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研究生：	李秉鴻 Lee, Bing-Hong
論文名稱：	以流體化床反應器探討Fe2O3/TiO2載氧體於化學環路燃燒CO、H2及CH4之研究 Study on Chemical Looping Combustion of CO, H2, and CH4 Using Fe2O3/TiO2 Oxygen Carrier in a Fluidized Bed Reactor
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：	2019
畢業學年度：	107
語文別：	英文
論文頁數：	163
中文關鍵詞：	化學環路燃燒、載氧體、Fe2O3/TiO2 、流體化床、合成氣
外文關鍵詞：	Chemical looping combustion, Oxygen carrier, Fe2O3/TiO2, Fluidized bed reactor, Syngas
相關次數：	點閱：71 下載：0
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隨著經濟與科技的快速發展，大量的二氧化碳被排放到了大氣當中，造成了嚴重的全球暖化與氣候變遷等問題。因此，為了有效解決此問題，二氧化碳捕獲與封存技術(CCS)成為了世界各國的發展重點，在這些技術中，化學環路燃燒 (Chemical looping combustion, CLC) 被視為最有潛力且最具經濟效益之技術，可有效降低二氧化碳捕獲成本，避免NOx生成，同時提高燃燒效率。
本研究使用臨濕含浸法自製40 wt% Fe2O3/TiO2作為載氧體，於流體化床反應器中與氣化合成氣(H2, CO, CH4)進行化學環路燃燒，探討不同操作條件(氣體濃度、氣體流速、溫度)對載氧體反應性的影響。在流體化床反應器實驗中，反應速率隨著反應氣體濃度、氣體流速和操作溫度的增加而增加，然而當溫度從800oC升至1,000oC時H2與載氧體間會由於燒結的產生而降低了反應速率。在以CO作為反應氣體的條件下，當溫度從800oC升至1,000oC時利用率從0.45增加至0.77。在本研究中CH4會造成嚴重的積碳，以至於難以精確計算載氧體的利用率。於複合氣體(CO + H2)作為反應氣體的條件下，較高的氣體濃度可以增加反應速率，但同時也會因為過高的反應速率造成燒結的現象，使得載氧體最終利用率的下降。在10次的氧化還原循環試驗中，載氧體表現出優異的耐久性與穩定性。由XRD和TGA的結果證明，反應後載氧體被還原成FeO和Fe。由元素分析(EA)與EDS的結果可知，積碳隨著CO與CH4濃度的上升而增加，但是增加溫度可以減緩由CO所引起的積碳問題。

With the development of economic and technology, a huge number of CO2 has been released to the atmosphere, caused some severe problems such as global warming and climate change. In order to solve those problems, the carbon capture and storage (CCS) technology has been known as a promising solution. Among those technologies, the chemical looping combustion (CLC) has been considered as an efficient and promising technology which can decrease the cost of CO2 separation; avoid the formation of NOx and increase the combustion efficiency.
In this study, the 40 wt% Fe2O3/TiO2 oxygen carriers, which prepared by incipient wetness impregnation method, were used to react with coal and biomass gasified syngas composed of H2, CO, and CH4 under various reaction conditions to investigate the reactivity of oxygen carriers under various operation conditions. In fluidized bed reactor experiments, the reaction rate generally increases with the increasing CO or H2 concentration, superficial velocity, and operating temperature. However, when temperature is 1,000oC the reaction rate of H2 decreases because of the sintering of oxygen carrier. Moreover, the final utilization of 40 wt% Fe2O3/TiO2 under 25% CO, greatly affected by temperature, increases from 0.45 to 0.77 when the operating temperature increases from 800 to 1,000oC. For the case using CH4, it was hard to analyze and calculate the utilization of oxygen carriers due to the hydrogen production and carbon deposition from the decomposition of CH4. For the complex syngas CLC tests, the higher syngas concentration leads higher reaction rate due to the better diffusion capability. However, the higher reaction rate may cause the blocking or sintering of oxygen carrier so that the final utilization decreases with increasing syngas concentration. In the 10 redox cycles test, 40 wt% Fe2O3/TiO2 oxygen carrier shows excellent durability. After the reaction, the oxygen carrier is reduced to the state between FeO and Fe, which could be proved by the results of XRD and TGA. According to the Elementary analyses, it is found that the carbon deposition increases with increasing CO or CH4 concentration. However, when the operating temperature increases from 950 to 1,000oC, it can retard the carbon deposit caused by CO.

摘要	I
Abstract	II
致謝	IV
Content	VI
List of tables	XI
List of figures	XIII
Chapter 1 Introduction	1
1-1	Motivation	1
1-2	Objectives	3
Chapter 2 Literature and Review	4
2-1 Introduction of Carbon Dioxide	4
2-1.1 Influence of Carbon Dioxide	4
2-1.2 Carbon capture, utilization and storage (CCUS)	7
2-2 Power generation system	10
2-2.1 Integrated Gasification Combined Cycle (IGCC)	10
2-2.2 Chemical Looping Combustion (CLC)	13
2-2.3 Chemical Looping Reforming (CLR)	16
2-2.4 Chemical Looping with Oxygen Uncoupling (CLOU)	17
2-3 Characteristics of syngas	19
2-3.1 Carbon monoxide	19
2-3.2 Hydrogen	22
2-3.3 Methane	25
2-4 Preparation of Oxygen Carrier	26
2-4.1 Mechanical mixing	26
2-4.2 Co-precipitation	26
2-4.3 Sol-gel	27
2-4.4 Incipient wetness impregnation	27
2-4.5 Freeze granulation	28
2-5 Characteristics of oxygen carrier	29
2-5.1 Thermodynamics	30
2-5.2 Oxygen ratio	34
2-5.3 Stability of oxygen carrier	35
2-5.4 Mechanical strength	36
2-6 Type of Oxygen carrier	38
2-6.1 Fe-based oxygen carrier	38
2-6.2 Ni-based oxygen carrier	39
2-6.3 Cu-based oxygen carrier	39
2-6.4 Mn-based oxygen carrier	40
2-7 Fluidized bed	41
2-7.1 Fluidization	41
2-7.2 Minimum fluidized velocity	44
2-7.3 Experiment evaluation of minimum fluidized velocity and pressure drop	47
2-8 Deactivation of oxygen carrier	49
2-8.1 Sintering	49
2-8.2 Carbon deposition	49
2-8.3 Poisoning	50
2-8.4 Losses of active sites	50
2-9 Influence of operating parameters	51
2-10 Kinetics	52
2-10.1 Deactivation model	52
2-10.2 Arrhenius equation	54
Chapter 3 Material and Methods	55
3-1 Experimental methods	55
3-1.1 Experimental design	56
3-1.2 Experimental process	58
3-2 Experimental equipment	59
3-2.1 Experimental materials	59
3-2.2 Experimental facilities	60
3-2.3 Analyzer	66
3-3 Preliminary experiment	72
3-3.1 Preparation of oxygen carrier	72
3-3.2 Calibration curve preparation	73
3-3.3 Leakage proof of the system	75
3-3.4 Blank test	75
Chapter 4 Results and Discussion	77
4-1 Fluidization	77
4-1.1 The relationship between pressure drop and superficial velocity	77
4-1.2 Comparison of the experimental and simulated minimum fluidized velocity	79
4-2 Characteristics of oxygen carriers	83
4-2.1 X-ray diffraction (XRD) analysis	83
4-2.2 Inductively couple plasma optical emission spectrometry (ICP-OES)	84
4-2.3 Temperature programmed reduction (TPR) analysis	85
4-2.4 Isothermal thermogravimetric analysis	91
4-2.5 BET surface area analysis	94
4-3 Operating parameter experiment	96
4-3.1 Concentration of gaseous fuels: CO, H2 and CH4	99
4-3.2 Superficial velocity	104
4-3.3 Operating temperature	108
4-3.4 Complex syngas	111
4-3.5 Redox cycles	115
4-4 Characteristics of oxygen carrier before and after reaction	118
4-4.1 X-ray diffraction (XRD) analysis	118
4-4.2 Scanning electron microscope (SEM) analysis	120
4-4.3 Scanning electron microscope with energy dispersive spectroscopy (SEM-EDS) analysis	126
4-4.4 Mapping analysis	130
4-4.5 X-ray photoelectron spectroscope (XPS) analysis	134
4-4.6 Fourier transform infrared (FTIR) analysis	137
4-4.7 Elemental analysis (EA)	139
4-5 Kinetics	140
4-6 Mechanisms	145
Chapter 5 Conclusion and suggestion	147
5-1 Conclusion	147
5-2 Suggestion	150
Chapter 6 Reference	151

                                    

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