TW201800508A - 閥金屬基材或其合金之防腐塗料及其製法和電化電池凸緣之翻新方法 - Google Patents
閥金屬基材或其合金之防腐塗料及其製法和電化電池凸緣之翻新方法 Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 11
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- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 10
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 10
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- 238000011068 loading method Methods 0.000 claims description 4
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- 150000004706 metal oxides Chemical class 0.000 claims description 4
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 4
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- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 3
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- 239000010970 precious metal Substances 0.000 claims description 2
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- 229910000510 noble metal Inorganic materials 0.000 description 1
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- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
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Abstract
本發明係關於一種塗料，可供保護鈦表面之填隙腐蝕，諸如高度侵蝕性電解環境，例如鹽酸電解池、所用凸緣或其他設備。本發明塗料包括鈍化層，對此施加撥水性材料膜。本發明又涉及電化電池凸緣之防腐保護方法。
Description
本發明係關於一種塗料，可供保護鈦表面之填隙腐蝕，諸如高度侵蝕性電解環境，例如鹽酸電解池、所用凸緣或其他設備。
填隙腐蝕是電化領域公知的現象。在鈦和鈦合金製碱氯電池等電解電池組件，碰到含氯離子之溶液時所發生，填隙腐蝕現象是鹽酸電解池的主要問題。鹽酸電解為日漸有利益的電化製程，因鹽酸是使用氯的所有主要工業製法之副產品：提高現代設計工廠之生命容量，即形成大量鹽酸，其銷售呈現重大困難。鹽酸電解通常是在電解池內進行，有二室，利用離子交換膜隔開，在陽極室形成氯，可上游回收，致呈實質上閉路循環，在實務上無環境衝擊問題。陽極室的構造材料，必須能耐得住酸性、濕氯和陽極偏極化組合造成的高度侵蝕性環境；為此，構造材料最好使用閥金屬，諸如鈦、鈮和鋯，其中最常用者為鈦，為成本和容易處理打算，可視情形用合金。廣用例如鈦合金，含鎳、鉻，和少量貴金屬，諸如釕和鈀，諸如神戶鋼鐵公司產銷的AKOT®合金。發生陽極釋氯用的陽極，例如由鈦合金等閥金屬基材構成，塗佈能夠降低陽極排放之過電位，一般由鈦和釕的氧化物混合物構成。有些塗料型也用於不涉及釋氯的陽極室其他組件之腐蝕保護，尤其是在可能構成受到電解質滯流的填隙之區域。電解質缺乏充分交流，事實上會引起鈍化層的局部間斷，其目的在保護閥金屬觸發腐蝕現象，在小面積愈局部化愈危險。陽極室和陰極室二室之外凸緣，通常設有密封墊圈，為受到填隙腐蝕的電池區域例。工業實務上遇到最有利的情況是，鈦合金塗佈以釕和鈦的氧化物為基本之觸媒配方，可保證在鹽酸電解工廠連續操作24至48個月，才有腐蝕問題，導致凸緣區內電池元件密封損失。碱氯隔膜製法設備的鈦表面保護問題，在例如EP0397114
號中解決。EP0397114號載明應用單層結構，包括鉑族金屬或其氧化物之顆粒，按容量比1：2，分散於氟化聚合物之矩陣內。在EP0397114號所擬解決方案中，氟化聚合物有黏合劑功用，裡面分散有導電性顆粒。在此特殊型結構中，觸媒粒間之電氣連續性不良。缺乏電氣連續性的結果，即無法建立鈍化機制，憑以保護鈦基材。此外，在EP0397114號所述特殊結構中，聚合物量不能減少，會使結構本身的機械穩定性不夠。為改善鹽酸電解工業製法(其中反應環境比碱氯電池更具侵蝕性)之競爭力，必須進一步增加此等組件之使用壽命。
本發明各種要旨列在申請專利範圍附屬項內。
按照一要旨，本發明係關於閥金屬或其合金基材之防腐塗料，包括至少一鈍化層，和至少一層疏水性聚合物，施加於該至少一鈍化層，該至少一鈍化層包括至少一鉑族金屬的至少一氧化物和至少一閥金屬氧化物之混合物，該至少一鈍化層具有孔隙性，部份被施加於該至少一鈍化層的該至少一層疏水性聚合物所封閉。事實上，發明人等發現防腐塗料包括二層，一鈍化層，定著於基材，一疏水性層，從而定著於第一鈍化層，可有效阻止腐蝕液滲透入填隙內。此外，上述二層結構進一步優點是，在聚合物層損壞或要拆除時，基材表面仍受到第一鈍化層保護，延長其壽命。
在一具體例中，防腐塗料包括2-8g/m2該疏水性聚合物。
在一具體例中，本發明防腐塗料之疏水性聚合物層，與水接觸角度大於97°。發明人等意外觀察到，有些聚合物，例如聚四氟乙烯(PTFE)之撥水性能，足以阻止腐蝕性物質滲透入填隙內。與先前技術中通常用做防腐膜數毫米程度相較，本發明施用於第一鈍化層之聚合物膜很薄，數微米而已。
在一具體例中，疏水性聚合物為氟化聚合物。
在一具體例中，氟化聚合物為聚四氟乙烯(PTFE)。
在一具體例中，至少一鉑族金屬之至少一氧化物，為氧化釕，而至少一閥金屬氧化物為氧化鉭。
在一具體例中，本發明塗料具有鈍化層，含貴金屬載量，按金屬釕表示介於1和4g/m2之間。
在一具體例中，本發明塗料施加於鈦或鈦合金基材。
在一具體例中，塗料施加於電解槽，視情形為鹽水電解槽之鈦或鈦合金凸緣。
按照另一要旨，本發明係關於上述防腐塗料之製造方法，包括如下同時或接續步驟：˙於閥金屬基材施加釕和鉭之化合物溶液，塗一次或多次，每次塗後，隨即在450至550℃之溫度，進行熱分解5至20分鐘，最後熱處理在450至500℃進行1至3小時，直至獲得該鈍化層；˙施加(氟化)聚合物之水性懸浮液，塗一次或多次，每次塗後，接著在40至80℃溫度乾燥5至20分鐘，最後熱處理在300至360℃溫度進行5至15分鐘。
按照另一要旨，本發明係關於電解電池之凸緣處理方法，包括澱積上述防腐塗料。
第1圖表示按照實施例1製備樣品之掃描電子顯微(SEM/EDAX)影像，並指示有元素存在之濃度形態。"PTFE"指氟之濃度形態，完全歸因於PTFE存在。
下列實施例用來證明本發明特殊具體例，其可行性在申請專利範圍所請求數值範圍內，已獲充分證明。凡技術專家均知以下實施例所述組成份和技術，表示本發明在實際應用上已知功能性優良之組成份和技術；惟有鑑於本案之說明，技術專家均知所揭示特殊具體例，可有許多變化，仍然可得相似或類似結果，而保持在本發明範圍內。
實施例1
取AKOT®鈦合金板，尺寸為50mm×50mm，用丙酮在超音波浴內脫脂，並在煮沸20% HCl內浸泡過15分鐘。
取20重量% RuCl3和50g/l TaCl5，在10%鹽酸內混合，製得鈍化溶液。
鈍化溶液用刷塗4-5次，每次塗後，在50℃乾燥10分鐘，
在500℃熱分解處理5分鐘，直到獲得鉭和釕之氧化物之澱積物，釕總載量約3g/m2。熱分解過程結束時，板在500℃進行繼續熱循環2小時。
取杜邦-三井氟化學公司產品PTFE-31JR懸浮液(60重量%)，用脫離子水稀釋，經三次循環刷塗，每次塗後，在60℃乾燥8分鐘，最後熱處理在370℃進行15分鐘，PTFE總載量為6g/m2。所得樣本編為1號，以電子顯微鏡檢定；鈍化層組成份如表1所示，參見第1圖。
尤其是氟形態識別PTFE存在，並且證明PTFE已滲透入鈍化層。鈍化層的生理孔隙性容許之此項滲透，大為提高聚合物層和鈍化層間之黏著性。
比較例1
取AKOT®鈦合金板，尺寸為50mm×50mm，用丙酮在超音波浴內脫脂，在煮沸20% HCl內浸泡15分鐘。
取20重量% RuCl3和50g/l TaCl5，在10%鹽酸內混合，製得鈍化溶液。
鈍化溶液加以刷塗4至5次，每次塗後，在50℃乾燥10分鐘，在500℃熱分解處理5分鐘，直到獲得鉭和釕的氧化物澱積，釕總載量約3g/m2。熱分解過程結束時，板在500℃進行進一步熱循環2小時。製成樣本標示為C1。
實施例2
二樣本1和C1經腐蝕測試，模擬生產氯的電解槽凸緣或其他蔽護區內可能發生的填隙腐蝕條件。第一系列樣本在氮氣流下，浸入45℃已知容量的20重量% HCl內，模擬電解質滯留條件。測試80小時結束後，分析溶液從基材釋出之鉻和鎳濃度。結果如表2所示。
前述無意限制本發明，可按照各種具體例使用，不悖所述目的，其範圍則明確以所附申請專利範圍界定。
在本案說明和申請專利範圍中，「包括」字樣不排除其他額外元件、組件或處理步驟存在。
文本內包含文件、規範、材料、裝置、論文等的討論，單純目的在於提供本發明脈絡；惟並非意指此材料或其部份，構成本案所附申請專利範圍各項優先權日之前，與本發明相關領域之常識。
Claims (11)
- 一種閥金屬基材或其合金之防腐塗料，包括至少一鈍化層，和至少一層疏水性聚合物，施加於該至少一鈍化層，該至少一鈍化層包括至少一鉑族金屬的至少一氧化物和至少一閥金屬氧化物之混合物，該至少一鈍化層具有孔隙性，被施加於該至少一鈍化層的該至少一層疏水性聚合物所部份封閉者。
- 如申請專利範圍第1項之塗料，包括2至8g/m2之該疏水性聚合物者。
- 如申請專利範圍第1或2項之塗料，其中該至少一層疏水性聚合物與水之接觸角度大於97°者。
- 如申請專利範圍第1至3項之塗料，其中該疏水性聚合物係氟化聚合物者。
- 如前述申請專利範圍之一項塗料，其中該氟化聚合物為聚四氟乙烯者。
- 如申請專利範圍第1項之塗料，其中該至少一鉑族金屬之至少一氧化物，係氧化釕，而該至少一閥金屬氧化物，係氧化鉭者。
- 如申請專利範圍第1至4項之塗料，其中該鈍化層包含貴金屬，釕載量以金屬表示，介於1和4g/m2之間者。
- 如前述申請專利範圍之一項塗料，其中該基材為鈦或鈦合金者。
- 如申請專利範圍第8項之塗料，其中該鈦或鈦合金之基材，為電解槽之凸緣者。
- 一種如申請專利範圍第1至9項防腐塗料之製法，包括下列同時或依序步驟：˙於閥金屬基材施加釕和鉭之化合物溶液，塗一次或多次，每次塗後，在450至550℃之溫度乾燥並進行熱分解為時5至20分鐘，最後熱處理在450至500℃之溫度進行1至3小時，得該鈍化層；˙施加疏水性聚合物之水性懸浮液，塗一次或多次，每次塗後，在40至80℃之溫度乾燥5至20分鐘，最後熱處理在300至360℃之溫度，進行為時5至15分鐘者。
- 一種電化電池凸緣之翻新方法，包括澱積如申請專利範圍第1至9項所述防腐塗料者。
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| ITUB20159439A1 (it) | 2017-06-21 |
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| JP2019508590A (ja) | 2019-03-28 |
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