TW201311936A - 氣體擴散電極及其製法和電化電解池 - Google Patents
氣體擴散電極及其製法和電化電解池 Download PDFInfo
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- 238000009792 diffusion process Methods 0.000 title claims abstract description 84
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- 229910052799 carbon Inorganic materials 0.000 claims description 14
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- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001257 hydrogen Substances 0.000 claims description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
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- 229910052709 silver Inorganic materials 0.000 description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 239000011701 zinc Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 229910021641 deionized water Inorganic materials 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 125000006850 spacer group Chemical group 0.000 description 3
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
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- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
- C25B11/032—Gas diffusion electrodes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/46—Apparatus therefor
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Abstract
本發明係關於一種氣體擴散電極,設備燒結並鑄造之氣體擴散層,具有高度彈性模數。電極可用做去極電解池,諸如電解冶金、氯鹼或電透析電池之耗氫陽極或耗氧陰極。
Description
本發明係關於氣體擴散電極結構,適合做為電解池內之耗氣陽極或陰極。
氣體擴散電極之使用,已見於若干電化製法,尤其是去極電解製法,不論用做耗氫陽極或耗氧陰極,以及在燃料電池應用方面。氣體擴散電極通常由多孔性氣體擴散薄層構成,設備疏水性途徑,供氣體傳送越過其厚度,另視需要具備觸媒,嵌入或積層於集流構件上。集流構件亦可做為強化構件,視最後用途而定。集流構件之例為拉張或編製金屬、金屬發泡體、編製或標準碳布或金屬布或毡、碳紙。氣體擴散層可由視需要經觸媒催化之導電性粉體,例如金屬、氧化物或碳粉,加上粘合劑,通常為能夠形成適當網路以獲取導電性粉體的塑膠材料,所得多孔性固體組成物所組成。氣體擴散層並非自立構件,通常是利用各種技術,例如噴塗組成份之水性懸浮液,或利用凹版塗佈或刮塗水性漿液或糊劑,形成於集流構件上。氣體擴散層亦可在惰性載體上形成印圖,與集流構件積層後,利用剝離或瀝濾除去;另外形成氣體擴散層,隨後積層,為非常繁複之作業,氣體擴散層通常很薄而脆,難以處置。氣體擴散電極可有觸媒,加入到氣體擴散層內,或在氣體擴散層頂面,通常是在集流構件相反側,施加適當觸媒層,加以催化。此種構造導致薄電極構件維度界定和剛性不佳,必須利用適當間隔物和集流器充分支持,此為技術上所公知。
氣體擴散電極可用來去極化電化製法;例如氯鹼電解之進行,可藉氧加料至氣體擴散陰極,而非在金屬陰極釋出氣態氫,相關能量節省約30%。然而,在氯鹼電池內之耗氧陰極,必須面對一邊是氣體室,另一邊是液體電解質室,在此生成苛性溶液。已知氣體擴散電極無法承受工業用電解池
(即總高度超過30公分者)內苛性溶液生成物之液體落差,只能利用氣體室加壓補救到某一程度。液柱所施壓力事實上在底部比在頂部高,除非採取使電池設計變得複雜的特殊抗衡措施,諸如WO 03035939很麻煩的氣袋設計,不但所費不貲,而且不太可靠,或者如WO 03042430所揭載之濾萃器型電池。濾萃器構件可有效打破液體室內之液體落差,另方面,價格昂貴,對電池構造增加不需要的電阻降。濾萃器事實上由某些充填液體電解質的最小厚度之多孔性體組成,同時在需要時可作為氣體擴散電極和隔膜分離器間之間隔物,以補救氣體擴散電極維度界定和剛性不良,後者致使其不適於限定充分低厚度的明確間隙室。
另外在電冶應用上,諸如金屬電解冶金,可因在此情況下,於陽極側之製法去極化關聯的節省能源而獲益,金屬電極沉積事實上是適當電解池之陰極側進行,在陽極釋出氧。在適當氣體擴散電極以氫的氧化取代釋氧,會得到很高的能量節省,但因已知氣體擴散電極之機械特性,難以做到,以致不適於區隔窄間隙室,如此限制其用在電冶製法典型之不區分電解池。此外,在此情況下,已知氣體擴散電極亦不能夠承受工業用電解池常用的電解溶液之液體落差。
所以,亟需提供改進機械特性之氣體擴散電極,適於做為自立構件作業,構造公差小,有充分剛性,以區分電解池之窄間隙室,能夠提供液體靜力障壁,適於承受工業電解池典型之液體落差,例如20 kPa或以上。
本發明諸項要旨規範在所附申請專利範圍內。
本發明一要旨係關於一種具有高度彈性模數之氣體擴散電極,包括積層之強化構件上之氣體擴散層,尤指由燒結並鑄造之導電性粉體/氟化粘合劑組成物組成之氣體擴散層,積層氣體擴散層/強化構件總成之縱向(在平面內)彈性模數至少10,000 MPa;在一具體例中,氣體擴散層/強化構件
總成之縱向彈性模數在15,000至120,000 MPa之範圍內。在一具體例中,氣體擴散層之垂直(超出平面)彈性模數超過500 MPa。本發明人等發現,在可得橡膠狀氣體擴散層之條件下,鑄造含氟化粘合劑之預燒結組成物,使氣體擴散電極對所得電極賦予高度彈性模數,使其能夠承受極高液體落差(例如液體落差超過20 kPa,諸如80 kPa),並區分電解池內明確之間隙室,中間不需間隔物元件。在一具體例中,氣體擴散電極之強化構件,選自拉張或編製金屬、金屬泡沫體、碳或金屬布或毡,都能承受製法中之燒結和鑄造步驟。此優點是進一步增進所得氣體擴散電極之剛性和維度界定。在次佳具體例中,亦可使用碳紙,若經適當選擇製造條件。在一具體例中,氣體擴散層之燒結和鑄造組成物,含碳黑做為導電性粉體,例如低表面碳黑,諸如Shawinigan乙炔黑(SAB)。此優點是具有適當結實和導電性層。在一具體例中,燒結並鑄造組成物內之氟化粘合劑,係全氟粘合劑,諸如PTFE、FEP或PFA。此優點是提供在電解質環境內增進穩定性之氣體擴散電極,且在中等壓力和溫度條件下,方便達成橡膠狀氣體擴散層。在一具體例中,把燒結並鑄造的組成份內碳粉與氟化粘合劑重量比設定在1和2之間,即可得適當兼備之機械和電氣性能。在一具體例中,氣體擴散電極在強化構件對立側面,按上述在氣體擴散層上澱積觸媒層,即可加以催化。有數類觸媒層可聯結於燒結和鑄造之氣體擴散層:在一具體例中,從分散於液體離聚物懸浮液或溶液內觸媒粉體開始,可得觸媒層,做為再鑄造離聚物層。此優點是,對氣體擴散電極賦予離子導電性和親水性質,可用於若干用途。在另一具體例中,觸媒層亦由燒結和鑄造組成物組成,諸如燒結和鑄造碳承載觸媒粉體/氟化粘合劑組成物,積層於氣體擴散層上。此優點是,更加增進氣體擴散電極之維度界定和剛性。
本發明另一要旨,係關於上述氣體擴散電極之製法,包
括步驟為:於糊劑內添加氟化粘合劑和導電性粉體,例如從氟化粘合劑水性懸浮液或乳化液開始,以適當化學劑,諸如輕質醇,使粘合劑沉析,把沉析之粘合劑與碳黑等導電性粉末混合;把糊劑軋光成薄層,例如厚度低於2 mm,在一具體例中,低於0.2 mm;把各層在加熱壓機於100-150℃和壓力12-24 kPa下,積層於強化構件上,直到獲得積層結構,於一具體例中,需15-60分鐘;加溫至300-400℃,調壓至25-50 kPa,直到除去水性相,在一具體例中,各需15-60分鐘;放壓至大氣壓力,在鬆弛條件下引起完全燒結,其優點為使氣體擴散層緊密粘合於強化構件,在一具體例中,需1-15分鐘;把已燒結結構在加熱壓機於300-400℃和壓力30-60 kPa下鑄造,直到鑄成橡膠狀氣體擴散層,對總成賦予高度縱向彈性模數,在一具體例中,需15-60分鐘。
本發明又一要旨係關於一種電化電解池,包括氣體室和液體室,按前述以氣體擴散電極分開;氣體擴散電極可作為氣體擴散陽極,在其表面把含氫流動氧化,或作為氣體擴散陰極,在其表面把含氧流動,諸如純氧或空氣還原。在一具體例中,以氣體擴散電極與氣體室分開的液體室內,確立液體落差為20 kPa或以上,其優點是增進氣體擴散層能力,以承受液柱不氾流的壓力。本發明電解池可為氫去極化電解冶金電池,氧去極化氯鹼電池,在任一側或兩側塩分裂去極化用之電透析電池(即設有進料氫之氣體擴散陽極和/或進料氧之氣體擴散陰極,一如前述),惟其他類型之電解池或燃料電池,諸如鹼性燃料電池,亦具有上述氣體擴散電極之優點,自為技術專家明顯可知。
以下實施例包含在內,以證明本發明特殊具體例,其實施性在申請專利範圍數值內大大獲得證實。凡技術專家均知,下述實施例內揭示之組成物和技術,代表本發明人等發現在本發明實務上有充分功能之組成物和技術;惟技術專家均知鑒於本案內容,在所揭示特殊具體例內可做許多改變,仍可得同樣或類似結果,不違本發明之範圍。
取美國杜邦公司商業化的PTFE水性懸浮液,沉析入2-丙醇和脫離子水50:50容量混合液內。沉析之PTFE以機械方式混合於美國Cabot Corp.商業化之Shawinigan乙炔黑(SBA),碳對PTFE之重量比為60:40。得麵糰稠度之材料,立即經擠製機,使用軋輥處理成10 cm×10 cm×0.1 mm層。各層利用加熱壓機,積層在編製銀網之不同樣本上,網之孔寬0.50 mm,線徑0.14 mm,比重0.53 kg/m2;製程以多步驟進行,先把總成在17.9 kPa和120℃加壓30分鐘,再調溫至335℃,升壓到44.8 kPa,再經30分鐘,釋壓,把積層結構暴露於周圍空氣,經5分鐘,最後再將總成在34.5 kPa和335℃加壓,又經30分鐘。
所得全部樣本利用動態機械分析(DMA)測量縱向(在平面內)彈性模數,在35,000至49,000 MPa範圍。
重複實施例1之程序,使用日本Toray商業化之280 μm厚TGP-H-090碳紙,做為強化構件。按照實施例1軋光,得SAB/PTFE層,積層於各碳紙樣本;製程分多步驟進行,先將總成在13.7 kPa和120℃加壓30分鐘,再調溫至335℃,升壓至27.5 kPa,再經30分鐘,釋壓,把積層結構暴露於周圍空氣,經5分鐘,最後將總成在34.5 kPa和335℃再加壓,又經30分鐘。
所得全部樣本利用動態機械分析(DMA)測量縱向(在
平面內)彈性模數,在16,000至23,000 MPa範圍。
重複實施例1和2之程序,使用美國Textron Systems Corporation商業化之0.75 mm厚AvCarbTM 1243碳布,做為強化構件。按照前述實施例軋光而得SAB/PTFE層,並積層於各碳布樣本上;製程分多步驟進行,先將總成在20 kPa和120℃加壓30分鐘,再調溫至335℃,升壓至45.5 kPa,再經30分鐘,釋壓,把積層結構暴露於周圍空氣,經5分鐘,最後將總成在55 kPa和335℃再加壓,又經30分鐘。
所得全部樣本利用動態機械分析(DMA)測量縱向(在平面內)彈性模數,在45,000至73,000 MPa範圍。
取實施例1所得一氣體擴散電極,在銀網強化構件上,和實施例3所得一氣體擴散電極,在碳布強化構件上,在燒杯做成的實驗裝置內,有直徑8 cm的開口,用做加壓面積,在加壓下測試透氣率。
把金屬圈環和細網放入燒杯內,做為電極樣本之支座。圈環/網插件要與燒杯邊緣齊平,以防電極樣本有任何重大折曲,置放在燒杯邊緣供測試,介置以2 mm橡膠墊片。取第二個燒杯夾在總成頂部,也介置以橡膠墊片。頂部燒杯在密封之前,放約5 cc的水。使用真空泵從底部燒杯除去空氣,同時監視壓力,遞增約7 kPa時暫停,保持壓力,檢查洩漏,直到最大壓力約80 kPa,此為實驗裝置可達之最大值。
實施例1樣本(以銀網強化)能夠承受壓力20 kPa,而實施例3樣本(以碳布強化)直到施壓約80 kPa,未見任何洩漏。
裝設習用鉛銀(Pb0.75Ag)陽極板和鋁陰極之實驗用電解冶金電池,有50 cm2活性面積,1 cm間隙,用於測試從高
純度ZnO和試劑級硫酸溶解於脫離子水內所得,含50 g/l Zn和170 g/l H2SO4之硫酸塩電解質,沉積鋅,反應式如下:2 ZnSO4+2 H2O → 2 H2SO4+2 Zn+O2在500 A/m2和電池總電壓3.1 V進行測試。
取實施例3之一電極樣本,在碳布構件的相反面,以含有分散於美國Aldrich商業化液體Nation懸浮液的Vulcan XC-72碳黑所承載Pt觸媒之印墨塗刷,得氣體擴散電極。塗過的電極樣本在125℃乾燥,在其表面再鑄含觸媒之離聚物膜。
實驗用電解冶金電池之鉛銀陽極,改換如此製得之催化氣體擴散電極,安裝於適當框架內,催化表面朝向陰極,有1 cm間隙。氣體擴散電極從背側供以純氫氣,繼續鋅之電解冶金製程。發現在電流密度500 A/m2,電池電壓降850 mV。電池操作過夜無短路之問題。
按實施例1製得氣體擴散電極,惟氣體擴散層在銀網構件相反面,共同積層1 mm厚觸媒層,其製程是把同樣PTFE水性懸浮液,沉析入2-丙醇和脫離子水50:50容量混合液內,把沉析的PTFE與銀粉以機械方式混合,並以機械方式摻入5%重量鉑粉,使Ag-Pt對PTFE重量比為80:20,將所得糊劑以軋輥擠製。積層、燒結合鑄造步驟,按照實施例1進行,即得氣體擴散電極,縱向(在平面內)彈性模數為41,000 MPa。
把所得電極按照WO 03042430之實施例1和第1圖,組裝成為實驗用氯鹼電池內之氣體擴散陰極(10)、無多孔性平坦元件(9),而陰極(10)與隔膜(16)間隙為1 mm。電池可在400安培(4000 A/m2)、電池電壓2.4 V(比先前技術的低彈性模數之氣體擴散陰極可得最佳電池壓約低200 mV,陰極和隔膜間介置塑性濾萃元件),作業過夜,製成32%重量
苛性鈉。
前述無意限制發明,可按照不同具體例使用,不違其範圍,且其程度純以所附申請專利範圍為準。
本案說明書和申請專利範圍內使「包括」字眼,並不排除其他元件或添加劑的存在。
本說明書提到文件、規定、材料、裝置、文章等,其目的純為提供本發明之文脈,並非主張或代表任何或全部此等事項形成先前技術基礎之一部份,或是本發明相關領域在本案各項申請專利範圍在優先權之前的一般常識。
Claims (14)
- 一種氣體擴散電極,包括氣體擴散層,積層於強化構件上,該氣體擴散層係由燒結並鑄造導電性粉體/氟化粘合劑組成物所組成,氣體擴散層/強化構件總成之縱向彈性模數為至少10,000 MPa者。
- 如申請專利範圍第1項之氣體擴散電極,其中該氣體擴散層/強化構件總成之縱向彈性模數在15,000至120,000 MPa範圍內者。
- 如申請專利範圍第1或2項之氣體擴散電極,其中該強化構件係選自包含拉張金屬、編製金屬、金屬泡沫體、碳或金屬布或毡材料之組群者。
- 如前述申請專利範圍任一項之氣體擴散電極,其中該組成物內之該導電性粉體係碳黑者。
- 如前述申請專利範圍任一項之氣體擴散電極,其中該組成物內之該氟化粘合劑係PTFE、PFA或FEP者。
- 如申請專利範圍第4或5項之氣體擴散電極,其中該組成物內之碳粉體對氟化粘合劑之重量比在1至2範圍者。
- 如前述申請專利範圍任一項之氣體擴散電極,又包括觸媒,澱積在該氣體擴散層上,於該強化構件相反側者。
- 如申請專利範圍第7項之氣體擴散電極,其中該觸媒層係由含觸媒粉體之重鑄離聚物層組成者。
- 如申請專利範圍第7項之氣體擴散電極,其中該觸媒層係積層於該氣體擴散層上的燒結並鑄造之碳承載觸媒粉體/氟化粘合劑組成物所組成者。
- 一種如申請專利範圍第1至9項任一項氣體擴散電極之製法,包括步驟為:a.取得糊劑,包括氟化粘合劑和導電性粉體;b.把該糊劑軋光成厚度在2 mm以下之諸層;c.把該諸層在加熱壓機下,於溫度100至150℃和壓力12至24 kPa,積層於強化構件,得積層結構; d.調溫至300-400℃,並升壓至25-50 kPa;e.釋壓至大氣壓力,把積層結構暴露於空氣,引起燒結;f.把燒結結構在加熱壓機下,於溫度300-400℃和壓力30-60 kPa鑄造者。
- 如申請專利範圍第10項之方法,其中該步驟c,d,f為時15至60分鐘,而在步驟e之該暴露於大氣壓力空氣為時1至15分鐘者。
- 一種電化電解池,包括至少一氣體室和一液體室,以申請專利範圍第1至9項任一項之氣體擴散電極分開,氣體室為在該氣體擴散電極表面將氫流動氧化之陽極室,或在該氣體擴散電極表面將氧流動還原之陰極室者。
- 如申請專利範圍第12項之電化電解池,其中在該液體室內建立液體落差至少20 kPa者。
- 如申請專利範圍第12或13項之電解池,選自包含氫去極化電解冶金電池、氧去極化氯鹼電池、去極化電透析電池和燃料電池之組群者。
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- 2012-09-13 ES ES12761592T patent/ES2745508T3/es active Active
- 2012-09-13 DK DK12761592.0T patent/DK2756113T3/da active
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- 2012-09-13 US US14/342,887 patent/US20140227634A1/en not_active Abandoned
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- 2012-09-13 WO PCT/EP2012/067974 patent/WO2013037902A2/en active Application Filing
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EA027322B1 (ru) | 2017-07-31 |
US20140227634A1 (en) | 2014-08-14 |
HUE045380T2 (hu) | 2019-12-30 |
KR20140061412A (ko) | 2014-05-21 |
PT2756113T (pt) | 2019-09-30 |
ES2745508T3 (es) | 2020-03-02 |
PL2756113T3 (pl) | 2019-12-31 |
JP2014531513A (ja) | 2014-11-27 |
JP6220337B2 (ja) | 2017-10-25 |
EA201490334A1 (ru) | 2014-06-30 |
DK2756113T3 (da) | 2019-09-23 |
EP2756113A2 (en) | 2014-07-23 |
KR101956007B1 (ko) | 2019-03-11 |
WO2013037902A3 (en) | 2013-07-18 |
CN103827355B (zh) | 2017-04-12 |
EP2756113B1 (en) | 2019-06-26 |
WO2013037902A2 (en) | 2013-03-21 |
CN103827355A (zh) | 2014-05-28 |
CA2845679C (en) | 2020-02-25 |
TWI568888B (zh) | 2017-02-01 |
CA2845679A1 (en) | 2013-03-21 |
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