(1 發明範圍 本發明係關於製備用於燃料電池中用作爲聚合物 的織物。 Λ 發明背景 燃^池可用各種各樣的電解質,燃料及操作溫度以各 士、 土 加像虱或甲醇之類的燃料可以 接提供給燃料電池的電極。或者,然料如甲燒或甲醇 在電池本身外面轉化成富含氫的氣體混合物,然後提供 燃料電池。雖然在某些用途巾,氧是藉過氧化氫分解或自 低溫儲藏系統而得,但在大多數的燃料電池中空氣是氧氣 的來源。 T札疋乳乳 :然理論上電解質,燃料,氧化劑,溫度等有無數種 、、且口 ’但實際系統包括用氫或肼作爲燃料源及純氧作 化劑的固聚合物電解質系統。摻雜著強酸的聚苯並咪 (阳)是-個用於電解質系統之適當固體聚合物的實例 :技藝已知用強酸使聚苯並咪峻(pBI)密實薄膜吸取以 2成質子導介質。最近,美國專利第5,525,436號,(㈣ 六\月1 1曰頒予專利)描述了在PBI中摻雜強酸例如磷酸 硫酸以致形成-個單-相系統-亦即,酸溶於聚合物中 方沄。 匕既使由於本技藝有所進展,合適聚合物電解質物質 能,高成本和加工性能,就燃料電池之聚合物介質而 仍是燃料電池構造上的重要考慮。本技藝仍需要用於 燃料電池和燃料電池组件之新方法和材料。 ' ) μ 規格(2H)x7^y 可 給 的 氧 峻 或 之 的性 言, 製備 -Ί — ^--^裝·-- (請先閱讀背面之注意事項再填寫本頁)
、ST B7 五、發明说明(2 ) —方面,本發明提供一種製備用於燃料電池中作爲電解 液的聚合織物,較佳PBI織物的方法。在一具體實2例 中,該方法包含將未磺化或已磺化ΡΒ1纖維所组成的織物 浸泡在蠱性溶浚Φ。織物的孔隙係由於吸入酸之纖維膨脹 而關閉。爲了使隔膜氣密並阻止氣體在燃料電池運作時流 動穿過織物,關閉這些孔隙是必須的。 抓 另一方面,本發明提供由聚合物纖維的纖維織物,較佳 ΡΒΙ磺化或未磺化纖維所组成之織物,該織物之特徵爲具 有高酸含量及令人滿意的電化學和/或機械性能。"高酸ς 量',是指織物含有介於約40至約95重量%的吸入酸。這: 織物可以用標準的编織和針織方法製備。ΡΒΙ織物之特徵 可:比先前技藝生產出的織物具有更好的保留酸的能力: 逐有另一万面,本發明提供—種包含根據本發明之磺化 或未磺化吸酸PBI織物的燃料電池。 、 本發明的另夕卜-些方面與優點將在下面本發明較佳具體 實施例的詳細説明中加以進一步説明。 豆 發明之詳細説明 本發明提供_種對本技藝製備用在燃料電池中作爲電解 質之聚合織物之方法及對織物本身之改良。—般而言,根 據本發月’包含聚合纖維的織物係以酸溶液供其吸或浸泡 在酸中直到織物含有约40至约95重量%的酸爲止。 根據本發明’構成可用於本發明的織物的聚合纖維包 括’但不限於’聚苯並咪峻(PBI)、聚(峨淀)、 '經濟部中央標準局員工消費合作社印製 A7 —— ___B7 _ 五、發明説明(3 ) 咬)、聚咪吐、聚苯並咪唑、聚苯並噁唑、聚噁二唑、聚 喹噁啉、聚噻二唑、聚四氮芘及磺化,未磺化PBI和/或這 些聚合纖維的混合物。 目前,較佳的織物含有PBI纖維,其可磺化或未磺化。 本發明人等發現,申於PBI是一種基本聚合物,它對酸有 親合力且將在極端狀態下保留酸。特定言之,磺化織物, .比它是一種交聯織物,將比未交聯織物保留額外量的酸而 機械性能略爲降低。由於吸入的速度和製造出的織物的形 態’所以本發明的方法是很有利的。然而,既使有此優越 性’熟請本技藝者也可輕易的以包含其他聚合纖維的其他 織物取代。 、 適當的織物可以容易地從各種商業來源獲得,具較佳爲經 過編織的織物。然而,如此處所述,能吸取酸的針織或不 織織物也可以使用。 目前’本發明中所用織物的纖維宜爲小直徑,即,直徑 在約10至約500旦尼爾之範圍。更佳爲,纖維的直徑爲約 2 0旦尼爾。需要小尺寸的纖維,所得織物的厚度才會在 0.5至5密耳之範圍内。 曰 目前較佳的織物是一種經塗覆的織物,其係如同時提出 申清’同在審核中之美國專利案”製造用於燃料電池之聚 苯並咪唑霄及凝膠的方法"中所述製備,並該申請案併於 此以供參考。該聚合物織物,較佳爲可吸入酸的PBI,附 有介於0.1微米至1〇〇微米(較佳〗〇〜3〇微米)的pm膏或凝 膠塗層’且含有介於70〜99.9重量%,較佳約95〜99重量 ___ -6- 本紙張尺度適用中國國家榡準(CNS) A4規格(210X297公羞) -----r11!·:^^.裝------訂------^L--- (請先聞讀背面之注意事項#'填寫本頁} 五、發明説明(4 ) %的酸。PBI膏或凝膠是由PBI聚合物片和酸溶液混合而製 備,酸落液可讓聚合物膨脹而形成在室溫下具膏狀或凝膠 狀稠度的基體。這種方法已詳細説明於上面所述併於本文 供參考的專利申請案中。PBI膏或凝膠塗層係使用習知方 法施塗:經塗膜織物之製備已詳細説明於上述申請案中。 一旦選出合適的織物,即將織物浸入酸溶液中足夠時間 以使酸被吸入而不失去織物狀的型態。目前,較佳的酸溶 液包括溶於溶劑中的磷酸、硫酸、Triflic酸、甲磺酸及其 '昆合物。磷酸用於本發明未磺化纖維特佳。目前,最佳的 酸溶液包括磷酸和水或曱醇。然而,此酸及其他選用之其 他適當溶劑如二甲基乙醯胺和N_甲替吡咯烷酮,或這些溶 劑與水及/或曱醇的混合物,已爲熟諳本技藝者所知且可 輕易決定。 酸洛液宜含有约5至約1 00重量%的酸和約〇至約9 5重量% 的落劑。在目前的一較佳具體實施例中,酸溶液含有約 5 〇重量%酸及5 0重量%水或甲醇。 經濟部中央標準局員工消費合作社印製 在本發明方法之一具體實施例中,織物係浸入酸浴中, 在另一具體實施例中,織物和酸係在合適的混合容器中混 口。這種混合可以在室溫下進行,但在酸凝固點和沸點間 的任何溫度都可以使用。 視情況而定,將混合物加熱以能使織物吸酸比在室溫下 更快進行。宜將混合物加熱至介於約30。(:至約200°C之 間。更佳的溫度範圍爲在約50°c至約90。匸之間。加熱宜適 當地進行約3 0秒至約8小時。所要加熱時間持續約5分鐘 國家標準(CNS ) Α4» ( 210G97公釐) S98099 A7 B7 五、發明説明(5 ) 至2小時。就挑選的織物中纖維而言,例如,由未磺化 PBI纖維構成的織物可吸入少於約65%至約7〇%的酸。相 對而言,由磺化PBI纖維構成的織物係交聯者,可以吸入 大於約65%至約70%的酸而且還保持令人滿意的機械性
At Λ * * 月6 c 所得經酸浸泡之織物在室溫至約20{rc,較佳在約8(rc 至約18 0 C下烘乾,以除去殘餘溶劑如二甲基乙醯胺、 甲替吡咯烷酮、水、和/或甲醇。此一乾燥步驟將酸捕住 而形成吸取酸的織物。織物中的孔隙係藉吸取酸之纖維膨 脹而關閉,它使織物變成氣密(亦卽,氣體傳輸之有效障 〇和阻止氣體在燃料電池運流愈織物。 根據本發明之方法,所得吸取酸之織物含有高酸含量, 其量占吸酸織物重量的約40%至約95%。一般而言,爲使 織f在燃料電池中充份發揮作電解質的功能,需.要約5〇 ^ f %或更多的酸。更佳爲織物含有約5〇%至約Μ%的 酸,以吸酸織物(重量爲準。所得織物吸入的酸數量取決 於,且可藉纖維、織物、編織織物中編織之緊密度、溫 f、浸泡時間及溶液中的蜂槔度控制。以本揭示内容二 言,熟諳本技藝者可以容易地作出這些選擇和修改本發 明而仍在本發明(内。本發明方法的—個優點在於酸吸 取係在短時間範圍内發生,@先前技藝之方法則需用10 至72小時。這個優點反應在電解質成本降低性能又更 佳。 本發明的吸酸織物特別適合用在燃料電池中作爲電解 -8 - 本紙張纽顧巾_ (CNS) —_ .--^------IT (請先閲讀背面之注t事項#-填寫本瓦) 經濟部中央標準局員工消費合作社印製 經濟部中央標準局員工消費合作社印製 B9B099 五、發明酬(6 ) ' --- ^本發明㈣酸織物由於其爲織物形式很容易處理和益 2電解質中使用溶劑。再者,已發現,本發明之吸酸聚 二物織物保留酸而因此電解能力的時間比先前技藝之電解 更長久。這在本發明的吸酸織物尤其如此。因此,本發 明更進一步提供含有本發明吸酸織物之燃料電池。 以下實例將用PBI作爲代表性聚合物説明本發明之較佳 組合物和方法。這些實例僅係例證性而不限制本發明的範 圍。 复±11-未磺化PBI吸酴線舳 將未磺化PBI浸在含有8 5重量%磷酸的酸性水溶液中。 酸浸係在溫度約21τ下進行約24小時。然後,在约ΐ2〇τ 下將織物烘箱烘乾約12小時以除去殘餘的水。所得吸酸 織物含有約50重量%的酸。 重上】2 -磺化PBT叨酩繃舳 將磺化PBI織物浸在含有8 5重量%磷酸的酸性水溶液 中。酸浸係在溫度约60T下進行浸約4小時。然後,在約 120 C下將織物烘箱烘乾約i 2小時以除去殘餘的水。所得 吸酸織物含有約6 5重量%的酸/
.實例3 -吸酸和經塗膜的PBI 根據本發明的吸酸識物基本上係如上述實例i所述製 備。然而,吸酸PBI織物在用於電極總成之前也予以塗 膜。簡言之,這種織物係如下製備。 用下面方法製備的PBI膏塗覆實例i的吸酸PBI織物的兩 邊。把PBI聚合物(1克)加入到低速混合機中含有丨丨7克8 $ -9- |-裝--- (請先閲讀背面之注·意事項#填寫本頁) 訂 -T- ί r r i 一 s v '. 經濟部中央標準局員工消費合作社印製 S9B099 a? ______B7 五、發明説明(7 ) 重量%磷酸和15%水的溶液中。在升高溫度下,即在ι〇〇 °C下將混合物攪拌以除去殘餘的水直至得到均一膏。所得 骨或凝膠含有約99重量%的酸。所得每一邊塗層之厚度 爲約1密耳。在電極總.成中,與電極之接觸係藉凝膠/膏塗 層之存在促進而產生優越的燃料電池性能。 實例4 -隔膜電極總成 將由未續化PBI辩成的織物浸泡在含8 5重量%磷酸的酸 性水溶液中。此一酸泡係在溫度約60。(:下進行約4小時。 然後,織物可在約150eC下烘乾6小時以從酸處理中除去殘 餘的水。或者,把織物製造成隔膜電極總成,然後在燃料 電池中就地乾燥。所得吸酸織物含有约6 5重量%的酸。 然後製造隔膜電極總成,其法係將吸酸織物放在兩個電 極之間,並在.溫度13〇°C及壓力50公斤/平方公分下熱壓 結一段約3 0秒之時間。然後把隔膜電極放入燃料電池 中。在典型的0_7伏#換作條件下,所得電流密度及功率 密度分別爲約450毫安/平方公分及315毫瓦特/平方公分。 本發明之許多修正和變異已包括在上述已驗證的説明書 中,且預期熟讀本藝者將很明白。咸信,本發明组合物及 方法之這些修正及變化將涵蓋於随附申請專利範圍之範圍 内。 __ - 10- ^紙張尺度適用中國(CNS) A4規格(2lGx 297公·^ ----—‘--_--------丁_______ ^__S_________________ . 豸 、-贷 (請先閱讀背面之注*·事項#·填寫本頁}
Claims (1)
- 398099 ----- 六、申請專利範圍 1. —種製造吸酸聚苯並咪唑(ϊ»βι)織物之方 々成,包括以下 幾個步驟:提供包含ΡΒΙ纖維而纖維間有孔隙的織物· 及將織物浸泡在包含酸和溶劑的酸性溶液中,— —殿足夠 的時間,以使該纖維織物吸入該酸性溶液,藉以使纖維 膨脹而關閉纖維間的孔隙。 ''' 2. 根據申請專利範圍第1項之方法,其中該溶劑係自水、 甲醇、二甲基乙醯胺、Ν-甲替吡咯烷酮,及其混合物所 組成之族群中所選出。 3. 根據申請專利範圍第2項之方法’進—步包含將織物烘 乾以除去殘餘水及其他溶劑而彳吏酸濃縮至所需程度。 4. 根據申請專利範圍第1項之方法,其中該酸係自^酸、 硫酸、tnflic酸、曱磺酸、其他合適的酸,及其混合物 所组成之族群中所選出。 5·根據申請專利範圍第1項之方法,其中在該織物吸取之 酸性溶液爲介於約40至約95重量%之間,以該吸酸織 物之總重爲準。 6_根據申請專利範圍第}項之方法,其中在該織物吸取的 酸性溶液爲介於50至約75重量%之間,以該吸酸織物 之總重爲準。 7·根據申請專利範圍第1項之方法,其中在該織物吸取的 fe性溶液爲大於6 5 % ’以吸酸織物之總重量爲準。 8. 根據申請專利範圍第4項之方法,其中該酸性溶液進一 步包含介於約5至約1 〇〇重量%的酸。 9. 根據申請專利範圍第8項之方法,其中該酸性溶液進一 11 - 私紙張尺度適用中國國家標準(CNS ) Λ4規格(210X 297公釐 (請先閔讀背面之注意事哽再填寫本頁} 經濟部中央標準局員工消費合作社印製 ^---叫—裝------1T-------«線一^--^----^-I. 398099 A8 B8 C8 D8 、申請專利範圍 步包含多49 5重量%的溶劑。 10.根據申請專利範圍第9項之方法,其中該酸性溶液包含 約50%的酸和5〇%的溶劑。 11·根據申請專利範園第丄項之方法,纟中該織物是由未續 化PBI纖維所構成。 12.根據中請專利範圍第η之方法,纟中該織物是由續化 ΡΒΙ纖維所構成、 13_ —種包含酸含量介於約4〇至約95重量%之四〗織物。 14. 根據申請專利範圍第13項之織物,丨中該織物是由未 磺化ΡΒΙ纖維所構成。 15. 根據申請專利範圍第13項之織物,其中該織 化ΡΒΙ纖維所構成。 疋由令 16. —種包含Pm織物之燃料電池,該ρΒ][織物包 至約9 5重量%酸含量。(請先閱讀背面之注意事項再填寫本頁) I蠢—裝-- -----訂----^---- :線--經濟部中央標準局員工消費合作社印製 -12- 本紙張尺度it用巾國齡轉(⑽)八4驗(21〇χ297公釐
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BR (1) | BR9811507A (zh) |
CA (1) | CA2297121A1 (zh) |
DE (1) | DE69802093T2 (zh) |
ES (1) | ES2166167T3 (zh) |
TW (1) | TW398099B (zh) |
WO (1) | WO1999004444A1 (zh) |
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JP5005160B2 (ja) | 2003-12-08 | 2012-08-22 | 三星エスディアイ株式会社 | ゲル電解質及び燃料電池 |
KR100542203B1 (ko) * | 2004-06-30 | 2006-01-10 | 삼성에스디아이 주식회사 | 연료전지용 바인더 조성물, 막-전극 접합체 및 막-전극접합체의 제조방법 |
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KR100818255B1 (ko) | 2006-05-29 | 2008-04-02 | 삼성에스디아이 주식회사 | 폴리벤조옥사진계 화합물, 이를 포함한 전해질막 및 이를채용한 연료전지 |
KR101386162B1 (ko) * | 2006-07-21 | 2014-04-18 | 삼성에스디아이 주식회사 | 연료전지용 전극 및 이를 채용한 연료전지 |
KR100745741B1 (ko) | 2006-08-22 | 2007-08-02 | 삼성에스디아이 주식회사 | 연료전지용 막 전극 접합체 및 이를 채용한 연료전지 |
EP2036910B1 (en) * | 2007-09-11 | 2012-06-27 | Samsung Electronics Co., Ltd. | Benzoxazine-based monomer, polymer thereof, electrode for fuel cell including the same, electrolyte membrane for fuel cell includind the same, and fuel cell using the same |
EP2433947B1 (en) * | 2007-09-11 | 2014-05-07 | Samsung Electronics Co., Ltd. | Phosphorous containing benzoxazine-based monomer |
KR101366808B1 (ko) * | 2007-10-11 | 2014-02-25 | 삼성전자주식회사 | 폴리벤즈이미다졸-염기 복합체, 이로부터 형성된폴리벤조옥사진계 화합물의 가교체 및 이를 이용한연료전지 |
EP2357185B1 (en) | 2007-11-02 | 2014-04-23 | Samsung Electronics Co., Ltd. | Naphthoxazine Benzoxazine-Based Monomer and Polymer Thereof |
KR101537311B1 (ko) * | 2007-11-02 | 2015-07-17 | 삼성전자주식회사 | 연료전지용 전해질막 및 이를 이용한 연료전지 |
US8227138B2 (en) | 2007-11-02 | 2012-07-24 | Samsung Electronics Co., Ltd. | Phosphorus containing benzoxazine-based monomer, polymer thereof, electrode for fuel cell including the polymer, electrolyte membrane for fuel cell including the polymer, and fuel cell using the electrode |
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DK180360B1 (en) | 2019-08-14 | 2021-02-04 | Blue World Technologies Holding ApS | Method of producing separator plates by compaction and a production facility |
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CN114892341A (zh) * | 2022-05-10 | 2022-08-12 | 陕西科技大学 | 一种基于酸裂解的芳香族杂环纳米纤维薄膜及其制备方法 |
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-
1997
- 1997-07-16 US US08/895,060 patent/US6042968A/en not_active Expired - Fee Related
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1998
- 1998-05-19 WO PCT/US1998/010463 patent/WO1999004444A1/en active IP Right Grant
- 1998-05-19 EP EP98924835A patent/EP0996989B1/en not_active Expired - Lifetime
- 1998-05-19 BR BR9811507-3A patent/BR9811507A/pt not_active Application Discontinuation
- 1998-05-19 ES ES98924835T patent/ES2166167T3/es not_active Expired - Lifetime
- 1998-05-19 CN CNB988072440A patent/CN1147018C/zh not_active Expired - Fee Related
- 1998-05-19 JP JP2000503565A patent/JP4335434B2/ja not_active Expired - Fee Related
- 1998-05-19 KR KR10-2000-7000432A patent/KR100511153B1/ko not_active IP Right Cessation
- 1998-05-19 CA CA002297121A patent/CA2297121A1/en not_active Abandoned
- 1998-05-19 AT AT98924835T patent/ATE207249T1/de not_active IP Right Cessation
- 1998-05-19 DE DE69802093T patent/DE69802093T2/de not_active Expired - Lifetime
- 1998-05-19 AU AU76913/98A patent/AU7691398A/en not_active Abandoned
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Also Published As
Publication number | Publication date |
---|---|
CA2297121A1 (en) | 1999-01-28 |
ATE207249T1 (de) | 2001-11-15 |
DE69802093T2 (de) | 2003-02-13 |
KR100511153B1 (ko) | 2005-08-31 |
BR9811507A (pt) | 2000-09-26 |
CN1264501A (zh) | 2000-08-23 |
EP0996989A1 (en) | 2000-05-03 |
AU7691398A (en) | 1999-02-10 |
JP2001510879A (ja) | 2001-08-07 |
EP0996989B1 (en) | 2001-10-17 |
DE69802093D1 (de) | 2001-11-22 |
CN1147018C (zh) | 2004-04-21 |
WO1999004444A1 (en) | 1999-01-28 |
ES2166167T3 (es) | 2002-04-01 |
KR20010021868A (ko) | 2001-03-15 |
JP4335434B2 (ja) | 2009-09-30 |
US6042968A (en) | 2000-03-28 |
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