臺灣博碩士論文加值系統

本研究係利用高週波電漿系統，添加氧化劑(O2)或還原劑(CH4)，將甲硫醇、二甲基硫、二硫化碳及二氧化硫，分別於室溫環境下進行分解。主要之操作參數，包括輸入功率，反應物混合配比（O2/CH3SH、O2/DMS、O2/CS2或CH4/SO2比例），反應物進料濃度及操作壓力。研究內容探討反應物之分解率及最終產物之分布，並推論於電漿系統之反應路徑。最後，建構CS2/O2/Ar電漿模型進行數值模擬，比較與實驗值之差異。實驗設計方法及實驗結果顯示，影響分解率及產物分布之主要因素為輸入功率與反應物之混合配比。分解率方面，以CS2最容易分解，其次為CH3SH及DMS，SO2則因其熱力學上之穩定度高而最難分解。結果顯示輸入功率、添加劑濃度及解離物種之數量，影響高能及高活性物種之種類及濃度，進而影響分解率高低。產物分布方面，CH3SH及DMS在相同功率下，反應機制之差異主要在於起始反應：DMS大多分解為CH3S及CH3；而CH3SH分解為CH3、SH、CH3S及H。因DMS/Ar電漿中有高量之CH3自由基，導致CH4+C2H2+C2H4產率較高；然而CH3SH/Ar電漿因有SH可快速形成CS2，所以CS2產量較高。另外，在相同加氧比下，CH3SH/O2/Ar電漿具有較高之燃燒等值比，可迅速形成SO及CO，因此SO2及CO2產率較高，也因此，導致CH4+C2H2+C2H4、CH2O、CH3OH、CS2及OCS均較DMS/O2/Ar電漿少了許多。傳統上很難去除之SO2，在CH4/SO2進流比例=2之條件下，可同時使SO2及CH4保持在較高之分解率。當2%之SO2進料濃度於120 W功率下，SO2可達99.2%，CH4則為100%；產物分布則顯示，硫選擇性之比例為[S1]：[CS2] = 0.658：0.320。其中還原劑CH4轉化後之主產物為syngas (H2 + CO)，是工業上合成其他產品之重要原料，如CH3OH。分析S原子之反應機制發現，貧氧狀態之操作可將CH3SH或DMS轉化成CS2；而SO2亦可藉由控制CH4之濃度及輸入功率，選擇性地將S還原成元素硫及CS2。至於CS2，則可在貧氧條件下(O2/CS2 < 0.6)回收純度99.2%以上之元素硫。總結含硫化合物於RF電漿中，可選擇性地控制反應路徑以形成元素硫為反應終點，成為有潛力之硫回收方案。最後，電漿模式模擬結果顯示，常溫下無法反應之CS2/O2/Ar反應，可以在高能電子之協助下起始反應，模擬結果與實驗值大致上十分吻合。從敏感度分析可知：貧氧時(O2/CS2 = 0.6)對CS2分解最具影響力之反應式為電子解離反應CS2 + e- à CS + S + e- 及CS2 + e- à C + S2 + e-；而富氧時(O2/CS2 = 6.0)對CS2分解最具影響力之反應式為SO + O2 = SO2 + O及CS + O = CO + S。

The application of the RF (radio-frequency) cold plasma technique to the decomposition of CH3SH, (CH3)2S (DMS), CS2 and SO2 by adding oxidant (O2) or reductant (CH4) at room temperature, is investigated. The operational parameters are applied RF power, mixing ratio of reactants (O2/CH3SH, O2/DMS, O2/CS2 and CH4/SO2), inlet concentration of reactants and operational pressure. This study aims to gain insight into the decomposition fraction, product distributions and plasmachemical reaction mechanisms. Detailed CS2/O2/Ar plasma kinetic reactions are also conducted to elucidate the discrepancy between numerical modeling and experimental results. The factorial factor design method and experimental results indicated that the applied power and mixing ratio of reactants were the parameters that primarily influenced decomposition fraction and product selectivity. The results reveal that CS2 is easily decomposed, followed by CH3SH, and then DMS. SO2 is the most difficult compound to decompose because of its high thermodynamic stability. However, applying power, adduct concentration and amount of dissociated fragments affect the concentration of high energetic and active species and dominate the decomposition fraction. The main discrepancies in product patterns, between the reaction mechanisms of DMS and CH3SH are evident in the initial reactions. DMS is primarily dissociated into CH3S and CH3, while CH3SH is mainly dissociated into CH3, SH, CH3S and H. The presence of more CH3 in the DMS/Ar plasma provides more H and CHx (x = 1-3), to yield more CH4+C2H2+C2H4. SH in the CH3SH/Ar plasma proceeds by more channels to produce more CS2 than in the DMS/Ar plasma. Given the same percentage of O2, a higher equivalent ratio (Φ) lead to form SO and CO quickly to result in the yields of SO2 and CO2 in the CH3SH/O2/Ar plasma that are higher than those in the DMS/O2/Ar plasma, leaving only a trace of CH4+C2H2+C2H4, CH2O, CH3OH, CS2 and OCS in the former plasma. SO2 is typically hard to decompose. Results suggest that more SO2 and CH4 is converted at a CH4/SO2 ratio of 2, reaching conversion fractions of 99.2% for SO2 and 100% for CH4 at 120 W, with the sulfur-selectivity of S1: CS2 = 0.658: 0.320. Main by-products of the reaction are syngas (H2, CO), which are the important intermediate materials in the industrial production of CH3OH. In summary, the S atom of CH3SH and DMS can be selectively converted into mainly CS2; SO2 is converted into elemental sulfur and CS2 by altering the CH4/SO2 ratio and the applied power. For CS2, under conditions of oxygen-lean (O2/CS2 < 0.6), the majority of S atoms are converted to elemental sulfur whose purity is as high as 99.2%. Thus, this study provides an approach to recovering sulfur and thus reducing the emission of sulfur-containing compounds. Simulation results indicate that CS2/O2/Ar reactions that cannot be processed at room temperature can be performed through the initial electrical reactions, and gives yields of the product are very close to experimental yields. Sensitivity analysis reveals that the most important reactions for CS2 decomposition are electron dissociation reactions, CS2 + e- à CS + S + e- and CS2 + e- à C + S2 + e- at O2/CS2 = 0.6, and radical reactions, CS + O = CO + S and SO + O2 = SO2 + O at O2/CS2 = 6.0.

總 目 錄
授權書I
簽署人須知II
中文摘要III
英文摘要V
誌 謝VII
總 目 錄VIII
表 目 錄XII
圖 目 錄XIII
第一章 前 言1
1-1 緒論1
1-2 研究內容與流程綱要2
第二章 文獻回顧4
2-1 硫化物來源及特性4
2-1-1 元素硫之特性4
2-1-2 硫排放量及分布4
2-1-3 含硫臭味物質之特性6
2-1-4 含硫臭味物質之來源與影響8
2-2 電漿原理及應用12
2-2-1 電漿生成12
2-2-2 電漿特性14
2-2-3 電漿分類與電漿化方法17
2-3 含硫化合物之處理27
第三章 實驗設備、方法與流程30
3-1 實驗設備30
3-1-1 真空系統及測漏32
3-1-2 氣體進料／混合定量系統33
3-1-3 高週波產生系統34
3-1-4 電漿反應器34
3-1-5 定性/定量分析系統35
3-2 實驗藥品39
3-3 實驗流程40
3-3-1 實驗前準備事項40
3-3-2 操作參數與操作範圍41
3-3-3 實驗步驟43
3-3-4 不鏽鋼採樣瓶(canister)之採樣步驟44
3-3-5 固態沉積物之採樣46
3-3-6 檢量線製作(FTIR)46
第四章 CS2/O2/Ar電漿模型與電腦模擬47
4-1 CS2/O2/Ar電漿模型47
4-1-1 模型假設47
4-1-2 帶電粒子模型48
4-1-3 中性物種模型51
4-2 電腦模擬52
4-2-1 EEDF及電子反應速率常數之計算52
4-2-2 電漿化學反應之模擬基礎55
4-2-3 化學反應模擬軟體57
4-2-4 反應機制數值求解程序58
4-3 敏感度分析程式61
4-3-1 敏感度分析及敏感度係數61
4-3-2 敏感度分析程式62
4-3-3 敏感度分析程序63
第五章 結果與討論64
5-1 CH3SH之電漿分解64
5-1-1 部份因素配置法64
5-1-2 輸入功率對分解率之影響67
5-1-3 沈積物分析69
5-1-4 產物分析71
5-1-5 CH3SH/O2/Ar起始反應72
5-1-6 加氧比對產物分布及反應機制之影響74
5-2 DMS與CH3SH在電漿中轉化之比較84
5-2-1 分解率之比較84
5-2-2 產物分布之比較86
5-2-3 DMS及CH3SH起始反應之比較87
5-2-4 CS2、OCS及SO2硫轉化率之比較89
5-2-5 CxHy碳轉化率之比較94
5-2-6 CH2O及CH3OH碳轉化率之比較96
5-2-7 COx碳轉化率之比較98
5-2-8 總反應路徑之比較(overall reaction routes )99
5-3 CS2之電漿氧化與硫回收102
5-3-1 碳、硫平衡與沈積物102
5-3-2 CS2之分解率及起始反應104
5-3-3 氣相產物分布與分析106
5-3-4 氣相產物之生成與分解107
5-3-5 沈積物之成分及結構分析111
5-3-6 電漿聚合薄膜之成分及結構分析118
5-3-7 總反應式及反應路徑121
5-4 SO2/CH4之電漿分解125
5-4-1 最終產物組成125
5-4-2 CH4/SO2 比值對產物選擇性之影響127
5-4-3 CH4/SO2 比值及輸入功率對分解率之影響130
5-4-4 操作壓力及進流濃度對分解率之影響133
5-5 硫化物於電漿中反應機制之比較136
5-6 CS2/O2/Ar電漿反應之電腦模擬139
5-6-1 高週波電漿中二硫化碳氧化反應之機制139
5-6-2 電漿分解反應之電腦模擬值與實驗值之比較142
5-6-3 敏感度分析146
第六章 結論與建議153
6-1 結論153
6-2 建議156
參考文獻157
附錄A 定性物種之FTIR光譜168
附錄B 各物種之IR吸收峰波數169
附錄C CS2/O2/Ar 電漿電腦模擬物種之熱力學資料170
附錄D 鍵結解離能資料172
自 述173
表 目 錄
表2-1 硫與氧基本性質之比較5
表2-2 陸地源硫排放量之物種分布，單位：106 mol/d6
表2-3 天然及人為排放源之硫排放量分布，單位：109 mol/a6
表2-4 臭味來源與行業別之關聯8
表2-5 常見含硫化合物之氣味特徵、來源及對健康之影響9
表2-6 常見含硫化合物之基本性質11
表2-7 低溫電漿之特性參數19
表3-1 FTIR參數設定36
表3-2 實驗用藥品39
表3-3 實驗參數及操作範圍41
表5-1 部份因素實驗設計配置參數及水準66
表5-2 輸入功率對CH3SH電漿反應之影響 (P = 30 torr, R = 3.0)67
表5-3 DMS及CH3SH電漿產物之比較(30 W)88
表5-4 固體沈積物之化學分析(mass %)113
表5-5 不同功率下，總硫輸入量分別轉化至出流氣體（含未反應之CS2）、聚合薄膜及固態硫之定量比例(O2/CS2 = 0.6)114
表5-6 不同功率及不同進料濃度下，於CH4/SO2 = 2時之單位能量對SO2+CH4之總去除效率135
表5-7 不同加氧比狀況下，CS2/O2/Ar電漿反應電腦模擬之參數條件140
表5-8 CS2/O2/Ar電漿中模擬之基元反應機制141
表5-9 CS2/O2/Ar電漿中有關CS2最重要之五個反應式146
表5-10 CS2/O2/Ar電漿中有關CO最重要之五個反應式148
表5-11 CS2/O2/Ar電漿中有關CO2最重要之五個反應式149
表5-12 CS2/O2/Ar電漿中有關SO2最重要之五個反應式150
表5-13 CS2/O2/Ar電漿中有關OCS最重要之五個反應式151
表5-14 CS2/O2/Ar電漿中有關S2最重要之五個反應式151
圖 目 錄
圖1-1 研究流程3
圖3-1 高週波電漿分解實驗系統裝置31
圖3-2 電漿分解實驗步驟45
圖4-1 電子反應速率之計算流程54
圖4-2 CHEMKIN程式與SENKIN程式執行之流程圖60
圖5-1 個別參數對hCH3SH、FSO2、FCS2及FOCS之標準化影響（+表正影響，－表負影響）66
圖5-2 不同功率下，CH3SH之分解率(A)、功率密度(B)及移除效率(C)68
圖5-3 沈積物之電子顯微鏡圖，(A) O2/CH3SH = 0.6，(B) O2/CH3SH = 070
圖5-4 不同加氧比下，出流產物中CH4 (A)、C2H4 (B)及C2H2 (C)之莫耳分率76
圖5-5 不同加氧比下，出流產物中CO (A)、CO2 (B)之莫耳分率及CO2/CO 之比值(C)79
圖5-6 不同加氧比下，出流產物中CS2 (A)、SO2 (B)及OCS(C)之莫耳分率81
圖5-7 不同輸入功率(A) 及加氧比(B) 下，DMS及CH3SH分解率之比較85
圖5-8 無氧條件下，DMS及CH3SH各產物轉化率之比較90
圖5-9 加氧比3.0時，DMS及CH3SH生成CO、CO2、CS2及SO2轉化率之比較92
圖5-10 加氧比3.0時，DMS及CH3SH生成CH3OH、CH2O及OCS轉化率之比較93
圖5-11 加氧比3.0時，DMS及CH3SH生成CH4、C2H2、及C2H4轉化率之比較97
圖5-12 無氧環境之DMS及CH3SH反應路徑差異之比較100
圖5-13 有氧環境之DMS及CH3SH反應路徑差異之比較101
圖5-14 不同加氧比(A) 及輸入功率(B) 之條件下，CS2反應後殘留在出流氣體之碳及硫比例103
圖5-15 不同輸入功率下，CS2之分解率(A)及功率密度(B)105
圖5-16 不同輸入功率下，CS2分解後各產物之莫耳分率109
圖5-17 CS2/O2/Ar電漿分解後沈積物之產生及採樣位置112
圖5-18 樣品C0.6及D0.6之XRD分析圖116
圖5-19 樣品D0及D0.6之FTIR圖譜117
圖5-20 樣品F0.6及F0於S2P及C1P之XPS分解圖120
圖5-21 樣品F0.6及F0之電子顯微鏡比較圖122
圖5-22 CS2/O2/Ar電漿分解之反應路徑圖124
圖5-23 於90 W輸入功率，不同CH4/SO2比例下，經RF電漿分解後各產物之莫耳分率圖126
圖5-24 於90 W輸入功率下，不同CH4/SO2比例下，產生CS2及total sulfur之選擇性128
圖5-25 於90 W輸入功率，不同CH4/SO2比例下，SO2及CH4之分解率131
圖5-26 於CH4/SO2 = 2時，不同輸入功率之SO2及CH4分解率132
圖5-27不同輸入功率、不同SO2進流濃度及不同操作壓力下，SO2之分解率134
圖5-28 硫原子於RF電漿中反應之選擇性137
圖5-29 加氧比0.6(A)及6.0(B)下，CS2/O2/Ar電漿模擬之時間與產物濃度關係圖143
圖5-30 不同加氧比下，CS2分解率之實驗值與模擬值比較144
圖5-31 不同加氧比條件下，CS2/O2/Ar各產物莫耳濃度之實驗值與模擬值之比較145

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