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研究生：	柯宏杰 Ke, Hong-Jie
論文名稱：	釤鈷鐵磁體化學再生之研究 The study on chemical regeneration of samarium-cobalt magnets
指導教授：	申永輝 Shen, Yong-Hui
學位類別：	碩士 Master
系所名稱：	工學院 - 資源工程學系 Department of Resources Engineering
論文出版年：	2020
畢業學年度：	108
語文別：	中文
論文頁數：	88
中文關鍵詞：	釤鈷磁鐵、釤、鈷、溶媒萃取、離子交換樹脂、回收率、再生
外文關鍵詞：	SmCo magnet, Sm, Co, solvent extraction, ion exchange resin, recovery rate, regeneration
相關次數：	點閱：169 下載：6
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本研究針對釤鈷磁鐵的下腳料進行金屬資源再生的研究，實驗主要分為三大部分，第一部分為釤鈷磁鐵下腳料破碎後的粉末的特性分析和酸溶浸漬的研究，藉由分析粉末的化學成分、表面特性和結晶相，得到研究的相關數據的依據。破碎後的粉末，以100目的篩網(篩孔: 150 um)過篩後，對無法過篩的篩上物粉末和可以過篩的篩下物粉末，以王水作全溶消化實驗，篩上物粉末金屬成分的主要組成為釤:9.57%; 鈷:21.62%; 鐵:33.36%; 銅:1.42% ；另一方面，篩下物粉末的金屬成分的主要組成為釤:21.94%; 鈷:48.04%;鐵:16.96%; 銅:4.63%。因為篩下物的粉末較均質，故以篩下物的粉末進行酸溶浸漬實驗，再探討各項酸溶浸漬的參數，以求得到最佳浸漬的參數，並透過浸漬反應動力學的研究，得到反應的控制機制是表面化學反應和內擴散反應所共同支配的反應控制機制，各金屬的浸漬活化能分別為釤26.64 kJ/mol、鈷43.17 kJ/mol、鐵45.42 kJ/mol、銅47.56 kJ/mol。當達到最佳浸漬時，釤、鈷、鐵、銅的浸漬效率都達到98.1%以上。
本研究的第二部分是關於金屬分離純化的研究，主要的分離方法為離子交換和溶媒萃取及選擇性化學沉澱。先使用螯合型離子交換樹脂M4195進行第一階段的選擇性萃取，將銅離子吸附於樹脂中移除，釤、鈷、鐵離子則留在萃餘液中。之後再將萃餘液以萃取劑 Aliquat336 進行第二階段的溶媒萃取，萃餘液中的離子以特定濃度的鹽酸進行氯化錯合後以 Aliquat336 進行萃取，將鐵離子萃取至有機相，釤、鈷離子留在萃餘液中，再利用反萃取使有機相中的鐵離子洗提到水相中。反萃取過程中以硫酸和氫氧化鈉作為反萃取劑，硫酸可剝離少量萃取至有機相的鈷和部分的鐵，再以氫氧化鈉剝離大部分萃取至有機相的鐵，形成氫氧化鐵沉澱。之後再將富含釤、鈷離子的萃餘液以正磷酸進行選擇性化學沉澱，藉由釤離子與正磷酸形成淡黃色的磷酸釤沉澱，使釤、鈷有效分離。本研究的第三部分是金屬產物析出的研究，依照不同的最終產物，選擇合適的析出方法，第一種為選擇性化學沉澱法，利用正磷酸和氫氧化鈉進行化學沉澱反應，先用氫氧化鈉將富含釤、鈷離子萃餘液的 pH值調至5，並加入濃度0.4 mol/L的正磷酸，可得到純度達88.05%的磷酸釤沉澱物；第二種為旋轉蒸發結晶法，藉由旋轉蒸發儀減壓濃縮均勻加熱的方式，製成純度99.95%的硫酸鈷。各金屬分離再生前化合物的回收率:釤97.64%、鈷79.46%、鐵64.58%、銅100.00%。

The purpose of this study is to study the metal resources regeneration of the scraps of samarium-cobalt magnets. The experiments are divided into three parts, the first part is the characteristic analysis of the powders after crushing the scraps of samarium-cobalt magnets and the study of acid-soluble leaching.
By analyzing the chemical composition, surface characteristics and crystalline phase of the powders. In order to get the basis of the relevant data of the study.
The crushed powders with 100 mesh sieve ( sieve opening:150 um ) to sieve, the powders on the sieve that can not be sieved and the powders on the sieve that can be sieved to make the experiment of total-soluble digestion through aqua regia. The main composition of metal components of the powders on the sieve is Sm: 9.57%; Co: 21.62%; Fe: 33.36%; Cu: 1.42%; On the other hand, the main element of the metal components of the powders under the sieve is Sm: 21.94% ; Co: 48.04%; Fe: 16.96%; Cu: 4.63%. Because powders under the sieve are more homogeneous, so we use powders under the sieve to make the experiment of acid-soluble leaching. And then various parameters of the acid-soluble leaching were discussed for getting the parameters of the optimal leaching, and through the study of the leaching reaction kinetics, it shows the reaction control mechanism is a control mechanism of combination, and it is governed by the surface chemical reaction and internal diffusional reaction.
The activation energy of the leaching reaction of each metals is Sm :26.64 kJ / mol, Co: 43.17 kJ / mol, Fe: 45.42 kJ / mol, Cu: 47.56 kJ / mol. When the best leaching was reached, the leaching efficiency of Sm, Co, Fe, and Cu is all reached 98.1%,

The second part of this study is about metal separation and purification.
The three major methods are ion exchange, solvent extraction, and selective chemical precipitation. A chelating resin of ion exchange M4195 was used for the first stage of the selective extraction. Copper ions were adsorbed in resin to remove, and samarium, cobalt, iron ions were stayed in the raffinate. The raffinate was extracted with Aliquat336 extractant for the solvent extraction in the second stage. The ions in the raffinate were chlorinated by applying the hydrochloric acid of specific concentration and extracted with Aliquat336. The iron ions were extracted into the organic phase. The samarium and cobalt ions were remained in the raffinate, the stripping agents scrubbing iron ions from the organic phase into the aqueous phase. In stripping process, sulfuric acid and sodium hydroxide are used as stripping agents. Sulfuric acid can scrub a small amount of cobalt ions and partial iron ions that extracted to the organic phase, and then scrubbing most of iron ions that extracted to the organic phase with sodium hydroxide to form the precipitates of iron hydroxide. After that, samarium-rich and cobalt-rich ions in the raffinate are selectively chemically precipitated with orthophosphoric acid, samarium ions and orthophosphoric acid form the pale yellow precipitates of samarium phosphate to effectively separate samarium and cobalt.

The third part of this study is about the precipitation of metal products.
According to the different final products, choosing the appropriate method of precipitation . The first method is selective chemical precipitation method
, which uses orthophosphoric acid and sodium hydroxide to make a chemical precipitation reaction. First, sodium hydroxide is used to adjust the pH value
to 5 from the raffinate of samarium-rich and cobalt-rich ions, and 0.4 mol/L orthophosphoric acid was added to obtain a precipitated product of samarium phosphate with a purity of 88.05%. The second method is the method of the rotary evaporation crystallization. By a concentrated and uniformly heated method of rotary evaporator to produce cobalt sulfate with a purity of 99.95%.
The recovery rate of metallic compound of each metal before separation and regeneration is : Samarium 97.64%, Cobalt 79.46%, Iron 64.58%, Copper 100.00%.

目錄


口試合格證明……………………………………………………………………  I
中文摘要………………………………………………………………………………  1
Summary………………………………………………………………………………… 2
致謝………………………………………………………………………………………… 6
目錄……………………………………………………………………………………………7
表目錄………………………………………………………………………………… 11
圖目錄………………………………………………………………………………… 13
第一章 緒論	………………………………………………………… 15
  1.1 前言……………………………………………………………………… 15
  1.2 研究動機與目的……………………………………………… 17
第二章 理論基礎與文獻回顧…………………………………… 20
  2.1 釤鈷磁鐵(Samarium-Cobalt magnets)特性概述………………………20
  2.1.1 釤鈷磁鐵(Samarium-Cobalt magnets)………………………………20
  2.1.2 釤之性質及資源現況………………………………………………… 22
  2.1.3 鈷之性質及資源現況………………………………………………… 23
  2.1.4 鐵之性質及資源現況………………………………………………… 24
  2.1.5 銅之性質及資源現況………………………………………………… 25
  2.2 資源化與冶金技術……………………………………………………… 26
  2.2.1 火法冶金……………………………………………………………… 26
  2.2.2 濕法冶金……………………………………………………………… 27
  2.3 釤鈷磁鐵磁性材料之酸溶浸漬反應理論……………………………… 30
  2.3.1 浸漬反應熱力學……………………………………………………… 30
  2.3.2 浸漬反應動力學……………………………………………………… 32
  2.4 釤鈷磁鐵磁性材料之金屬分離純化理論……………………………… 34
  2.4.1 離子交換法…………………………………………………………… 34
  2.4.2 溶媒萃取法…………………………………………………………… 36
  2.4.3 選擇性化學沉澱法…………………………………………………… 42
  2.4.4 再結晶法……………………………………………………………… 43
第三章 實驗方法與步驟…………………………………………………………44
  3.1 實驗藥品………………………………………………………………… 44
  3.2 實驗流程………………………………………………………………… 45
  3.3 實驗架構………………………………………………………………… 46
  3.3.1 釤鈷磁鐵磁性材料之特性分析……………………………………… 46

  3.3.2 酸溶浸漬……………………………………………………………… 46
  3.3.3 離子交換……………………………………………………………… 47
  3.3.4 溶媒萃取……………………………………………………………… 48
  3.3.5 選擇性化學沉澱……………………………………………………… 50
  3.3.6 金屬化合物析出……………………………………………………… 50
  3.3.7 再結晶法……………………………………………………………… 51  
  3.4 實驗設備及儀器………………………………………………………… 51 
  3.4.1 掃描式電子顯微鏡(SEM)及能量色散光譜儀(EDS)………………… 51
  3.4.2 X光螢光光譜儀(XRF) ………………………………………………  52
  3.4.3 X光繞射分析儀(XRD)………………………………………………… 52
  3.4.4火焰式原子吸收吸收光譜儀(AAS)…………………………………… 53
  3.4.5旋轉減壓濃縮機(Rotary Evaporators)………………………………53
第四章 結果與討論………………………………………………………………54
4.1 釤鈷磁鐵廢棄物之特性分析…………………………………………… 54

4.1.1 表面特性分析………………………………………………………… 54

4.1.2 化學成分分析………………………………………………………… 56

4.1.3 粉末結晶相分析……………………………………………………… 57

4.2釤鈷磁鐵廢棄物粉末之浸漬溶出…………………………………………58

  4.2.1 浸漬參數對浸漬效率的影響………………………………………… 60
  4.2.2 浸漬反應動力學……………………………………………………… 65
  4.2.3 浸漬溶出總結………………………………………………………… 67
  4.3 金屬分離純化研究探討………………………………………………… 69
  4.3.1 離子交換-M4195 系統…………………………………………………69

  4.3.2 溶媒萃取-Aliquat336系統……………………………………………72

  4.3.3 溶媒萃取總結………………………………………………………… 77
  4.3.4 選擇性化學沉澱……………………………………………………… 79
第五章　結論…………………………………………………………………… 81
  5.1 結論……………………………………………………………………… 81
參考資料………………………………………………………………………… 83
實驗流程圖……………………………………………………………………… 88















表目錄


Table.1-1 在挑選的產品群組中關鍵金屬的使用…………………………… 17
Table.3-1 實驗化學藥品資訊………………………………………………… 44

Table.3-2 XRD的儀器操作設定…………………………………………………52
Table.3-3  AA儀器測定的波長表………………………………………………53
Table.4-1 釤鈷磁鐵廢棄物粉末之成分分析………………………………… 56

Table.4-2 不同酸液作為浸漬液對於樣品裡金屬的浸漬率………………… 59

Table.4-3 硫酸對釤鈷磁鐵磁性材料的浸漬反應之化學反應式…………… 59

Table.4-4 釤鈷磁鐵廢棄物破碎後粉末等溫浸漬實驗數據—線性擬合表 66
Table.4-5 表面化學反應控制的Sm、Co、Fe、Cu金屬離子的活化能………66

Table.4-6 擴散反應控制的Sm、Co、Fe、Cu金屬離子的活化能……………67

Table.4-7 共同反應支配的Sm、Co、Fe、Cu金屬離子的活化能……………67

Table.4-8 釤鈷磁鐵廢棄物粉末酸溶浸漬最佳參數………………………… 68

Table.4-9 酸溶浸漬後浸漬液裡金屬離子的濃度…………………………… 69

Table.4-10 調整浸漬液pH值後以M4195離子交換樹脂進行吸附………… 70

Table.4-11 油水比對萃取效率的影響…………………………………………74

Table.4-12	硫酸濃度對反萃取效率的影響……………………………………75

Table.4-13	氫氧化鈉濃度對反萃取效率的影響………………………………75
Table.4-14 油水比對反萃取效率的影響………………………………………76 

Table.4-15 Aliquat336萃取的最佳參數………………………………………77

Table.4-16 Aliquat336萃取的最佳分配比和分離係數………………………78

Table.4-17 Aliquat336系統反萃取的最佳參數………………………………78

















圖目錄


Fig.1-1 2016年電子廢棄物的收集方法……………………………………… 18
Fig.2-1 Sm、Co、Fe、Cu的Pourbaix Diagram……………………………  31
Fig.2-2 縮核模型……………………………………………………………… 32
Fig.2-3 Aliquat336的結構 ……………………………………………………39
Fig.3-1 實驗流程……………………………………………………………… 45

Fig.4-1 下腳料破碎後粉末…………………………………………………… 54
Fig.4-2 釤鈷磁鐵下腳料破碎後粉末SEM分佈圖…………………………… 55

Fig.4-3 釤鈷磁鐵下腳料破碎後粉末EDS分佈圖…………………………… 55
Fig.4-4 釤鈷磁鐵下腳料破碎後粉末的XRD分析…………………………… 57
Fig.4-5永久磁鐵最大磁能積時間演變圖…………………………………… 58
Fig.4-6 硫酸濃度對浸漬效率的影響………………………………………… 60

Fig.4-7 鹽酸濃度對浸漬效率的影響………………………………………… 61

Fig.4-8 硫酸液固比對浸漬效率的影響……………………………………… 62

Fig.4-9 反應時間對浸漬效率的影響………………………………………… 63

Fig.4-10 浸漬溫度對浸漬效率造成的影響……………………………………64

Fig.4-11 不調整浸漬液pH值M4195離子交換樹脂的吸附曲線…………… 70

Fig.4-12 以氫氧化銨作為脫附劑M4195離子交換樹脂的脫附曲線…………71

Fig.4-13 硫酸浸漬液中氯離子濃度對萃取的影響……………………………73

Fig.4-14 不同反應平衡pH值對磷酸沉澱金屬離子的效率………………… 80

Fig.4-15 選擇性化學沉澱的磷酸釤固體在XRD儀器分析的繞射強度圖……80
Fig.5-1 實驗流程圖…………………………………………………………… 88
                                    

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