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研究生：	黃瀞瑩 Huang, Jing-ying
論文名稱：	以Fe2O3/SiO2吸收劑高溫去除硫化氫及硫化羰之研究 High-Temperature Sorption of Hydrogen Sulfide and Carbonyl Sulfide by Fe2O3/SiO2
指導教授：	朱信 Chu, Hsin
學位類別：	碩士 Master
系所名稱：	工學院 - 環境工程學系 Department of Environmental Engineering
論文出版年：	2007
畢業學年度：	95
語文別：	中文
論文頁數：	200
中文關鍵詞：	氣化氣、硫化氫、除硫、吸收劑、金屬氧化物、硫化羰
外文關鍵詞：	metal oxides, sulfur removal, syngas, hydrogen sulfide, carbonyl sulfide, sorbent
相關次數：	點閱：97 下載：9
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隨著世界人口的增加與科技的需求，石油及天然氣等能源短缺，導致油價不停地上漲，為了因應多元化能源利用，未來在燃煤發電之使用將明顯的上升。煤炭氣化複循環發電技術(IGCC)是以煤炭作為能源，能夠降低污染物之釋放，以達到煤炭高效率、清潔之使用，未來將成為發電技術主流之ㄧ。現行商業運轉之大型煤炭氣化複循環發電機組(IGCC)皆使用溼式商業化之除硫程序，但由於用水量大，使得系統熱效率降低，為解決此問題以降低發電及環保成本，利用高溫下乾式除硫方法將是未來的趨勢。
本研究以自行自備之高表面積Fe2O3/SiO2吸收劑吸收處理硫化氫/硫化羰，研究成果分成下列幾點探討：
1. 負載於不同載體之三氧化二鐵吸收劑之脫硫效能以負載於SiO2 之吸收劑脫硫效果較好，負載於ZrO2及γ-Al2O3載體上之三氧化二鐵吸收劑脫硫效果較差。
2. 經由一系列的操作溫度對於單獨去除硫化氫及同時去除硫化氫、硫化羰之影響實驗可以發現，最佳的操作溫度應為500℃。
3. 觀察改變操作參數對於Fe2O3/SiO2吸收劑除硫效能之影響，發現一氧化碳濃度增加、氫氣濃度減小會增加吸收劑利用率，這可能和
Water-shift reaction有關；而空間流速在3,000~18,000 mL·hr-1·g-1之間時脫硫容量受空間流速之影響並不顯著；硫化氫及硫化羰進流濃度對吸收劑利用率無顯著之影響。
4. 由氧化/還原氣氛之熱重分析觀察Fe2O3/SiO2吸收劑的重量變化，還原氣氛下，Fe2O3於高溫下會被還原為低氧化數的鐵氧化物；氧化氣氛下，發現有部分脫硫後之產物FeS會先轉為FeSO4，之後才繼續氧化成為Fe2O3。
5. 由動力研究發現，第一型衰退模式所求得之活化能為103 kJ/mol，碰撞因子A = 1.4 × 1017 ，第二型衰退模式所求得之活化能為65.5 kJ/mol，碰撞因子A = 4.3 × 1014。

With the increase of the population and demands for better life in the world, the energy, such as petroleum and natural gas, are exhausted and their prices are booming. For the need of diversified clean energy, the use of
coal-burning power will increase obviously in the future. Integrated Gasification Combined Cycle (IGCC) is one of the ideal technologies, which mainly uses coal to generate power. It can reduce the emissions and improve the efficiency of coal-burning. This technology will become the main stream of power supply in the future. Nowadays, all commercial IGCC power plants use wet desulfurization processes to remove H2S from hot syngas, but they have to use large amount of water and, thus, decrease the
thermal efficiency of the system. In order to solve this problem, the high temperature desulfurization by dry techniques is a trend for related fields.
Desulfurization of hot coal gas using homemade Fe2O3/SiO2 sorbent in a fixed bed reactor was conducted in this study. The discussion of results can be divided into five major parts.
1. The Fe2O3 sorbent supported on SiO2 exhibits higher sorbent utilization than the Fe2O3 sorbents supported on γ-Al2O3 and ZrO2.
2. The operating temperatures around 500℃ is optimal for the Fe2O3/SiO2 sorbent.
3. The effects of operating parameters, such as space velocity and inlet concentrations of CO, H2, H2S and COS, on the removal of H2S and COS were performed. Results indicate that the breakthrough time increases with the CO concentration and decreases with the H2 concentration. Thiscan be explained through the water-shift reaction. Space velocity between 3,000~18,000 mL·hr-1·g-1, H2S concentration and COS concentration, however, maintain nearly constant sorbent utilization in the operation conditions.
4. Under reduction conditions, Fe2O3 sorbent will be reduced to low-activity iron oxides. Under oxidation conditions, the sulfurated ferrite sorbent will be oxidized to FeSO4 first. It will be further oxidized to the ferrite sorbent.
5. In the operating range of this study, it can be found that the activation energy, Ea, is 103 kJ/mol and the frequency factor, A, is 1.4 × 1017 for type I model. The activation energy, Ea, is 65.5 kJ/mol and the frequency
factor, A, is 4.3 × 1014 for type II model.

摘要....................................................................................................................I
Abstract............................................................................................................ III
目錄.................................................................................................................. A
表目錄...............................................................................................................E
圖目錄.............................................................................................................. G
第一章 前言..................................................................................................... 1
1-1 研究動機............................................................................................. 1
1-2 研究內容與架構................................................................................. 3
第二章 文獻回顧............................................................................................. 5
2-1 IGCC 發電簡介................................................................................... 5
2-2 硫化氫及硫化羰之特性..................................................................... 8
2-2.1 硫化氫之來源......................................................................... 8
2-2.2 硫化氫之性質......................................................................... 8
2-2.3 硫化氫之危害....................................................................... 10
2-2.4 硫化羰之性質....................................................................... 12
2-2.5 硫化羰之危害....................................................................... 14
2-3 硫化氫及硫化羰之控制技術........................................................... 15
2-3.1 濕式除硫技術....................................................................... 15
2-3.2 乾式除硫技術....................................................................... 19
2-4 吸收劑特性....................................................................................... 25
2-5 吸收劑之選擇................................................................................... 28
2-5.1 單一金屬氧化物吸收劑....................................................... 29
2-5.2 混合型吸收劑....................................................................... 31
2-5.3 載體型吸收劑....................................................................... 33
2-6 氧化鐵之簡介................................................................................... 34
2-7 吸收劑活性衰退............................................................................... 38
2-8 硫化氫及硫化羰轉化之操作參數................................................... 40
2-9 吸收劑脫硫反應動力之探討........................................................... 43
2-9.1 衰退模式............................................................................... 44
2-9.2 Arrhenius 表示式................................................................... 47
第三章 研究方法與實驗器材....................................................................... 48
3-1 研究方法........................................................................................... 48
3-1.1 實驗規劃............................................................................... 48
3-1.2 實驗步驟與方法................................................................... 49
3-2 實驗器材........................................................................................... 52
3-2.1 實驗系統裝置....................................................................... 52
3-2.2 吸收劑與氣體....................................................................... 60
3-3 預備實驗........................................................................................... 62
3-3.1 吸收劑之製備....................................................................... 62
3-3.2 檢量線製作........................................................................... 66
3-3.3 空白實驗............................................................................... 68
第四章 結果與討論....................................................................................... 69
4-1 自製吸收劑之特性分析................................................................... 70
4-1.1 不同載體之氧化鐵吸收劑脫硫性能比較........................... 70
4-1.2 不同活性金屬吸收劑脫硫性能之比較............................... 76
4-1.3 不同鍛燒溫度及鍛燒時間對10%Fe2O3/SiO2 吸收劑晶相之
影響....................................................................................... 80
4-1.4 不同氧化鐵含量之吸收劑脫硫性能之比較....................... 90
4-2 脱硫-再生循環對吸收容量影響之探討......................................... 95
4-2.1 吸收劑再生之程溫脱附試驗............................................... 95
4-2.2 10% Fe2O3/SiO2 吸收劑脫硫－再生循環測試..................... 97
4-2.3 硫回收率分析..................................................................... 102
4-2.4 XRD 分析............................................................................. 104
4-3 操作參數對以10% Fe2O3/SiO2 單獨去除硫化氫之影響............ 108
4-3.1 不同操作溫度對以10% Fe2O3/SiO2 單獨去除硫化氫之影響
............................................................................................. 108
4-3.2 CO 濃度、H2 濃度、H2S 濃度對以10% Fe2O3/SiO2 單獨去
除硫化氫之影響................................................................. 110
4-3.3 空間流速對以10% Fe2O3/SiO2 單獨去除硫化氫之影響. 119
4-4 操作參數對以10% Fe2O3/SiO2 同時去除硫化氫及硫化羰之影響
........................................................................................................ 121
4-4.1 不同操作溫度對以10% Fe2O3/SiO2 同時去除硫化氫及硫化
羰之影響............................................................................. 121
4-4.2 CO 濃度、H2 濃度、H2S 及COS 濃度對以10% Fe2O3/SiO2 同
時去除硫化氫及硫化羰之影響......................................... 126
4-4.3 空間流速對以10%Fe2O3/SiO2 同時去除硫化氫及硫化羰之
影響..................................................................................... 139
4-5 熱重分析......................................................................................... 142
4-5.1 還原氣氛下之熱重分析..................................................... 142
4-5.2 氧化氣氛下之熱重分析..................................................... 146
4-6 吸收劑脫硫前後之分析................................................................. 149
4-6.1 SEM 分析............................................................................. 149
4-6.2 SEM-EDS 分析.................................................................... 155
4-6.3 Mapping 分析....................................................................... 159
4-6.4 BET 表面積與孔洞特性..................................................... 165
4-7 脱硫反應動力模式模擬................................................................. 169
4-7.1 第一型之衰退模式............................................................. 169
4-7.2 第二型之衰退模式............................................................. 173
4-8 以具高溫除塵潛力之Fe2O3/SiO2 吸收劑進行高溫去除硫化氫及硫
化羰................................................................................................ 176
4-8.1 不同吸收劑之硬度測試..................................................... 176
4-8.2 Fe2O3/SiO2 及MnO/SiO2 吸收劑單獨去除硫化羰測試.... 177
4-8.3 以不同表面積之SiO2 為載體之氧化鐵吸收劑金屬回收率
分析..................................................................................... 179
4-8.4 具除塵潛力之Fe2O3/SiO2 吸收劑脫硫再生循環測試..... 182
4-8.5 結論..................................................................................... 184
4-9 綜合比較......................................................................................... 186
第五章 結論與建議..................................................................................... 191
5.1 結論................................................................................................. 191
5-2 建議.................................................................................................. 194
參考文獻....................................................................................................... 195
                                    

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