本研究係採逆向實務可行之原則加以規劃設計處理流程回收混合型廢鋰離子電池中之有價金屬，希冀在實驗室規模研究各處理程序所求得之最佳操作條件，未來能予以放大驗證及應用。於國內某廢乾電池回收處理廠採集之混合型廢鋰離子電池以Co, Mn, Cu及Zn為其主要元素，分別占整體含量之42%、16%、10%及16%。由酸浸漬/酸溶試驗得知：混合型廢鋰離子電池於80 ºC 添加3 M硫酸及5 vol%過氧化氫可得最佳溶出效率。由金屬離子分離試驗發現：(1) 混合型廢鋰離子電池酸溶出液在pH 4時，由磺化煤油為稀釋劑之0.4 M D2EHPA對Al、Fe及Zn有最佳移除率；(2) 經 (1) 萃取後之萃餘液於pH 6.5對Al及Cu有最佳移除率；(3) 經 (2) 沉澱後之上澄液於pH 10且以添加劑量為莫耳比0.5之碳酸鈉可藉由共沉澱分離出Co/Mn；將共沉澱物以0.4 M 硫酸及2.5 vol%過氧化氫，於室溫下進行酸浸漬/酸溶，可獲得最佳回溶率。金屬離子分離試驗後，於金屬電析精煉試驗發現：在電流密度250 A/m2下，電沉積5小時，即可將MnSO4及CoSO4電解液中Mn及Co回收。混合型廢鋰離子電池中之Mn及Co整體回收率分別為88%及86%，其中，鈷純度為97%，由上述得以證實本研究所設計之回收處理流程具有實廠應用之潛力。

Based on the principle of technically feasible reverse implementation, the objective of this work was to determine the optimal operating conditions that can be scaled up to recover valuable metals from spent mixed-type lithium-ion batteries (LIBs). First, after pretreatments the samples of screen undersize of spent mixed-type LIBs were collected from a local spent battery recycling plant. After analysis, it was found that major elements in the spent mixed-type LIBs were Co, Mn, Cu and Zn having 42 wt%, 16 wt%, 10 wt%, and 16 wt%, respectively. Results of the acid leaching tests showed that the optimal leaching conditions were determined to be 80˚C, 3 M H2SO4 and 5 vol% H2O2 for the spent mixed-type LIBs. Then various separation methods have been used for the separation of metallic ions in the leached solution. The relevant test results for the spent mixed-type LIBs are given as follows: (1) Under the condition of pH 4, 0.4 M D2EHPA could extract up to 70% of Zn without co-extraction of target metals; (2) The stripping efficiency for Zn was 100% if 0.4 M H2SO4 was used as the stripping agent; (3) As for raffinate from (1), under the condition of pH 6.5, 90% of Al and 98% of Cu were removed; (4) After precipitation, when ([Co2+] +[Mn2+]) : [CO32-] molar ratio was under 0.5 and pH was adjusted to 10, the precipitation efficiency of Co and Mn were 100%, and the precipitate formed would be dissolved by 0.4 M H2SO4 and 2.5 vol% H2O2. Tests results for electrowinning of metals are given as follows: The operation of electrowinning for 5 h could recover 98% of Co and 97% of MnO2 from CoSO4 and MnSO4 contained in the electrolyte recovered from (4) indicated above. Based on the test results obtained from the aforementioned unit operations, the overall recoveries of 86% Co and 88% Mn were obtained for the spent mixed-type LIBs. Accordingly, a satisfactory recycling flowchart has been devised in this study. It is suggested that a semi-full scale testing should be carried out in the future to verify the findings obtained in this study.

學位論文審定書 i
謝誌 ii
摘要 iii
Abstract iv
目錄 vi
表目錄 xi
圖目錄 xii
第一章 前言 1
1.1研究緣起 1
1.2研究目標 7
1.3研究內容與架構 7
第二章 文獻回顧 11
2.1鋰離子電池 11
2.1.1類型與組成 11
2.1.2組成份元素之潛在危害性 12
2.2 廢鋰離子電池常見之回收處理技術 14
2.2.1火法冶金 15
2.2.2濕法冶金 17
2.2.2.1酸浸漬/酸溶 (Acid leaching) 20
2.2.2.2溶出液中的金屬離子分離 23
2.2.2.3金屬電析精煉 28
第三章 材料與方法 30
3.1實驗材料 30
3.1.1廢鋰離子樣品來源 30
3.1.2材料與試劑 31
3.2實驗設備及儀器 32
3.3實驗方法 33
3.3.1廢鋰離子電池基本特性分析 33
3.3.2酸浸漬/酸溶試驗 34
3.3.3溶出液中的金屬離子分離 36
3.3.3.1溶劑萃取法萃取Al、Cu及Zn 36
3.3.3.2氫氧化物沉澱法移除Al及Cu 39
3.3.3.3共沉澱回收CoCO3及MnCO3 40
3.3.3.4酸浸漬/酸溶試驗回收CoSO4及MnSO4 41
3.3.4金屬電析精煉 42
第四章 結果與討論 44
4.1廢鋰離子電池標基本特性分析 44
4.2酸浸漬/酸溶試驗 48
4.2.1反應溫度對於酸浸漬/酸溶之影響 48
4.2.2硫酸濃度對於酸浸漬/酸溶之影響 50
4.2.3添加過氧化氫對酸浸漬/酸溶之影響 55
4.3混合型廢鋰離子電池溶出液中金屬離子分離 58
4.3.1溶劑萃取法移除Zn 58
4.3.1.1不同稀釋劑對於萃取溶劑效能之影響 58
4.3.1.2不同水相 pH 值對於萃取溶劑效能之影響 60
4.3.1.3不同皂化率對於萃取溶劑效能之影響 61
4.3.1.4萃取溶劑之重複利用對於萃取溶劑效能之影響 64
4.3.2化學沉澱法移除Al及Cu 65
4.3.3化學沉澱法回收CoCO3及MnCO3 66
4.3.4酸回溶CoCO3及MnCO3共沈澱物回收CoSO4及MnSO4 70
4.4 CoSO4及MnSO4之同步電析/電解精煉金屬 72
4.4.1不同電解液組成對於同步電析效果之影響 72
4.4.2不同電流密度對於同步電析效果之影響 75
4.4.3不同反應時間對於同步電析效果之影響 77
4.5 技術可行性評估 87
4.6 經濟可行性評估 90
4.7 綜合討論 92
第五章 結論與建議 93
5.1 結論 93
5.2 建議 94
參考文獻 96
附錄 107
附錄一 廢棄物及底泥中金屬檢測方法－酸消化法 (NIEA M353.02C) 107
附錄二 沉積物、污泥及油脂中金屬元素總量之檢測方法-微波消化原子光譜法 (NIEA R355.00C) 109
附錄三 乾電池汞、鎘、鉛含量檢測方法 (NIEA R315.02B) 111
附錄四 事業廢棄物水分測定方法－間接測定法 (NIEA R203.02C) 112
碩士在學期間發表之學術論文 113

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