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Title Page

ABSTRACT

Contents

1. Introduction 11

1.1. Background 11

1.2. Research Objective 12

2. Experimental Section 14

2.1. Materials 14

2.2. Bio-oil 15

2.3. Preparation of tungstate-zirconia supppots 15

2.4. Preparation of catalysts 16

2.5. Apparatus 19

2.6. Hydrodeoxygenation of bio-oils 21

2.7. Characterization of reactants and products 22

2.8. Characterization of catalysts 23

3. Results and discussion 25

3.1. Feedstocks 25

3.2. Extraction with diethyl ether 28

3.3. Hydrodexoygenation of extracted bio-oils on commercial and synthesis catalysts 29

3.4. Comparison of catalytic activity and coke deposition on synthesis catalysts with high LHSV 41

3.5. Phase separation 44

3.6. Coking resistance 46

3.7. Tungstate-zirconia supported catalyst 52

4. Conclusion 59

References 61

List of Tables

Table 1. Summary of commercial and synthesized catalysts properties. 17

Table 2. Compositions of the bio-oil and ether extracted bio-oil. 26

Table 3. Hydrodeoxygenation result of extracted bio-oils on commercial and synthesis catalysts. 32

Table 4. Composition of hydrodeoxygenated bio-oils. 34

Table 5. Main 20 compounds of (a) diethyl ether extracted bio-oil (b)... 39

Table 6. Hydrodeoxygenation result of extracted bio-oils with high LHSV. 42

Table 7. Composition of upgraded bio-oils with high LHSV. 43

Table 8. CO-Chemisorption and N₂-physisorption results of several tested catalysts. 51

Table 9. The amount of acidic sites measured by NH₃-TPD and pyridine-FT-IR. 56

List of Figures

Fig. 1. Scheme of fixed-bed continuous flow reactor system. 20

Fig. 2. Optical microscope images of (a) crude pyrolysis oil (b) ether-... 28

Fig. 3. SimDis-GC results of upgraded liquid product using 3 wt%... 36

Fig. 4. Hydrodeoxygenated bio-oil over 3 wt% Ru/WZr(Wako) with Low... 37

Fig. 5. GC-MS spectroscopy of (a) diethyl ether extracted bio-oil (b) upgraded... 38

Fig. 6. Hydrodeoxygenated bio-oil over (a) 3 wt% Ru/Al₂O₃, (b) 3 wt%... 45

Fig. 7. Thermogravimetry results (a) fresh 3 wt% Ru/ZrO₂, (b) fresh 3 wt%... 48

Fig. 8. Powder X-ray diffraction patterns of (a) fresh 3 wt% Ru/Al2O3, (b)... 49

Fig. 9. Powder X-ray diffraction patterns of (e) fresh 3 wt% Ru/ZrO2, (f)... 50

Fig. 10. NH₃-TPD results of the catalysts. 54

Fig. 11. In-situ FT-IR spectra using pyridine as a probe desorbed at 150℃. 54

Fig. 12. NH₃-TPD results of catalysts measured through TCD and MS. (NH₃... 55

Fig. 13. Proposed reaction mechanism for HDO of bio-oil depending on acidic... 57

Fig. 14. Powder X-ray diffraction patterns of WOx-ZrO₂(WOx-ZrO₂ is notated...[이미지참조] 58

Fig. 15. Raman spectra of WOx-ZrO₂(WOx-ZrO₂ is notated as WZr), ZrO₂ and...[이미지참조] 58

초록보기

Catalytic hydrodeoxygenation of sawdust pyrolysis oils using catalysts was carried out in fixed-bed continuous flow reactor under excess hydrogen condition at 300-350℃ with 100 bar. Fuel-like hydrocarbon was formed as a final liquid product in this reaction. This highly deoxygenated product provides an alternative route for conventional fossil fuels. Although upgrading process is one of the promising technique to improve quality of bio-oil, severe catalyst deactivation, especially in coke formation, is considered major challenge in this study. Therefore, several catalysts were investigated to find an optimum one having high catalytic activity with less formation of cokes for bio-oil upgrading using fixed-bed continuous flow reactor. Tungstate-zirconia-supported Ru catalysts was regarded as an optimum catalyst for bio-oil upgrading. This tungstate-zirconia support showed different acidic and structural properties according to loading of the tungsten wt-% over zirconia. In our study, 10.9 wt% of tungstate-zirconia was identified as ideal loading value which was associated with saturated polytungstate monolayer on zirconia.

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