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研究生： 邱炳嶔
Ping-Chin Chiu
論文名稱： Fe2O3/Al2O3載氧體應用於化學迴圈程序移動床燃料反應器之評估研究
Performance Evaluation of Fe2O3/Al2O3 Oxygen Carrier for Chemical Looping Process by Moving Bed Fuel Reactor
指導教授： 顧洋
Young Ku
口試委員: 談駿嵩
Chung-Sung Tan
蔣本基
Pen-Chi Chiang
曾堯宣
Yao-Hsuan Tseng
郭俞麟
Yu-Lin Kuo
徐恆文
Hen-Wen Hsu
邱耀平
Yau-Pin Chyou
學位類別： 博士
Doctor
系所名稱： 工程學院 - 化學工程系
Department of Chemical Engineering
論文出版年： 2014
畢業學年度： 102
語文別： 英文
論文頁數： 177
中文關鍵詞： 化學迴圈 、載氧體 、移動床反應器 、甲烷 、異丙醇溶液 、聚氨酯 、聚丙烯 、產氫
外文關鍵詞： chemical looping, methane, isopropanol solution, polyurethane, polypropylene, hydrogen generation, oxygen carrier, moving bed
相關次數： 點閱：210  下載：16 
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    • 化學迴圈程序(Chemical Looping Process)為一項具有二氧化碳捕獲能力的能源技術，可產出熱能作為發電使用，同時不需使用額外的氣體分離單元即可產生純度95%以上之二氧化碳。化學迴圈程序係透過載氧體(常為金屬氧化物)在燃料反應器與燃料燃燒進行還原反應，同時可產出高純度二氧化碳；還原後之載氧體藉由輸送裝置進入空氣反應器，由空氣將載氧體氧化至最氧化態，同時產生熱能。載氧體在燃料反應器與空氣反應器之間不斷循環，因此被稱為化學迴圈程序。本研究所製備之含有60 wt% Fe2O3之Fe2O3/Al2O3載氧體在1300 °C下燒結後具有良好的反應性。還原後之載氧體經過XRD鑑定主要晶相為FeAl2O4，可同時具備載體與載氧體之功能。還原後的Fe2O3/Al2O3載氧體置於固定床反應器測試，可透過水氣分解(water splitting)反應產出氫氣。 Fe2O3/Al2O3載氧體壓製為3 mm大小之錠材經過破碎強度測試與熱重分析測試，具有良好的機械強度與反應性，適合應用於移動床反應器之操作。甲烷、異丙醇(IPA)溶液、聚氨酯(PU)及聚丙烯(PP)為本研究所使用之燃料，並與Fe2O3/Al2O3載氧體於移動床燃料反應器進行燃燒反應。當載氧體/燃料進料比達1.14以上反應溫度達900 °C時，可將進料之甲烷完全燃燒。反應後之載氧體經過XRD鑑定後主要晶相為FeO與FeAl2O4，表示透過移動床反應器的操作可增加鐵系載氧體內氧的使用量。CO與H2為異丙醇溶液燃燒時主要的燃料氣體，當載氧體/燃料進料比達7.94以上反應溫度達900 °C時，異丙醇轉化率與CO2產率可達100%。藉由程序熱值之計算，70%的熱輸出功率可提供給其他設備使用，而剩餘熱能則需補充系統內用於氣化液體之熱損。透過程序熱效率之分析，使用水溶液作為液體燃料時，水的蒸發熱將是主要的系統熱損來源，尤其是含碳量較低的溶液。PU與PP之燃燒本研究採用雙套管式移動床反應器(ADMBR)，使固體燃料可在反應器內同時發生氣化與燃燒反應。CO與H2為PU與PP之燃燒時主要的燃料氣體，當PU與PP顆粒之氧體/燃料進料比分別達3.10 與10.94以上反應溫度達900 °C時，PU與PP顆粒之燃料轉化率與CO2產率可達100%。氣化PU與PP顆粒所需之熱能經過熱值計算分別佔21%與52%的系統輸出功率。本研究從製備Fe2O3/Al2O3載氧體、移動床反應器的操作到各種燃料的燃燒，完整評估化學迴圈程序各項重要參數。利用Fe2O3/Al2O3載氧體在移動床反應器除可充分燃燒各種燃料，還原後的載氧體亦具備後續用於產氫之性質。因此本研究所製備之載氧體經各項評估之後，可符合化學迴圈程序應用之需求。

    Chemical looping process is a potential energy technology with inherent CO2 capture to provide superior energy efficiency than existing CO2 capture technologies. Oxygen carriers are applied for chemical looping process in place of air to offer oxygen for fuel combustion; therefore, to enhance CO2 purity in the effluent stream. Alumina supported Fe2O3 were prepared and demonstrated reasonable reactivity for Fe2O3/Al2O3 particles containing 60 wt% Fe2O3 and sintered at 1300 °C. FeAl2O4 was characterized by XRD after reduction and served as supporting material as well as oxygen carrier in practical operation. Hydrogen generation was demonstrated to be feasible by steam oxidation with reduced Fe2O3/Al2O3 oxygen carriers in a fixed bed reactor. Fe2O3/Al2O3 pellets were examined by crush strength and TGA demonstrated proper crush strength and reasonable reactivity as oxygen carrier for chemical looping process. Methane, isopropanol (IPA), polyurethane (PU) and polypropylene (PP) combustions are conducted by a moving bed fuel reactor using the prepared Fe2O3/Al2O3 oxygen carriers. Complete combustion of methane was achieved with oxygen carrier-to-fuel ratio higher than 1.14 at 900 °C. The oxygen carriers that moving out of the moving bed reactor were composed of mainly FeO and FeAl2O4, characterized by X-ray diffraction (XRD) analysis, indicating further utilization of oxygen in Fe-based oxygen carriers can be achieved by moving bed operation. For IPA combustion, CO and H2 were the fuel gases generated by IPA solution in the moving bed reactor prior to combustion with oxygen carriers. The IPA conversion and CO2 yield in the outlet stream from moving bed reactor reached 100% as oxygen carrier-to-fuel ratio was higher than 7.94 at 900 °C. By analysis of system processing capacity, 70% of output processing capacity is available for energy use of external facility. By analysis of processing efficiency, aqueous solution as liquid fuel would cause considerable heat consumption for water evaporation, especially for dilute solution. For PU and PP combustion, an annular duel-tube moving bed reactor (ADMBR) was used as fuel reactor for gasification and combustion of PU and PP particles. CO and H2 were the major components of fuel gas generated by gasification of PU and PP particles in ADMBR. Complete conversion of plastic particles and 100% CO2 yield of fuel gas were achieved as oxygen carrier-to-fuel ratio for PU and PP particles reached 3.10 and 10.94, respectively. The heat demands for ADMBR were calculated to be 21% and 52% of output processing capacity by heat consumptions of fuel gasification in the fuel reactor of CLC system, respectively. This study evaluated essential parameters on preparation of Fe2O3/Al2O3 oxygen carrier, operation of moving bed reactor and fuel combustion. Fe2O3/Al2O3 oxygen carrier was completely combusted fuels in the moving bed reactor; furthermore, the reduced Fe2O3/Al2O3 oxygen carrier was capable for hydrogen generation by steam oxidation. Hence, the prepared Fe2O3/Al2O3 composite was validated as oxygen carrier for chemical looping process.

    Chinese Abstract………………………………………………………………………. I English Abstract……………………………………………………………………. III Acknowledgement………………………………………………………………….. V Contents……………………………….…………………………………………. VII Figures………………………………………………………………………….…. XI Tables….…………………………..………………………………………….…. XV Nomenclatures….………………………………………………………….……. XVII Chapter 1 Introduction……………………………………………..…………………. 1 1.1 Background..……………………………………………..………..……. 1 1.2 Objective and Scope……………………………………...……………. 4 Chapter 2 Review of Literature………………………………………………………. 7 2.1 Introduction of Chemical Looping Processes..……………….……...…. 8 2.1.1 Chemical Looping Combustion………...……………………...…. 8 2.1.2 Chemical Looping Gasification and Reforming….......……...…. 13 2.1.3 Chemical Looping Hydrogen Generation………..…...……...…. 15 2.1.4 Chemical Looping with Oxygen Uncoupling………………..…. 19 2.2 Oxygen Carrier.………………………………………………………. 21 2.3 Reactor System……………………………………...………..………. 28 2.3.1 Fluidized Bed Reactor………………………...………..………. 28 2.3.2 Moving Bed Reactor………………………...………..………. 31 2.4 Fuel Combustion……………………………………..………..………. 34 2.4.1 Methane Combustion……………...…………...……….………. 36 2.4.2 Syngas Combustion……...………………..…...………..………. 38 2.4.3 Solid Fuel Combustion……...………...…..…...………..………. 40 2.4.4 Waste Treatment……...………...…..……….....………..………. 44 Chapter 3 Materials and Experiments.………………………...…...……..………. 47 3.1 Chemicals and Apparatus…………..…...…...………....…...………… 47 3.2 Experimental Framework…………...…...………..…....…...………… 50 3.3 Preparation and Characterization of Fe2O3/Al2O3 Oxygen Carrier……. 52 3.3.1 Preparation of Fe2O3/Al2O3 Oxygen Carrier…………..………. 54 3.3.2 Texture Analyzer……………………………...………..………. 57 3.3.3 Thermogravimetric Analyzer (TGA)………....………..………. 57 3.3.4 Fixed Bed Reactor……………………….…...………..………. 60 3.3.5 Nondispersive Infrared (NDIR) Analyzer……………....………. 62 3.3.6 Gas Chromatograph (GC)……………………..………..………. 62 3.3.7 Field Emission Scanning Electron Microscopy (FESEM) .…... 62 3.3.8 X-ray Diffraction (XRD)…………..……..………..…..………. 63 3.4 Moving Bed Fuel Reactor…….……………………...………..………. 64 3.4.1 Methane Combustion…..……………………...………..………. 64 3.4.2 IPA Combustion…………………..…………...………..………. 67 3.4.3 PU and PP Combustion…………………………….…..………. 70 3.5 Analysis of Fuels…………………………………...………..………. 73 3.5.1 Decomposition of Methane…….……………...………..………. 73 3.5.2 Evaporation of IPA…………………….……...………..………. 73 3.5.3 Gasification of PU and PP………………………..……..………. 74 Chapter 4 Results and Discussion……………………………….....……….………. 75 4.1 Performance of Fe2O3/Al2O3 Oxygen Carrier…………………….....… 76 4.1.1 Thermogravimetric Analysis………………...………..………. 76 4.1.2 Reduction Mechanism of Fe2O3/Al2O3 Oxygen Carrier………. 80 4.1.3 Gas yields in Fixed Bed Reactor…………………..…..………. 84 4.1.4 Hydrogen Generation in Fixed Bed Reactor……………………. 86 4.1.5 Crush Strength of Fe2O3/Al2O3 Oxygen Carriers…………….…. 88 4.1.6 Redox Cycling of Fe2O3/Al2O3 Pellets………………..…….…. 89 4.2 Methane Combustion in Moving Bed Reactor……....………..………. 94 4.2.1 Effect of Retention Time……………………....………..………. 94 4.2.2 Effect of Oxygen Carrier-to-fuel Ratio..……...………..………. 98 4.2.3 X-ray Diffraction Analysis…………………….………..……. 101 4.3 IPA Combustion in Moving Bed Reactor………….....………………. 103 4.3.1 IPA Evaporation in Empty Bed Reactor……………..………. 104 4.3.2 IPA Combustion in Moving Bed Reactor………………..……. 109 4.3.3 Heat Analysis for Chemical Looping System………....………. 111 4.4 PU and PP Combustion in Moving Bed Reactor…………….……. 117 4.4.1 PU and PP Gasification in Empty Bed Reactor……………..…. 117 4.4.2 PU and PP Combustion in Moving Bed Reactor……..…..……. 122 4.4.3 Heat Analysis for Chemical Looping System………....………. 129 Chapter 5 Conclusions and Recommendations……………….....………..………. 133 References…………………………………………………..….....……..………. 139 Appendix……………………………………………………..…..………..………. 151 Curriculum Vitae……………………………………………….....……..………. 169

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